CN107555412A - A kind of preparation method of N doping porous carbon and its application on lithium ion battery - Google Patents
A kind of preparation method of N doping porous carbon and its application on lithium ion battery Download PDFInfo
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- CN107555412A CN107555412A CN201710801446.8A CN201710801446A CN107555412A CN 107555412 A CN107555412 A CN 107555412A CN 201710801446 A CN201710801446 A CN 201710801446A CN 107555412 A CN107555412 A CN 107555412A
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Abstract
The present invention discloses a kind of preparation method of N doping porous carbon and its application on lithium ion battery, nitrogen source is dissolved in solvent including step 1) and is configured to clear solution, and proper amount of carbon source is added in above-mentioned solution, fluffy flakes material is formed, above-mentioned flakes material is placed in freeze drier and dried 1 10 hours；2) compounding substances obtained after step 1) is dried are warming up to 300 1200 DEG C of 1 8h of insulation under argon gas atmosphere in vacuum tube furnace with 18 DEG C/min speed, then through separating-purifying, you can obtain target product.Raw material used in the present invention is easy to get, and synthetic method is simple, and operating procedure controllability is high, and products obtained therefrom is purity height, uniform particle diameter, is relatively easy to expanding production；Meanwhile obtained nitrogen-doped porous carbon material is shown into excellent chemical property as lithium ion battery negative material.
Description
Technical field
The present invention relates to the preparation method that a kind of N doping improves carbon material, and use it for the negative pole material of lithium ion battery
Material, and in particular to a kind of preparation method of N doping porous carbon and its application on lithium ion battery.
Background technology
Lithium ion battery is widely used due to having the advantages that operating voltage is high, energy density is high, memory-less effect
In the small-sized movable electronics field such as video camera, mobile phone, notebook computer, and in the field such as electrokinetic cell and energy-storage battery
Also the development prospect to attract people's attention is shown.It is but fast with the aggravation of energy crisis and portable electric appts and Electric power car
Speed increases, and commercial Li-ion battery graphite cathode material can not meet the needs of people at present, it would be highly desirable to find a kind of improvement
The new method of carbon material performance.
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 lithium ion battery and ultracapacitor.Why very attractive N doping is,
Mainly there is the reason for following several respects：First, nitrogen-atoms is smaller than carbon atom, and electronegativity is strong, and nitrogen atom doping, which can strengthen, to be incorporated
Combination between miscellaneous carbon material and lithium, so as to be advantageous to the insertion of lithium ion；Second, by nitrogen be incorporated into graphite-like carbon structure (such as
CNT) in be a kind of effective ways to form n-type doping, it is possible to increase the electric conductivity of carbon material；Finally, N doping meeting
The defects of a large amount of is caused in carbon structure, these defects can provide more avtive spots for the storage of lithium.
Traditional N doping porous carbon preparation method mainly uses NH3, the post treatment method such as plasma or hydrazine is in carbon
Nitrogen-atoms is introduced in material.These methods are mostly more complicated, and mix nitrogen atom content it is limited, be difficult to realize uniformly,
It is controllable doped.Thus up to the present, the nitrogen-doped carbon material that chemical constituent uniformity is good, purity is high, microstructure is regular
There is not been reported for preparation method, and this constrains further applying for lithium cell negative pole material significantly.
The content of the invention
In view of the above-mentioned problems of the prior art, the present invention provides a kind of preparation method of N doping porous carbon, it is used
Raw material be easy to get, synthetic method is simple, and operating procedure controllability is high.Present invention also offers the N doping porous carbon in lithium ion
Application on battery.
To achieve these goals, the preparation method for a kind of N doping porous carbon that the present invention uses, is specifically included following
Step：
1) nitrogen source is dissolved in solvent and is configured to clear solution, and proper amount of carbon source is added in above-mentioned solution, formed fluffy
Flakes material, above-mentioned flakes material is placed in freeze drier and dries 1-10 hours；
2) compounding substances obtained after step 1) is dried are in vacuum tube furnace with 1-8 DEG C/min speed under argon gas atmosphere
Rate is warming up to 300-1200 DEG C of insulation 1-8h, then through separating-purifying, you can obtain target product.
