CN107623105A - A kind of preparation method of lithium ion battery GND and conductive agent material - Google Patents
A kind of preparation method of lithium ion battery GND and conductive agent material Download PDFInfo
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- CN107623105A CN107623105A CN201710930859.6A CN201710930859A CN107623105A CN 107623105 A CN107623105 A CN 107623105A CN 201710930859 A CN201710930859 A CN 201710930859A CN 107623105 A CN107623105 A CN 107623105A
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Abstract
The invention provides the preparation method of a kind of lithium ion battery GND and conductive agent material, comprise the following steps：Biological material pre-processes：It is biomass carbonated：First step activation process：Second step activation process：3rd step activation process：It is prepared by the electrode slice that biomass carbon is used as GND：Biomass carbon is used as the preparation of battery conductive agent electrode slice：Battery assembles；Biomass material is with Fructus Colocasiae Esculentae stem, rice husk, lotus leaf dry, watermelon vine, peanut shell etc..It is an advantage of the invention that：Resourceful bio-waste is rationally fully make use of, the conductive Carbon Materials prepared have good conducting three-dimensional passage.The conductive characteristic better than conventional conductive agent is shown as conductive agent using its conductive charcoal；There is high specific discharge capacity, high rate performance and cycle life as negative material.
Description
Technical field
The invention belongs to field of lithium ion battery material preparation, is related to a kind of lithium ion battery GND and conductive agent
The preparation method of material.
Background technology
Lithium ion battery have that operating voltage is high, energy density is big, specific capacity is high and can the protrusion such as fast charging and discharging it is excellent
Point, it is widely used in the electronic installations such as mobile phone, notebook computer, portable tester at present；With high-capacity lithium from
Sub- battery is succeeded in developing, and lithium ion battery is widely used and paid close attention to fields such as space flight in electrokinetic cell automobile.So
And high lithium ion battery price turns into the bottleneck for restricting electrokinetic cell development and promoting.Important set as lithium ion battery
Into negative pole, currently used material has carbon, Li4Ti5O12, silicon substrate, alloy anode etc., wherein because Carbon anode price is relatively low
The advantages such as Volume Changes are small before and after honest and clean, low to lithium voltage, circulation, are widely used in high density energy-storage battery and power-type power electric
Chi Zhong.
Porous carbon is prepared due to its complex process by artificial synthesis, cost is high, and pore-size distribution is relatively single, and its
It is made up of more the not good enough agraphitic carbon of electric conductivity, the lithium ion battery applications field of needs good conductive can not be met.It is and biological
Material stable physicochemical properties, is provided effective passage for the transmission of material, made due to its considerable specific surface area
It turns into the important functional material of lithium ion cell electrode.
The content of the invention
The purpose of the present invention is the preparation method for being to provide a kind of lithium ion battery GND and conductive agent material,
This method fully rationally make use of aboundresources using the biomass such as Fructus Colocasiae Esculentae stem, rice husk, lotus leaf dry, watermelon vine, peanut shell as raw material
Bio-waste, the conductive Carbon Materials prepared have good conducting three-dimensional passage.Using its conductive charcoal as conductive agent
Show the conductive characteristic better than conventional conductive agent；There is high specific discharge capacity, high rate performance and circulation as negative material
Life-span.
