CN107275578A - A kind of method that use nitrogen-doped porous carbon material makes kalium ion battery negative pole - Google Patents
A kind of method that use nitrogen-doped porous carbon material makes kalium ion battery negative pole Download PDFInfo
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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Abstract
A kind of method that use nitrogen-doped porous carbon material makes kalium ion battery negative pole, belongs to the preparation method of kalium ion battery negative pole.Nitrogen-doped porous carbon material is prepared first, is taken technical parameter in high temperature solid-phase sintering method simple and easy to get, regulation and control course of reaction, is prepared nitrogen-doped porous carbon material structure, kalium ion battery negative pole is then made using nitrogen-doped porous carbon material；Nitrogen source is dissolved in solvent, clear solution is formed, and proper amount of carbon source will be added in above-mentioned solution, makes the full and uniform diffusion of nitrogen source by stirring and being continuously added solvent, obtains white product；White product is placed in after being dried 3 10 hours in freeze drier and be transferred in crucible, and in vacuum tube furnace under argon gas atmosphere with 1 10 DEG C/min speed be warming up to 350 1200 degrees Celsius be incubated 36 hours, the product of generation produces target product through separating-purifying.Kalium ion battery negative pole, electrochemical performance, low in raw material price, synthetic method is simple, and operating procedure controllability is high, is relatively easy to expanding production.
Description
Technical field
The present invention relates to a kind of preparation method of kalium ion battery negative pole, particularly one kind uses nitrogen-doped porous carbon material
The method for making kalium ion battery negative pole.
Background technology
Lithium ion battery has that energy density is high, have extended cycle life and the outstanding advantages such as pollution-free, it has also become Battery Market
Main flow, and start be applied to driving electric automobile.But with the large-scale application of lithium ion battery, the price of lithium and resource
Finiteness is increasingly worried by people.In recent years, many new replacement energy-storage batteries arise at the historic moment, and develop rapidly, main bag
Include the secondary cells such as sodium ion, potassium ion, magnesium ion, calcium ion.Kalium ion battery has many advantages, wherein potassium resource price just
Preferably, the normal reduction potential of the rich content in the earth's crust, kalium ion battery and lithium ion battery is closest thus energy
Density is high, and the active height of kalium ion battery electrolyte electrochemical is conducive to the transmission of ion and electronics.At present the potassium reported from
Sub- cell negative electrode material is less, and wherein carbon material there is relatively low deintercalation potassium current potential easily to form dendrite cause potential safety hazard.Cause
This exploitation environmental protection, Stability Analysis of Structures, electrochemistry deintercalation potassium platform is suitable, and the big new kalium ion battery of specific capacity has very
Important meaning.
Recently, the N doping of carbon material causes the extensive concern of researcher, because N doping is a kind of improvement carbon material
The effective ways of chemical property in the device such as kalium ion battery and ultracapacitor.Why very attractive N doping is,
Main cause is as follows.First, nitrogen-atoms is smaller than carbon atom, and electronegativity is strong, nitrogen atom doping can strengthen be doped carbon material with
Combination between potassium, so as to be conducive to the insertion of potassium ion；Secondly, nitrogen is incorporated into graphite-like carbon structure (such as CNT)
It is a kind of effective ways to form n-type doping, the electric conductivity of carbon material can be improved.Finally, N doping can be in carbon structure
Substantial amounts of defect is caused, these defects can provide more avtive spots for the storage of potassium.
But traditional N doping porous carbon preparation method mainly uses NH3, the post treatment method such as plasma or hydrazine
Nitrogen-atoms is introduced in carbon material.But these methods are mostly more complicated, and the nitrogen atom content mixed is limited, is difficult to realize
Uniform, controllable adulterates.However, the N doping carbon materials that up to the present chemical constituent uniformity is good, purity is high, microstructure is regular
There is not been reported for the preparation method of material, and this constrains further applying for kalium ion battery negative material significantly.
The content of the invention
The invention aims to provide a kind of raw material used to be easy to get, synthetic method is simple, and operating procedure controllability is high
The method that kalium ion battery negative pole is made using nitrogen-doped porous carbon material.
