CN109742373A - A kind of preparation method of the band-like porous carbon of nitrogen-doped nanometer - Google Patents
A kind of preparation method of the band-like porous carbon of nitrogen-doped nanometer Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of the band-like porous carbon of nitrogen-doped nanometer, the preparation method is the following steps are included: polyaniline and nano strip phenolic resin based polyalcohol In-situ reaction, the preparation of the band-like porous carbon of nitrogen-doped nanometer, the band-like porous carbon of nitrogen-doped nanometer and elemental sulfur are compound, the band-like porous carbon of nitrogen-doped nanometer is mixed with elemental sulfur according to mass ratio for 2:3, it is uniform that dehydrated alcohol grinding is added, carbon tetrachloride is added to promote the dissolution of elemental sulfur, it is placed in baking oven and keeps the temperature after it is spontaneously dried, obtain the composite material of nitrogen-doped nanometer band-like porous carbon and sulphur.The present invention is after being carbonized and being activated by one-step method, and N doping porous carbon can effectively promote the chemisorption on carbon between oxygen-containing functional group and more lithium sulfides, which shows excellent cyclical stability.
Description
Technical field
The invention belongs to new energy materials and electrochemical field, and in particular to a kind of system of the band-like porous carbon of nitrogen-doped nanometer
Preparation Method.
Background technique
Information age is the world economy booming epoch, is the period that science power enhances energetically.With micro- electricity
The equipment of the fast development of sub- technology, miniaturization is increasing, proposes very high requirement to power supply.Lithium battery has energy close
Spend height, long service life, voltage rating height, quick charge, memory-less effect, it is light-weight, environmentally protective the advantages that.Therefore lithium electricity
Pond enters the large-scale practical stage therewith.Wherein, lithium-sulfur cell is with its theoretical energy density height (2600Wh/kg), cost
Low, the advantages that safety is good, it is considered to be very promising lithium battery.But lithium-sulfur cell is still in scientific research rank at this stage
Section, is that there is also three main problems because of lithium-sulfur cell: first, the poorly conductive of elemental sulfur, and the final product Li of reaction2S2
And Li2S is also electronic body, is unfavorable for the high rate capability of battery；Second, lithium polysulfide (Li2S2、Li2S6 Hes
Li2S4) it is soluble in electrolyte, generate shuttle effect, destructible electrolyte interface film (SEI film)；Third, sulphur is in charge and discharge process
In, there is up to 79% volume expansion/contraction, it is possible to lead to cell damage, nearly ten years, in order to improve asking for lithium-sulfur cell
Topic, researcher has conducted extensive research the modification of composite cathode material, most important one porous carbon because of its high conductivity,
High-specific surface area, high porosity, high chemistry and mechanical stability and easily prepared and greatly paid close attention to and studied.According to
Its structure, porous carbon are divided into one-dimensional material (such as carbon nanotube), two-dimensional material (such as graphene) and three-dimensional material (such as hollow carbon
Ball).In various porous carbons, multi-stage porous carbon material has obtained wider research in lithium-sulfur cell, because they have spy
Different pore-size distribution exists simultaneously micropore (<2nm), mesoporous (2-50nm) and macropore (>50nm).Therefore, multi-stage porous carbon material exists
The synergistic effect of multi-stage porous is shown in lithium-sulfur cell, this shows as micropore and provides anchor point for limiting polysulfide, in
Elementary sulfur is contained in hole, and macropore ensures excellent electrolyte-impregnated.Micro-, mesoporous physical adsorption characteristic can effectively improve lithium sulphur
The cyclical stability of battery.
Meanwhile exploitation has chemisorption sulphur or lithium sulfide (Li2S) the new type functional carbon material of ability is that especially have suction
Gravitation, chemisorption can make sulphur and Li2S is uniformly distributed on carbon, promotes good electrical contact, and can pass through
Prevent dissolution that effectively polysulfide is limited in anode, so as to effectively improve the cyclical stability of lithium-sulfur cell.