The technical solution adopted by the present invention is as follows：A kind of preparation side of lithium ion battery GND and conductive agent material
Method, it is characterised in that comprise the following steps：
(1) biological material pre-processes：After supersonic cleaning machine cleaning removes the impurity in biomass, dried at 50 DEG C~80 DEG C
2~6h or so, then material is put into vacuum drying chamber, 10~36h is dried at 100 DEG C~130 DEG C；Finally, by material disintegrating
Make material granular less than 2cm for barred body of the length less than 3cm or particle diameter；
(2) it is biomass carbonated：Under inert atmosphere, 400 DEG C~900 DEG C are heated under 1~25 DEG C/min heating rate
Carbonized, and maintain 1~5h of this temperature；
(3) first step activation process：Acid is added in biomass carbon, 2~10h is stirred at 40 DEG C~80 DEG C, is spent after centrifugation
Ionized water is cleaned to about neutrality, is dried overnight at 50 DEG C~80 DEG C；
(4) second step activation process：Next toward aqueous slkali is added in biomass carbon, stir 2 at 40 DEG C~90 DEG C~
10h, cleaned to about neutrality with deionized water after centrifugation, be dried overnight at 50 DEG C~80 DEG C；
(5) the 3rd step activation process：Salting liquid is added into biomass carbon, 2~12h, centrifugation are stirred at 40 DEG C~90 DEG C
Cleaned to about neutrality with deionized water, be dried overnight at 50 DEG C~80 DEG C afterwards；
(6) biomass carbon is used as the electrode slice preparation of GND：
The first step, the preparation of battery anode slice：Positive active material is mixed with adhesive, conductive agent, solvent and passes through ball
Grinding machine high-speed stirred is uniform, obtain anode sizing agent is uniformly coated on aluminium foil, under vacuum conditions, 70-120 DEG C baking 10-
After 36h, roll-in, cutting obtain positive plate；
Second step, the preparation of negative plate：The biomass carbon of acquisition is mixed with adhesive, conductive agent, solvent and passes through ball milling
Machine high-speed stirred is uniform, obtain cathode size is uniformly coated on copper foil, under vacuum conditions, 70-120 DEG C baking 10-36h
Afterwards, roll-in, cutting obtain negative plate；
(7) biomass carbon is used as the preparation of battery conductive agent electrode slice：
The first step, the preparation of battery anode slice：Positive active material and adhesive, biomass carbon conductive agent, solvent are mixed
Close by ball mill high-speed stirred it is uniform, obtain anode sizing agent is uniformly coated on aluminium foil, under vacuum conditions, 70-120 DEG C
After toasting 10-36h, roll-in, cutting obtain positive plate；
Second step, the preparation of negative plate：The biomass carbon of acquisition is mixed with adhesive, biomass carbon conductive agent, solvent
It is uniform by ball mill high-speed stirred, obtain cathode size is uniformly coated on copper foil, under vacuum conditions, 70-120 DEG C baking
After roasting 10-36h, roll-in, cutting obtain negative plate；
(8) battery assembles；Positive plate, barrier film, negative plate are laminated into battery core together, are placed in battery case, injection electrolysis
Liquid, chemical conversion, partial volume, obtain cylinder and plastic-aluminum Soft Roll type lithium-ion-power cell.
In step (1) of the present invention, biological material is：Fructus Colocasiae Esculentae stem, lotus leaf, lotus leaf are dry, millet stalk, rice husk, reed
Reed, sweet potato stem, watermelon vine, bamboo pole, peanut shell, cotton stem.
In step (2) of the present invention, inert gas is：Helium, nitrogen, argon gas.
In step (3) of the present invention, acid is：Sulfuric acid, nitric acid, hydrochloric acid, perchloric acid, permanganic acid, oxalic acid, phosphoric acid, acetic acid.
In step (4) of the present invention, aqueous slkali is：Sodium hydroxide, potassium hydroxide, nickel hydroxide.
In step (5) of the present invention, salting liquid is：Zinc chloride, sodium chloride, potassium chloride, potassium carbonate, sodium carbonate, sulfuric acid
Sodium, potassium sulfate.
Positive-active of the present invention is rich lithium manganese anode material, cobalt acid lithium, LiMn2O4, nickel-cobalt-manganese ternary material, nickel cobalt
Aluminium ternary material, LiFePO4, lithium manganese phosphate etc..
Adhesive of the present invention is PVDF.
Solvent of the present invention is NMP.
Biomass carbon conductive agent of the present invention is by obtaining after biomass through pyrolysis that invention content is protected
Charcoal).
Advantages of the present invention：(1) biomass carbon obtained has graded porous structure, in-situ three-dimensional graphite linings knot again be present
Structure, good conductive channel is provided for the carrier in electrochemical reaction process, using biomass carbon as conductive agent or lithium from
After the negative pole of sub- battery, the high rate performance, charge/discharge capacity and cycle life of lithium ion battery are improved；(2) used in the present invention
Biological material abundant raw material, cheap, it, which is pyrolyzed obtained biomass carbon, can lift the synthesis electrochemistry of battery
Energy, the cost of lithium ion battery is greatly reduced.
Brief description of the drawings
Fig. 1 is the reed pyrolytic carbon shape appearance figure of embodiments of the invention 1.
Fig. 2 is the Fructus Colocasiae Esculentae stem pyrolytic carbon shape appearance figure of embodiments of the invention 3.
Fig. 3 obtains reed by embodiments of the invention 1 and 3, Fructus Colocasiae Esculentae stem is pyrolyzed charcoal as conductive agent and conventional pilot
The discharge capacity of electric agent material.
Embodiment
It is for a more detailed description to inventing with reference to example, but it is not limited to the following example.
Embodiment 1：
(1) reed collected is cleaned by ultrasonic 3 times, each 30min, in 60 DEG C in air dry oven after removing impurity
Under, 4h is dried, is placed into vacuum drying chamber, 10h is dried at 110 DEG C.Finally, it is the material disintegrating after drying is small to length
In the 3cm body of rod.