The object of the present invention is achieved like this：The preparation method of kalium ion battery negative pole：It is porous that N doping is prepared first
Carbon material, takes technical parameter in high temperature solid-phase sintering method simple and easy to get, regulation and control course of reaction, prepares N doping many
Hole carbon material structure, then makes kalium ion battery negative pole using nitrogen-doped porous carbon material.
The preparation method of kalium ion battery negative pole, is comprised the following steps that：
(1) it is 70: 20 in mass ratio by the nitrogen-doped porous carbon material of preparation, conductive black and binding agent Kynoar
: 10 are scattered in 1-METHYLPYRROLIDONE solution slurry are made, and slurry is uniformly coated in copper foil current collector；Again by film
Electrode slice afterwards is dried in air dry oven under 50 ± 20 degrees Celsius, obtains electrode slice；
(2) electrode slice of acquisition is cut into a diameter of 14 millimeters of circular electrode, and after being suppressed with powder press, then
120 degrees Celsius are placed in vacuum drying oven to dry 12 hours, then move into after being placed 24 hours in special gloves case i.e. acquisition potassium from
Sub- battery electrode piece；The pressure of described powder press is 15 MPas.
Described nitrogen-doped porous carbon material preparation method, comprises the following steps：
(1) nitrogen source is dissolved in solvent, nitrogen source is 1 with solvent burden ratio mass ratio:2~5, it is configured to transparent solution；And
Carbon source is added in above-mentioned solution, solution is 1 with carbon source quality proportioning:0.8~2, form a kind of whiteness；
(2) above-mentioned whiteness is placed in drying in freeze drier and produces initial product in 3-10 hours；
(3) initial product for obtaining step (2) in vacuum tube furnace under argon gas atmosphere with 1-10 DEG C/min speed
It is warming up to 350-1200 degrees Celsius and is incubated 3-6 hours, then through separating-purifying is that can obtain nitrogen-doped porous carbon material.
Described nitrogen source is ammonium salt, is ammonium carbonate ((NH4)2CO3), ammonium hydrogen carbonate (NH4HCO3), ammonium chloride (NH4Cl) or
Urea (CO (NH2)2) in one kind；It is preferred that, nitrogen source is ammonium chloride (NH4) or urea (CO (NH Cl2)2)。
Described solvent is deionized water or ethanol.
Described carbon source is modified high water soluble polymer (polyacrylic resin).
Separating-purifying in described step (3) is centrifugation or Buchner funnel suction filtration, deionized water cyclic washing.
Kalium ion battery electrode slice is tested：
In the environment full of argon gas, electrode slice, barrier film and potassium piece are assembled into button cell in conventional manner and carried out
Constant current charge-discharge capacity and cycle performance test；
Result of the test：Nitrogen-doped porous carbon material is under the current condition of 50 milliamperes/gram, first and second of discharge capacity
Respectively 1153,533 MAhs/g, capacity tends towards stability thereafter, fully shows high specific capacity.
Beneficial effect：As a result of such scheme, nitrogen-doped porous carbon material has been prepared first, and raw material used is easy
, preparation method is simple, it is easy to operate, and the product of institute is high-purity, and particle diameter distribution is narrower, regular appearance, is relatively easy to advise greatly
Mould industrialized production.Meanwhile, the structural material is shown to excellent chemical property as kalium ion battery negative material,
Both the low shortcoming of the traditional carbon negative pole material specific capacity of commercialization kalium ion battery is overcome, but also with conventional transition metal oxygen
The excellent cycling stability that compound negative material does not possess, has directive function to developing new kalium ion battery.
Advantage：Raw material used is easy to get, and synthetic method is simple, and operating procedure controllability is high, and products obtained therefrom be purity it is high,
Uniform particle diameter, is relatively easy to expanding production.Meanwhile, the porous structure material is shown as kalium ion battery negative material excellent
Different chemical property.
Brief description of the drawings：
Fig. 1 is the powder X-ray diffraction pattern figure of the nitrogen-doped porous carbon material of the embodiment of the present invention 1.