As an improvement, the nitrogen source is water soluble salt of ammonia, selected from melamine, ammonium chloride, urea, ammonium hydrogen sulfate or nitric acid
Any of ammonium.
As an improvement, the solvent of the nitrogen source is selected from deionized water or ethanol.
As an improvement, the carbon source is any of high-hydroscopicity Sodium Polyacrylate, polyacrylic acid potassium, polyacrylic acid.
As an improvement, the separating-purifying in the step 2) is filtered using centrifugation or Buchner funnel, then it is anti-with deionized water
After backwashing is washed.
In addition, present invention also offers above-mentioned preparation method to be made application of the N doping porous carbon on lithium ion battery,
The N doping porous carbon is used for the negative pole of lithium ion battery, specifically includes following steps：
1) it is by weight X:(9-X):1 ratio weighs N doping porous carbon, conductive black and Kynoar respectively；
Kynoar and 1-METHYLPYRROLIDONE solution are made into the binder solution that concentration is 5%；System is added into ball grinder again
Binder solution, N doping porous carbon, the conductive black obtained, ball milling 2 hours, obtains pasty electrode slurry；
2) obtained electrode slurry is uniformly coated in copper foil current collector；
3) will be dried again in air dry oven of the electrode slice of coating sizing-agent at 50-70 DEG C, the electrode slice of acquisition according to
Predetermined size is cut, and after being suppressed with powder press, is placed in 120 DEG C of vacuum drying oven and is dried 12h, finally move into gloves
24h is placed in case to can be used.
As an improvement, the pressure of powder press is 15MPa in the step 3).
Compared with prior art, the beneficial effects of the invention are as follows：
1) nitrogen-doped porous carbon material has been prepared using the inventive method, raw material used is easy to get, and preparation method is simple,
It is easily operated, and products obtained therefrom purity is high, particle diameter distribution is narrower, regular appearance, is relatively easy to large-scale industrial production.
2) obtained N doping porous carbon is used for lithium ion battery negative material, shows excellent chemical property,
Both overcome commercial Li-ion battery with traditional carbon negative pole material specific capacity it is low the shortcomings that, but also with conventional transition metal oxygen
The excellent cycling stability that compound negative material does not possess, there is directive function to exploitation new type lithium ion battery.
Brief description of the drawings
Fig. 1 is the powder X-ray diffraction pattern that nitrogen-doped porous carbon material is made in the embodiment of the present invention, wherein vertical sit
Relative intensity (Intensity) is designated as, abscissa is angle of diffraction (2 θ)；
Fig. 2 is the electron scanning micrograph that N doping porous carbon is made in the embodiment of the present invention；
Fig. 3 is the charge and discharge cycles figure that nitrogen-doped porous carbon material is made in the embodiment of the present invention.
Embodiment
To make the object, technical solutions and advantages of the present invention of greater clarity, below by drawings and Examples, to this
Invention is further elaborated.However, it should be understood that the specific embodiments described herein are merely illustrative of the present invention,
The scope being not intended to limit the invention.
Unless otherwise defined, all technical terms and scientific terminology used herein are led with belonging to the technology of the present invention
The implication that the technical staff in domain is generally understood that is identical, and used term is intended merely to retouch in the description of the invention herein
State the purpose of specific embodiment, it is not intended that in the limitation present invention.
A kind of preparation method of N doping porous carbon, specifically includes following steps：
1) nitrogen source is dissolved in solvent and is configured to clear solution, and proper amount of carbon source is added in above-mentioned solution, formed fluffy
Flakes material, above-mentioned flakes material is placed in freeze drier and dries 1-10 hours；
2) compounding substances obtained after step 1) is dried are in vacuum tube furnace with 1-8 DEG C/min speed under argon gas atmosphere
Rate is warming up to 300-1200 DEG C of insulation 1-8h, then through separating-purifying, you can obtain target product.