(2) under argon gas atmosphere, 600 DEG C is heated under 3 DEG C/min heating rate and is carbonized, be incubated 4h.
(3) hydrochloric acid is added in above-mentioned biological pyrolytic carbon, 6h is stirred at 60 DEG C, is cleaned after centrifugation with deionized water to about
After neutrality, it is dried overnight at 70 DEG C.
(4) sodium hydroxide solution is added in the material by acid solution cleaning, 8h is stirred at 80 DEG C, deionization is used after centrifugation
Water is cleaned to about neutrality, is dried overnight at 70 DEG C.
(5) liquor zinci chloridi is added, 10h is stirred at 90 DEG C, is cleaned after centrifugation with deionized water to about neutrality, 70
DEG C it is dried overnight.
(6) biomass carbon is used as the electrode slice preparation of GND：
The first step, the preparation of battery anode slice：Rich lithium manganese positive active material is mixed with PVDF, Super P, NMP, led to
Cross that ball mill high-speed stirred is uniform, obtained anode sizing agent is uniformly coated on aluminium foil, under vacuum environment, 110 DEG C of baking 12h
Afterwards, roll-in, cutting obtain positive plate；
Second step, the preparation of negative plate：The biomass carbon of acquisition is mixed with PVDF, Super P, NMP and passes through ball mill
High-speed stirred is uniform, and obtained cathode size is uniformly coated on copper foil, under vacuum conditions, after 110 DEG C of baking 12h, roll-in,
Cutting obtains negative plate；
(7) biomass carbon is used as the preparation of electrode slice during battery conductive agent：
The first step, the preparation of battery anode slice：By rich lithium manganese positive active material and PVDF, biomass carbon conductive agent, NMP
Mixing, uniform by ball mill high-speed stirred, obtained anode sizing agent is uniformly coated on aluminium foil, under vacuum conditions, 110 DEG C
After toasting 12h, roll-in, cutting obtain positive plate；
Second step, the preparation of negative plate：Graphite cathode is mixed with PVDF, biomass carbon conductive agent, NMP and passes through ball mill
High-speed stirred is uniform, and obtained cathode size is uniformly coated on copper foil, under vacuum conditions, after 110 DEG C of baking 12h, roll-in,
Cutting obtains negative plate.
(8) battery assembles；Positive plate, barrier film, negative plate are laminated into battery core together, are placed in battery case, injection electrolysis
Liquid, chemical conversion, partial volume, obtain cylinder and plastic-aluminum Soft Roll type lithium-ion-power cell.
Embodiment 2：
With (1) the step of embodiment 1.
(1) under nitrogen atmosphere, 800 DEG C is heated under 5 DEG C/min heating rate and is carbonized, be incubated 4h.
(2) nitric acid is added in above-mentioned biological pyrolytic carbon, 6h is stirred at 60 DEG C, is cleaned after centrifugation with deionized water to about
After neutrality, it is dried overnight at 70 DEG C.
(3) potassium hydroxide solution is added in the material by acid solution cleaning, 8h is stirred at 80 DEG C, deionization is used after centrifugation
Water is cleaned to about neutrality, is dried overnight at 70 DEG C.
(4) solution of potassium carbonate is added, 10h is stirred at 90 DEG C, is cleaned after centrifugation with deionized water to about neutrality, 70
DEG C it is dried overnight.
(5) biomass carbon is used as the electrode slice preparation of GND：With implementation column 1.
(6) biomass carbon is used as the preparation of electrode slice during battery conductive agent：With implementation column 1.
(7) battery assembles：With implementation column 1.
Embodiment 3：
(1) Fructus Colocasiae Esculentae stem collected is cleaned by ultrasonic 5 times, each 30min, in 70 in air dry oven after removing impurity
At DEG C, 5h is dried, places into vacuum drying chamber, dries 12h at 110 DEG C.Finally, the material disintegrating after drying to length is less than
The 3cm body of rod.
(2) under argon gas atmosphere, 600 DEG C is heated under 5 DEG C/min heating rate and is carbonized, be incubated 6h.
(3) sulfuric acid is added in above-mentioned biological pyrolytic carbon, 6h is stirred at 60 DEG C, is cleaned after centrifugation with deionized water to about
After neutrality, it is dried overnight at 70 DEG C.
(4) potassium hydroxide and potassium carbonate mixed solution are added in the material by acid solution cleaning, 12h is stirred at 80 DEG C,
Cleaned to about neutrality with deionized water after centrifugation, be dried overnight at 70 DEG C.
(5) biomass carbon is used as the electrode slice preparation of GND：With implementation column 1.