Fig. 2 is the electron scanning micrograph of the N doping porous carbon of the embodiment of the present invention 1.
Fig. 3 is charging and discharging curve of the nitrogen-doped porous carbon material of the embodiment of the present invention 1 in milliampere/gram of constant current density 50
Figure.
Embodiment
The preparation method of kalium ion battery negative pole：Nitrogen-doped porous carbon material is prepared first, takes high temperature simple and easy to get
Technical parameter in solid-phase sintering method, regulation and control course of reaction, is prepared nitrogen-doped porous carbon material structure, is then mixed using nitrogen
Miscellaneous porous carbon materials make kalium ion battery negative pole.
The preparation method of kalium ion battery negative pole, is comprised the following steps that：
(1) it is in mass ratio by the nitrogen-doped porous carbon material of preparation, conductive black and graphite, binding agent Kynoar
Be scattered in 1-METHYLPYRROLIDONE solution be made slurry at 70: 20: 10, and slurry is uniformly coated in copper foil current collector；Again
Electrode slice after film is dried in air dry oven under 50 ± 20 degrees Celsius, electrode slice is obtained；
(2) electrode slice of acquisition is cut into a diameter of 14 millimeters of circular electrode, and after being suppressed with powder press, then
120 degrees Celsius are placed in vacuum drying oven to dry 12 hours, then move into after being placed 24 hours in special gloves case i.e. acquisition potassium from
Sub- battery electrode piece；The pressure of described powder press is 15 MPas.
Described nitrogen-doped porous carbon material preparation method, comprises the following steps：
(1) nitrogen source is dissolved in solvent, nitrogen source is 1 with solvent burden ratio mass ratio:2~5, it is configured to transparent solution；And
Carbon source is added in above-mentioned solution, solution is 1 with carbon source quality proportioning:0.8~2, form a kind of whiteness；
(2) above-mentioned whiteness is placed in drying in freeze drier and produces initial product in 3-10 hours；
(3) initial product for obtaining step (2) in vacuum tube furnace under argon gas atmosphere with 1-10 DEG C/min speed
It is warming up to 350-1200 degrees Celsius and is incubated 3-6 hours, then through separating-purifying is that can obtain nitrogen-doped porous carbon material.
Described nitrogen source is ammonium salt, is ammonium carbonate ((NH4)2CO3), ammonium hydrogen carbonate (NH4HCO3), ammonium chloride (NH4Cl) or
Urea (CO (NH2)2) in one kind, it is preferred that nitrogen source be ammonium chloride (NH4) or urea (CO (NH Cl2)2)；
Described solvent is deionized water or ethanol；
Described carbon source is modified high water soluble polymer (polyacrylic resin).
Separating-purifying in described step (3) is centrifugation or Buchner funnel suction filtration, deionized water cyclic washing.
Kalium ion battery electrode slice is tested：
In the environment full of argon gas, electrode slice, barrier film and potassium piece are assembled into button cell in conventional manner and carried out
Constant current charge-discharge capacity and cycle performance test；
Result of the test：Nitrogen-doped porous carbon material is under the current condition of 50 milliamperes/gram, first and second of discharge capacity
Respectively 1153,533 MAhs/g, capacity tends towards stability thereafter, fully shows high specific capacity.
Embodiment 1：The preparation of nitrogen-doped porous carbon material and structural characterization
Take 0.3g NH4Cl, which is put into beaker and adds 1ml deionized water sonic oscillations, is configured to clear solution, by 1.2g
High water soluble polymer (polyacrylic resin) is added in above-mentioned clear solution, the ultrasonic agitation when adding；It is last slowly to add
Enter deionized water to the more fluffy whiteness of formation.Above-mentioned substance is transferred in freeze drier and dried 10 hours, obtains white
Color powder.After the completion of drying, take appropriate powder be put in crucible and in vacuum tube furnace under argon gas atmosphere with 3 DEG C/min speed
Rate be warming up to 850 degrees Celsius be incubated 5 hours, the black product of generation through deionized water cyclic washing, and with Buchner funnel suction filtration,
Dry black powder product.Product is penetrated through German Brooker Bruker D8ADVANCE x-ray powder diffraction instruments with Cu K α
Line (wavelengthScanning leg speed is 0.08 °/sec) unordered carbon material (Fig. 1) is accredited as, nitrogen-doped porous carbon material exists
24 ° or so have wideization diffraction maximum, (002) face of correspondence graphite structure, no other impurities peak occurs.