As an improvement, the nitrogen source is water soluble salt of ammonia, selected from melamine (C3H6N6), ammonium chloride (NH4Cl), urea
(CO(NH2)2), ammonium hydrogen sulfate (NH4HSO4) or ammonium nitrate (NH4NO3Any of).
As an improvement, the solvent of the nitrogen source is selected from deionized water or ethanol.
As an improvement, the carbon source is any of high-hydroscopicity Sodium Polyacrylate, polyacrylic acid potassium, polyacrylic acid.
As an improvement, the separating-purifying in the step 2) is filtered using centrifugation or Buchner funnel, then it is anti-with deionized water
After backwashing is washed.
In addition, present invention also offers above-mentioned preparation method to be made application of the N doping porous carbon on lithium ion battery,
The N doping porous carbon is used for the negative pole of lithium ion battery, specifically includes following steps：
1) it is by weight X:(9-X):1 ratio weighs N doping porous carbon, conductive black and Kynoar respectively；
Kynoar and 1-METHYLPYRROLIDONE solution are made into the binder solution that concentration is 5%；System is added into ball grinder again
Binder solution, N doping porous carbon, the conductive black obtained, ball milling 2 hours, obtains pasty electrode slurry；
2) obtained electrode slurry is uniformly coated in copper foil current collector；
3) will be dried again in air dry oven of the electrode slice of coating sizing-agent at 50-70 DEG C, the electrode slice of acquisition according to
Predetermined size is cut, and with after powder press (operating pressure 15MPa) compacting, is placed in 120 DEG C of vacuum drying oven and is dried
Dry 12h, it is that can be used finally to move into glove box and place 24h.
Embodiment 1
A kind of preparation method of N doping porous carbon, specifically includes following steps：
1) 0.3g NH are taken4Cl is put into beaker and adds 1ml deionized waters, and sonic oscillation is configured to clear solution, gradually
1.2g high water solubles Sodium Polyacrylate is added in above-mentioned clear solution, is stirred by ultrasonic when adding；Finally it is slowly added to
Above-mentioned substance is transferred in freeze drier and dried 10 hours, obtain to more fluffy White snowflake shape material is formed by ionized water
White dried powder；
2) dry after the completion of, take appropriate powder be put in crucible and in vacuum tube furnace under argon gas atmosphere with 3 DEG C/min
Speed be warming up to 850 DEG C insulation 5h, the black product of generation washs repeatedly through deionized water, and is filtered, done with Buchner funnel
It is dry, obtain black powder product.
Product through German Brooker Bruker D8ADVANCE x-ray powder diffraction instruments with Cu K alpha rays ( Scanning leg speed is 0.08 °/sec) impalpable structure (as shown in Figure 1) of nitrogen-doped porous carbon material is accredited as, at 24 °
There is the diffraction maximum of wideization left and right, and (002) face of corresponding graphite structure, no other impurities peak occurs.
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 forms, and uniform in size, Size Distribution is narrower.
Electrochemical property test：
1) it is 7 by weight:2:1 ratio weighs N doping porous carbon, conductive black and Kynoar respectively；Will be poly-
Vinylidene is made into the binder solution that concentration is 5% with 1-METHYLPYRROLIDONE solution；Made from being added again into ball grinder
Binder solution, N doping porous carbon, conductive black, ball milling 2 hours, obtain pasty electrode slurry；
2) obtained electrode slurry is uniformly coated in copper foil current collector；
3) will be dried again in air dry oven of the electrode slice of coating sizing-agent at 60 DEG C, the electrode slice of acquisition is according to predetermined
Size cut, and with powder press (operating pressure 15MPa) compacting after, be placed in 120 DEG C of vacuum drying oven and dry
12h, it is that can be used finally to move into glove box and place 24h.
In the glove box full of argon gas, electrode slice, barrier film and lithium piece are assembled into button cell in conventional manner and gone forward side by side
Row constant current charge-discharge capacity and cycle performance test.Its chemical property is as shown in Figure 3.