And traditional lithium-sulfur cell cyclical stability is undesirable, thus it is proposed that a kind of band-like porous carbon of nitrogen-doped nanometer
Preparation method.
Summary of the invention
The invention provides the following technical scheme: a kind of preparation method of the band-like porous carbon of nitrogen-doped nanometer, the preparation method
The following steps are included:
Step 1: polyaniline and nano strip phenolic resin based polyalcohol In-situ reaction, the monomer aniline of polyaniline is added
Enter the stirring and dissolving into 200mL citric acid solution, add nano strip phenolic resin based polyalcohol, stirring or ultrasound make its point
It dissipates uniformly, is then placed into 0 DEG C of environment and freezes 30 minutes, configured 40mL ammonium persulfate solution is then added, magnetic force stirs
Rear filtration drying is mixed, the compound of polyaniline Yu nano strip phenolic resin based polyalcohol, the composite polymeric finally obtained are obtained
In object, the mass ratio of polyaniline and nano strip phenolic resin based polyalcohol is between 1:2-1:5.
Step 2: the preparation of the band-like porous carbon of nitrogen-doped nanometer, above-mentioned polyaniline and nano strip phenolic resin base are gathered
The compound for closing object heats under an argon atmosphere, then passes to CO2Heat preservation 40 minutes forms the band-like porous carbon of nitrogen-doped nanometer.
Step 3: the band-like porous carbon of nitrogen-doped nanometer and elemental sulfur are compound, by the band-like porous carbon of above-mentioned nitrogen-doped nanometer with
Elemental sulfur is 2:3 mixing according to mass ratio, and the grinding of 2mL dehydrated alcohol is added uniformly, adds 1mL carbon tetrachloride to promote simple substance
The dissolution of sulphur keeps the temperature in the baking oven for being placed in 155 DEG C after it is spontaneously dried, obtains the band-like porous carbon of nitrogen-doped nanometer and sulphur
Composite material.
Preferably, the magnetic agitation time is 12 hours in step 1.
Preferably, in the preparation step of the band-like porous carbon of nitrogen-doped nanometer, by polyaniline and nano strip phenolic resin base
The compound of polymer is added to 950 DEG C under an argon atmosphere.
Preferably, the soaking time of the band-like porous carbon of the nitrogen-doped nanometer and baking oven in elemental sulfur recombination process is 12 small
When.
Compared with prior art, the beneficial effects of the present invention are:
1. the quasi- nano strip nanostructure and three-dimensional network-like structure using nano strip porous carbon of the present invention, by polyphenyl
Amine is compound with porous carbon, and the pattern of gained composite material is almost the same with the pattern of original porous carbon, and wherein porous carbon not only rises
It to the effect of conducting matrix grain and the more lithium sulfides of absorption, and is template, pattern directly determines the pattern of composite material, and
Polyaniline is to provide the raw material of nitrogen, and active site, the more lithium sulfides of efficient absorption, along with more are formed after high-temperature activation
Suction-operated of the hole carbon to more lithium sulfides can be effectively suppressed the dissolution of more lithium sulfides and improve the cyclical stability of lithium-sulfur cell.
2. polyaniline and nano strip phenolic resin based polyalcohol are carried out In-situ reaction by the present invention, since polyaniline is straight
It connected reaction to generate on the nanobelt of nano strip phenolic resin based polyalcohol, so being carbonized and activating by one-step method
Afterwards, nitrogen-atoms forms active site in the porous carbon surface of nano strip, obtains the band-like porous carbon of nitrogen-doped nanometer, and porous carbon rises and leads
Electricity and the effect for adsorbing more lithium sulfides, and N doping porous carbon can effectively promote on carbon between oxygen-containing functional group and more lithium sulfides
Chemisorption, which shows excellent cyclical stability.