(6) biomass carbon is used as the preparation of electrode slice during battery conductive agent：With implementation column 1.
(7) battery assembles：With implementation column 1.
Embodiment 4：
(1) with embodiment 3.
(2) under helium atmosphere, 850 DEG C is heated under 8 DEG C/min heating rate and is carbonized, be incubated 6h.
(3) phosphoric acid is added in above-mentioned biological pyrolytic carbon, 6h is stirred at 80 DEG C, is cleaned after centrifugation with deionized water to about
After neutrality, it is dried overnight at 70 DEG C.
(4) sodium hydroxide and sodium carbonate mixture are added in the material by acid solution cleaning, 12h is stirred at 80 DEG C,
Cleaned to about neutrality with deionized water after centrifugation, be dried overnight at 70 DEG C.
(5) biomass carbon is used as the electrode slice preparation of GND：With implementation column 1.
(6) biomass carbon is used as the preparation of electrode slice during battery conductive agent：With implementation column 1.
(7) battery assembles：With implementation column 1.
Embodiment 5：
(1) rice husk collected is cleaned by ultrasonic 6 times, each 30min, after removing impurity in vacuum drying chamber, in 110
10h is dried at DEG C.Finally, it is the material disintegrating after drying to length is granular less than 2cm.
(2) under argon gas atmosphere, 600 DEG C is heated under 3 DEG C/min heating rate and is carbonized, be incubated 4h.
(3) oxalic acid is added in above-mentioned biological pyrolytic carbon, 8h is stirred at 50 DEG C, is cleaned after centrifugation with deionized water to about
After neutrality, it is dried overnight at 70 DEG C.
(4) sodium hydroxide solution is added in the material by acid solution cleaning, 8h is stirred at 80 DEG C, deionization is used after centrifugation
Water is cleaned to about neutrality, is dried overnight at 70 DEG C.
(5) sodium carbonate liquor is added, 10h is stirred at 90 DEG C, is cleaned after centrifugation with deionized water to about neutrality, 70
DEG C it is dried overnight.
(6) biomass carbon is used as the electrode slice preparation of GND：
The first step, the preparation of battery anode slice：Positive active material cobalt acid lithium is mixed with PVDF, acetylene black, NMP, led to
Cross that ball mill high-speed stirred is uniform, obtained anode sizing agent is uniformly coated on aluminium foil, under vacuum environment, 110 DEG C of baking 12h
Afterwards, roll-in, cutting obtain positive plate；
Second step, the preparation of negative plate：The biomass carbon of acquisition is mixed by ball mill height with PVDF, acetylene black, NMP
Speed is stirred, and obtained cathode size is uniformly coated on copper foil, under vacuum conditions, after 110 DEG C of baking 12h, roll-in, is divided
Cut acquisition negative plate；
(7) biomass carbon is used as the preparation of electrode slice during battery conductive agent：
The first step, the preparation of battery anode slice：By positive active material cobalt acid lithium and PVDF, biomass carbon conductive agent, NMP
Mixing, uniform by ball mill high-speed stirred, obtained anode sizing agent is uniformly coated on aluminium foil, under vacuum conditions, 110 DEG C
After toasting 12h, roll-in, cutting obtain positive plate；
Second step, the preparation of negative plate：By Li4Ti5O12Mix with PVDF, biomass carbon conductive agent, NMP and pass through ball mill
High-speed stirred is uniform, and obtained cathode size is uniformly coated on copper foil, under vacuum conditions, after 110 DEG C of baking 12h, roll-in,
Cutting obtains negative plate.
(8) battery assembles：With implementation column 1.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires rather than described above limits, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.Any reference in claim should not be considered as to the involved claim of limitation.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that those skilled in the art should for clarity
Using specification as an entirety, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
It is appreciated that other embodiment.