Result of the test：Nitrogen-doped porous carbon material is under the current condition of 100 milliamperes/gram, and first and second of electric discharge is held
Amount is respectively 1068,679 MAhs/g, and capacity tends towards stability thereafter；When elevated currents successively to 200,500,1000,
2000 milliamperes/gram, its capacity are respectively 520,443,389,332 MAhs/g；When electric current recovers to 100 milliampere/gram conditions
Under, its capacity still be able to recover to 573 MAhs/g, and circulate 100 circle it is unattenuated, fully show high specific capacity and
Excellent high rate performance.
Embodiment 2
A kind of preparation method of N doping porous carbon, specifically includes following steps：
1) 0.3g NH are taken4Cl, which is put into beaker and adds 1ml deionized water sonic oscillations, is configured to clear solution, gradually
1.2g high water solubles polyacrylic acid potassium is added in above-mentioned clear solution, is stirred by ultrasonic when adding；Finally it is slowly added to
Above-mentioned substance is transferred in freeze drier and dried 10 hours, obtain to more fluffy White snowflake shape material is formed by ionized water
White dried powder；
2) dry after the completion of, take appropriate powder be put in crucible and in vacuum tube furnace under argon gas atmosphere with 3 DEG C/min
Speed be warming up to 650 DEG C insulation 5h, the black product of generation washs repeatedly through deionized water, and is filtered, done with Buchner funnel
It is dry to obtain black powder product.
Gained superfine powder is the disordering structure of N doping porous carbon, the nanometer that product is about 170nm by average grain diameter
Grain composition.
Electrochemical property test：
1) it is 5 by weight:4:1 ratio weighs N doping porous carbon, conductive black and Kynoar respectively；Will be poly-
Vinylidene is made into the binder solution that concentration is 5% with 1-METHYLPYRROLIDONE solution；Made from being added again into ball grinder
Binder solution, N doping porous carbon, conductive black, ball milling 2 hours, obtain pasty electrode slurry；
2) obtained electrode slurry is uniformly coated in copper foil current collector；
3) will be dried again in air dry oven of the electrode slice of coating sizing-agent at 70 DEG C, the electrode slice of acquisition is according to predetermined
Size cut, and with powder press (operating pressure 15MPa) compacting after, be placed in 120 DEG C of vacuum drying oven and dry
12h, it is that can be used finally to move into glove box and place 24h.
Embodiment 3
A kind of preparation method of N doping porous carbon, specifically includes following steps：
1) 0.5g CO (NH are taken2)2It is put into beaker and adds 1ml deionized water sonic oscillations and is configured to clear solution, by
Gradually 1g high water solubles polyacrylic acid is added in above-mentioned clear solution, is stirred by ultrasonic when adding；Finally be slowly added to from
Above-mentioned substance is transferred in freeze drier and dried 10 hours, obtain white to more fluffy White snowflake shape material is formed by sub- water
Color powdered substance；
2) dry after the completion of, take appropriate white powder in crucible and in vacuum tube furnace under argon gas atmosphere with 3 DEG C/
Min speed is warming up to 650 DEG C of insulation 5h, and the black product of generation washs repeatedly through deionized water, and filtered with Buchner funnel,
Dry black powder product.
Gained superfine powder is the disordering structure of nitrogen-doped porous carbon material, and product is about receiving for 200nm by average grain diameter
Rice grain forms.
Embodiment 4
A kind of preparation method of N doping porous carbon, specifically includes following steps：
1) 0.5g NH are taken4NO3It is put into beaker and adds the vibration of 1ml EtOH Sonicates and is configured to clear solution, will by gram
1.2g high water solubles Sodium Polyacrylate is added in above-mentioned clear solution, is stirred by ultrasonic when adding；Finally be slowly added to from
Above-mentioned substance is transferred in freeze drier and dried 3 hours, obtain white to more fluffy White snowflake shape material is formed by sub- water
Powdered substance；
2) dry after the completion of, take appropriate white powder in crucible and in vacuum tube furnace under argon gas atmosphere with 8 DEG C/
Min speed is warming up to 1000 DEG C of insulation 2h, and the black product of generation washs repeatedly through deionized water, and is taken out with Buchner funnel
Filter, dry black powder product.