Detailed description of the invention
Fig. 1 is scanning electron microscope (SEM) figure of the band-like porous carbon of nitrogen-doped nanometer prepared by the embodiment of the present invention two；
Fig. 2 is high magnification scanning electron microscope (SEM) figure of the band-like porous carbon of nitrogen-doped nanometer prepared by the embodiment of the present invention two；
Fig. 3 is the band-like porous carbon of nitrogen-doped nanometer/sulphur composite material high magnification scanning prepared by the embodiment of the present invention two
Electronic Speculum (SEM) figure；
Fig. 4 is the attached isothermal curve figure of adsorption/desorption of the band-like porous carbon of nitrogen-doped nanometer prepared by the embodiment of the present invention two；
Fig. 5 is the graph of pore diameter distribution of the band-like porous carbon of nitrogen-doped nanometer prepared by the embodiment of the present invention two；
Fig. 6 is the X-ray photoelectron spectroscopic analysis figure of the band-like porous carbon of nitrogen-doped nanometer prepared by the embodiment of the present invention two；
Fig. 7 is the cycle performance figure of lithium-sulfur cell prepared by the embodiment of the present invention two；
Fig. 8 is scanning electron microscope (SEM) figure of nano strip porous carbon prepared by comparative example one；
Fig. 9 is high magnification scanning electron microscope (SEM) figure of nano strip porous carbon prepared by comparative example one；
Figure 10 is nano strip porous carbon/sulphur composite material high magnification scanning electron microscope (SEM) figure prepared by comparative example one；
Figure 11 is the attached isothermal curve figure of adsorption/desorption of nano strip porous carbon prepared by comparative example one；
Figure 12 is the graph of pore diameter distribution of nano strip porous carbon prepared by comparative example one；
Figure 13 is the X-ray photoelectron spectroscopic analysis figure of nano strip porous carbon prepared by comparative example one；
Figure 14 is the cycle performance figure of lithium-sulfur cell prepared by comparative example one.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Embodiment one
1, polyaniline and nano strip phenolic resin based polyalcohol In-situ reaction: take 0.96g citric acid that water is added to be made into 200mL
1.86g aniline and 3.2g nano strip phenolic resin based polyalcohol is added in solution, and stirring or ultrasound make it be uniformly dispersed, then
It is placed in 0 DEG C of environment and freezes 30 minutes, add 4.56g ammonium persulfate and solution that 40g water is made into, magnetic agitation 12 hours
Filtration drying afterwards obtains composition polymer.In the composition polymer finally obtained, polyaniline polymerize with nano strip phenolic resin base
The mass ratio of object is 1:2.
2, above-mentioned polyaniline and nano strip phenolic resin based polyalcohol the preparation of the band-like porous carbon of nitrogen-doped nanometer: are taken
Compound 1.2g is heated to 950 DEG C under an argon atmosphere, then passes to CO2 and keeps the temperature 40 minutes, it is band-like more to obtain nitrogen-doped nanometer
Hole carbon.
3, the band-like porous carbon of nitrogen-doped nanometer and elemental sulfur are compound: the band-like porous carbon 0.08g of above-mentioned nitrogen-doped nanometer is taken, then
Elemental sulfur 0.12g is taken, the grinding of 2mL dehydrated alcohol is added after mixing uniformly, adds 1mL carbon tetrachloride to promote the molten of elemental sulfur
Solution is placed in 155 DEG C of baking oven after it is spontaneously dried and keeps the temperature 12 hours, obtains the band-like porous carbon of nitrogen-doped nanometer and sulphur
Composite material.
4, the electrochemical property test of lithium-sulfur cell: by gained positive electrode, binder (Kynoar), conductive agent
(acetylene black) is uniformly mixed according to mass ratio 80:10:10, and solvent (N-Methyl pyrrolidone) is added and is ground into uniform slurry,
It scratches on aluminium foil, disk of the dry backlash at diameter 15mm, tabletting is weighed after drying again, and being then assembled into specification is
The button battery of CR2016, wherein cathode is metal lithium sheet, and electrolyte is general lithium-sulfur cell electrolyte, charge-discharge test
Electric current is 0.167mA/g, and measuring its first discharge specific capacity is 1268mAh/g, first charge discharge efficiency 93%, specific volume after recycling 50 times
Amount is 926mAh/g.