Fig. 1 is the powder X-ray diffraction pattern of N doping porous carbon；Wherein left ordinate is relative intensity
(Intensity), abscissa is angle of diffraction (2 θ).
Using the pattern of the porous carbon nano-particle of JSF-6700 scanning electron microscopic observation N dopings, as shown in Fig. 2 N doping is more
The nano particle that hole carbon is mainly distributed in 200nm or so by grain size is constituted, and uniform in size, Size Distribution is narrower.
Electrochemical property test：Nitrogen-doped carbon material, electrically conductive graphite are weighed respectively by weight for 70: 20: 10 ratio
And Kynoar, ball milling 2 after adhesive Kynoar is mixed by a certain percentage with 1-METHYLPYRROLIDONE solution solvent
Hour, active material and binder solution, ball milling 2 hours are added in ball grinder by a certain percentage, electrode slurry is obtained；Will slurry
Material is uniformly coated in copper foil current collector；The electrode slice after film is dried in air dry oven under 50 ± 20 degrees Celsius again
It is dry；The electrode slice of acquisition is cut according to predetermined dimensions, and after being suppressed with powder press (15 MPas of pressure), then it is placed in vacuum
Dried 12 hours for 120 degrees Celsius in baking oven, then move into 24 hours rears of placement in glove box and can be used；In the hand full of argon gas
In casing, electrode slice, barrier film and potassium piece are assembled into button cell in conventional manner and constant current charge-discharge capacity is carried out.Its electrification
Learn performance as shown in Figure 3.
Embodiment 2：Take 0.3g NH4Cl be put into beaker and add 1ml deionized water sonic oscillations be configured to it is transparent molten
Liquid, adds 1.2g high water solubles polymer (polyacrylic resin) in above-mentioned clear solution by gram, and when adding, ultrasound is stirred
Mix；Deionized water is finally slowly added to the more fluffy whiteness of formation.Above-mentioned substance is transferred in freeze drier and done
Dry 10 hours, obtain white dried powder.After the completion of drying, appropriate powder is taken to be put in crucible and the argon gas gas in vacuum tube furnace
Under atmosphere with 3 DEG C/min speed be warming up to 650 degrees Celsius be incubated 5 hours, the black product of generation through deionized water cyclic washing,
And with Buchner funnel suction filtration, dry black powder product.
Gained superfine powder is the amorphous carbon structure of nitrogen-doped porous carbon material, and product is about 170nm's by average grain diameter
Nano particle is constituted.
Embodiment 3：Take 0.5g CO (NH2)2Be put into beaker and add 1ml deionized water sonic oscillations be configured to it is transparent molten
Liquid, 1g high water solubles polymer (polyacrylic resin) is added in above-mentioned clear solution, the ultrasonic agitation when adding；Finally
Deionized water is slowly added to the more fluffy whiteness of formation.Above-mentioned substance is transferred in freeze drier dry 10 small
When, obtain white powder material.After the completion of drying, take it is appropriate in crucible and in vacuum tube furnace under argon gas atmosphere with 3 DEG C/
Min speed is warming up to 650 degrees Celsius and is incubated 5 hours, and the black product of generation leaks through deionized water cyclic washing, and with Bu Shi
Struggle against suction filtration, dry black powder product.
Gained superfine powder is the amorphous carbon structure of nitrogen-doped porous carbon material, the nanometer for being about 200nm by average grain diameter
Particle is constituted.
Claims (7)
1. a kind of method that use nitrogen-doped porous carbon material makes kalium ion battery negative pole, it is characterized in that：Kalium ion battery is born
The preparation method of pole：Nitrogen-doped porous carbon material is prepared first, takes high temperature solid-phase sintering method simple and easy to get, regulation and control reaction
During technical parameter, prepare nitrogen-doped porous carbon material structure, then using nitrogen-doped porous carbon material make potassium from
Sub- GND.