Gained superfine powder is the disordering structure of nitrogen-doped porous carbon material, and product is about receiving for 180nm by average grain diameter
Rice grain forms.
Embodiment 5
A kind of preparation method of N doping porous carbon, specifically includes following steps：
1) 0.4g C are taken3H6N6It is put into beaker and adds the vibration of 1ml EtOH Sonicates and be configured to clear solution, by gram by 1g
High water soluble Sodium Polyacrylate is added in above-mentioned clear solution, is stirred by ultrasonic when adding；Finally it is slowly added to deionized water
To more fluffy White snowflake shape material is formed, above-mentioned substance is transferred in freeze drier and dried 6 hours, obtains white powder
Shape material；
2) dry after the completion of, take appropriate white powder in crucible and in vacuum tube furnace under argon gas atmosphere with 6 DEG C/
Min speed is warming up to 850 DEG C of insulation 5h, and the black product of generation washs repeatedly through deionized water, and filtered with Buchner funnel,
Dry black powder product.
Gained superfine powder is the disordering structure of nitrogen-doped porous carbon material, and product is about receiving for 200nm by average grain diameter
Rice grain forms.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
Any modification, equivalent substitution or improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (7)
1. a kind of preparation method of N doping porous carbon, it is characterised in that specifically include following steps：
1) nitrogen source is dissolved in solvent and is configured to clear solution, and proper amount of carbon source is added in above-mentioned solution, form fluffy snowflake
Shape material, above-mentioned flakes material is placed in freeze drier and dries 1-10 hours；
2) compounding substances obtained after step 1) is dried are in vacuum tube furnace with 1-8 DEG C/min speed liter under argon gas atmosphere
Warm to 300-1200 DEG C insulation 1-8h, then through separating-purifying, you can obtain target product.
2. the preparation method of a kind of N doping porous carbon according to claim 1, it is characterised in that the nitrogen source is water-soluble
Property ammonium salt, selected from any of melamine, ammonium chloride, urea, ammonium hydrogen sulfate or ammonium nitrate.
A kind of 3. preparation method of N doping porous carbon according to claim 2, it is characterised in that the solvent of the nitrogen source
Selected from deionized water or ethanol.
4. the preparation method of a kind of N doping porous carbon according to claim 1, it is characterised in that the carbon source is inhaled to be high
Any of aqueous polyacrylamide acid sodium, polyacrylic acid potassium, polyacrylic acid.
5. the preparation method of a kind of N doping porous carbon according to claim 1, it is characterised in that in the step 2)
Separating-purifying is filtered using centrifugation or Buchner funnel, then is washed repeatedly with deionized water.
6. application of the N doping porous carbon on lithium ion battery is made in a kind of any one of the claim 1-5 preparation method,
Characterized in that, the N doping porous carbon to be used for the negative pole of lithium ion battery, following steps are specifically included：
1) it is by weight X:(9-X):1 ratio weighs N doping porous carbon, conductive black and Kynoar respectively；Will be poly-
Vinylidene is made into the binder solution that concentration is 5% with 1-METHYLPYRROLIDONE solution；Made from being added again into ball grinder
Binder solution, N doping porous carbon, conductive black, ball milling 2 hours, obtain pasty electrode slurry；
2) obtained electrode slurry is uniformly coated in copper foil current collector；
3) will be dried again in air dry oven of the electrode slice of coating sizing-agent at 50-70 DEG C, the electrode slice of acquisition is according to predetermined
Size cut, and after being suppressed with powder press, be placed in 120 DEG C of vacuum drying oven and dry 12h, finally move into glove box
24h is placed to can be used.
A kind of 7. application of N doping porous carbon on lithium ion battery according to claim 6, it is characterised in that the step
It is rapid 3) in the pressure of powder press be 15MPa.
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