Claims (6)
1. the preparation method of a kind of lithium ion battery GND and conductive agent material, it is characterised in that comprise the following steps：
(1) biological material pre-processes：Supersonic cleaning machine cleaning remove biomass in impurity after, at 50 DEG C~80 DEG C dry 2~
6h or so, then material is put into vacuum drying chamber, 10~36h is dried at 100 DEG C~130 DEG C；Finally, material disintegrating is made into material
Expect for length less than 3cm barred body or particle diameter be less than 2cm it is granular；
(2) it is biomass carbonated：Under inert atmosphere, 400 DEG C~900 DEG C progress are heated under 1~25 DEG C/min heating rate
Charing, and maintain 1~5h of this temperature；
(3) first step activation process：Acid is added in biomass carbon, 2~10h is stirred at 40 DEG C~80 DEG C, deionization is used after centrifugation
Water is cleaned to about neutrality, is dried overnight at 50 DEG C~80 DEG C；
(4) second step activation process：Next toward adding aqueous slkali in biomass carbon, 2~10h of stirring at 40 DEG C~90 DEG C, from
Cleaned to about neutrality with deionized water after the heart, be dried overnight at 50 DEG C~80 DEG C；
(5) the 3rd step activation process：Salting liquid is added into biomass carbon, 2~12h is stirred at 40 DEG C~90 DEG C, is used after centrifugation
Deionized water is cleaned to about neutrality, is dried overnight at 50 DEG C~80 DEG C；
(6) biomass carbon is used as the electrode slice preparation of GND：
The first step, the preparation of battery anode slice：Positive active material is mixed with adhesive, conductive agent, solvent and passes through ball mill
High-speed stirred is uniform, obtain anode sizing agent is uniformly coated on aluminium foil, under vacuum conditions, 70-120 DEG C baking 10-36h
Afterwards, roll-in, cutting obtain positive plate；
Second step, the preparation of negative plate：The biomass carbon of acquisition is mixed by ball mill height with adhesive, conductive agent, solvent
Speed stirs, obtain cathode size is uniformly coated on copper foil, under vacuum conditions, 70-120 DEG C baking 10-36h after,
Roll-in, cutting obtain negative plate；
(7) biomass carbon is used as the preparation of battery conductive agent electrode slice：
The first step, the preparation of battery anode slice：Positive active material is mixed with adhesive, biomass carbon conductive agent, solvent and led to
It is uniform to cross ball mill high-speed stirred, obtain anode sizing agent is uniformly coated on aluminium foil, under vacuum conditions, 70-120 DEG C baking
After 10-36h, roll-in, cutting obtain positive plate；
Second step, the preparation of negative plate：The biomass carbon of acquisition is mixed and passed through with adhesive, biomass carbon conductive agent, solvent
Ball mill high-speed stirred is uniform, obtain cathode size is uniformly coated on copper foil, under vacuum conditions, 70-120 DEG C baking
After 10-36h, roll-in, cutting obtain negative plate；
(8) battery assembles；Positive plate, barrier film, negative plate are laminated into battery core together, are placed in battery case, injection electrolyte, is changed
Into, partial volume, cylinder and plastic-aluminum Soft Roll type lithium-ion-power cell are obtained.
2. the preparation method of a kind of lithium ion battery GND according to claim 1 and conductive agent material, it is special
Sign is：In the step (1), biological material is：Fructus Colocasiae Esculentae stem, lotus leaf, lotus leaf are dry, millet stalk, rice husk, reed, sweet potato
Stem, watermelon vine, bamboo pole, peanut shell, cotton stem.
3. the preparation method of a kind of lithium ion battery GND according to claim 1 and conductive agent material, it is special
Sign is：In the step (2), inert gas is：Helium, nitrogen, argon gas.
4. the preparation method of a kind of lithium ion battery GND according to claim 1 and conductive agent material, it is special
Sign is：In the step (3), acid is：Sulfuric acid, nitric acid, hydrochloric acid, perchloric acid, permanganic acid, oxalic acid, phosphoric acid, acetic acid.
5. the preparation method of a kind of lithium ion battery GND according to claim 1 and conductive agent material, it is special
Sign is：In the step (4), aqueous slkali is：Sodium hydroxide, potassium hydroxide, nickel hydroxide.
6. the preparation method of a kind of lithium ion battery GND according to claim 1 and conductive agent material, it is special
Sign is：In the step (5), salting liquid is：Zinc chloride, sodium chloride, potassium chloride, potassium carbonate, sodium carbonate, sodium sulphate, sulfuric acid
Potassium.
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| CN109742384A (en) * | 2019-01-07 | 2019-05-10 | 中国矿业大学 | A kind of biomass porous carbon is used as the method for kalium ion battery cathode |
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| CN114039050B (en) * | 2021-11-01 | 2023-08-29 | 哈尔滨万鑫石墨谷科技有限公司 | Carbonized biomass conductive slurry, and preparation method and application thereof |
| CN114665053A (en) * | 2022-05-24 | 2022-06-24 | 中科南京绿色制造产业创新研究院 | Manganese dioxide nano-material positive pole piece, preparation method thereof and zinc ion battery containing manganese dioxide nano-material positive pole piece |
| CN114665053B (en) * | 2022-05-24 | 2022-08-16 | 中科南京绿色制造产业创新研究院 | Manganese dioxide nano-material positive pole piece, preparation method thereof and zinc ion battery containing manganese dioxide nano-material positive pole piece |
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