2. the method that a kind of use nitrogen-doped porous carbon material according to claim 1 makes kalium ion battery negative pole, its
It is characterized in：The preparation method of kalium ion battery negative pole, is comprised the following steps that：
(1) it is 70: 20: 10 in mass ratio by the nitrogen-doped porous carbon material of preparation, conductive black and binding agent Kynoar
It is scattered in 1-METHYLPYRROLIDONE solution and slurry is made, slurry is uniformly coated in copper foil current collector；Again by after film
Electrode slice in air dry oven under 50 ± 20 degrees Celsius dry, obtain electrode slice；
（2）The electrode slice of acquisition is cut into a diameter of 14 millimeters of circular electrode, and after being suppressed with powder press, then be placed in
Dried 12 hours for 120 degrees Celsius in vacuum drying oven, then move into and potassium ion electricity is obtained after being placed 24 hours in special gloves case
Pond electrode slice；The pressure of described powder press is 15 MPas.
3. the method that a kind of use nitrogen-doped porous carbon material according to claim 1 or 2 makes kalium ion battery negative pole,
It is characterized in that：Described nitrogen-doped porous carbon material preparation method, comprises the following steps：
（1）Nitrogen source is dissolved in solvent, nitrogen source is 1 with solvent burden ratio mass ratio:2 ~ 5, it is configured to transparent solution；And by carbon
Source is added in above-mentioned solution, and solution is 1 with carbon source quality proportioning:0.8 ~ 2, form a kind of whiteness；
（2）Above-mentioned whiteness is placed in drying in freeze drier and produces initial product within 3-10 hours；
（3）By step（2）Obtained initial product is heated up in vacuum tube furnace under argon gas atmosphere with 1-10 DEG C/min speed
3-6 hours are incubated to 350-1200 degrees Celsius, then through separating-purifying is that can obtain nitrogen-doped porous carbon material.
4. the method that a kind of use nitrogen-doped porous carbon material according to claim 3 makes kalium ion battery negative pole, its
It is characterized in：Described nitrogen source be ammonium salt, be ammonium carbonate (（NH4）2CO3), ammonium hydrogen carbonate (NH4HCO3), ammonium chloride（NH4Cl）Or urine
Element (CO (NH2)2）In one kind.
5. the method that a kind of use nitrogen-doped porous carbon material according to claim 3 makes kalium ion battery negative pole, its
It is characterized in：Described solvent is deionized water or ethanol.
6. the method that a kind of use nitrogen-doped porous carbon material according to claim 3 makes kalium ion battery negative pole, its
It is characterized in：Described carbon source is modified high water soluble polymer（Polyacrylic resin）.
7. the method that a kind of use nitrogen-doped porous carbon material according to claim 3 makes kalium ion battery negative pole, its
It is characterized in：Described step（3）In, separating-purifying is centrifugation or Buchner funnel suction filtration, deionized water cyclic washing.
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Cited By (8)
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| CN107768645A (en) * | 2017-11-28 | 2018-03-06 | 吉林大学 | A kind of porous nitrogen-doped carbon nanometer sheet composite negative pole material and preparation method thereof |
| CN108598419A (en) * | 2018-04-24 | 2018-09-28 | 珠海光宇电池有限公司 | A kind of lithium carbon compound cathode piece and preparation method thereof and lithium secondary battery |
| CN109301220A (en) * | 2018-10-10 | 2019-02-01 | 东北大学秦皇岛分校 | A kind of N doping hard carbon material, preparation method and its kalium ion battery as cathode |
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| CN109768235A (en) * | 2018-12-24 | 2019-05-17 | 肇庆市华师大光电产业研究院 | A kind of lithium ion battery negative material and preparation method thereof |
| CN111682205A (en) * | 2020-05-30 | 2020-09-18 | 中国海洋大学 | Method for preparing bubble-cushion-like porous carbon material with assistance of double-salt crystal template and potassium storage application of bubble-cushion-like porous carbon material |
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