Embodiment two
1, polyaniline and nano strip phenolic resin based polyalcohol In-situ reaction: take 0.64g citric acid that water is added to be made into 200mL
1.24g aniline and 3.2g nano strip phenolic resin based polyalcohol is added in solution, and stirring or ultrasound make it be uniformly dispersed, then
It is placed in 0 DEG C of environment and freezes 30 minutes, add 3.04g ammonium persulfate and solution that 40g water is made into, magnetic agitation 12 hours
Filtration drying afterwards obtains composition polymer.In the composition polymer finally obtained, polyaniline polymerize with nano strip phenolic resin base
The mass ratio of object is 1:3.
2, above-mentioned polyaniline and nano strip phenolic resin based polyalcohol the preparation of the band-like porous carbon of nitrogen-doped nanometer: are taken
Compound 1.2g is heated to 950 DEG C under an argon atmosphere, then passes to CO2 and keeps the temperature 40 minutes, it is band-like more to obtain nitrogen-doped nanometer
Hole carbon.
3, the band-like porous carbon of nitrogen-doped nanometer and elemental sulfur are compound: the band-like porous carbon 0.08g of above-mentioned nitrogen-doped nanometer is taken, then
Elemental sulfur 0.12g is taken, the grinding of 2mL dehydrated alcohol is added after mixing uniformly, adds 1mL carbon tetrachloride to promote the molten of elemental sulfur
Solution is placed in 155 DEG C of baking oven after it is spontaneously dried and keeps the temperature 12 hours, obtains the band-like porous carbon of nitrogen-doped nanometer and sulphur
Composite material.
4, the electrochemical property test of lithium-sulfur cell: by gained positive electrode, binder (Kynoar), conductive agent
(acetylene black) is uniformly mixed according to mass ratio 80:10:10, and solvent (N-Methyl pyrrolidone) is added and is ground into uniform slurry,
It scratches on aluminium foil, disk of the dry backlash at diameter 15mm, tabletting is weighed after drying again, and being then assembled into specification is
The button battery of CR2016, wherein cathode is metal lithium sheet, and electrolyte is general lithium-sulfur cell electrolyte, charge-discharge test
Electric current is 0.167mA/g, and measuring its first discharge specific capacity is 1359mAh/g, first charge discharge efficiency 91%, specific volume after recycling 50 times
Amount is 978mAh/g.
Embodiment three
1, polyaniline and nano strip phenolic resin based polyalcohol In-situ reaction: take 0.48g citric acid that water is added to be made into 200mL
1.488g aniline and 3.2g nano strip phenolic resin based polyalcohol is added in solution, and stirring or ultrasound make it be uniformly dispersed, then
It is placed in 0 DEG C of environment and freezes 30 minutes, add 2.28g ammonium persulfate and solution that 40g water is made into, magnetic agitation 12 hours
Filtration drying afterwards obtains composition polymer.In the composition polymer finally obtained, polyaniline polymerize with nano strip phenolic resin base
The mass ratio of object is 1:4.
2, above-mentioned polyaniline and nano strip phenolic resin based polyalcohol the preparation of the band-like porous carbon of nitrogen-doped nanometer: are taken
Compound 1.2g is heated to 950 DEG C under an argon atmosphere, then passes to CO2 and keeps the temperature 40 minutes, it is band-like more to form nitrogen-doped nanometer
Hole carbon.
3, the band-like porous carbon of nitrogen-doped nanometer and elemental sulfur are compound: the band-like porous carbon 0.08g of above-mentioned nitrogen-doped nanometer is taken, then
Elemental sulfur 0.12g is taken, the grinding of 2mL dehydrated alcohol is added after mixing uniformly, adds 1mL carbon tetrachloride to promote the molten of elemental sulfur
Solution is placed in 155 DEG C of baking oven after it is spontaneously dried and keeps the temperature 12 hours, obtains the band-like porous carbon of nitrogen-doped nanometer and sulphur
Composite material.
4, the electrochemical property test of lithium-sulfur cell: by gained positive electrode, binder (Kynoar), conductive agent
(acetylene black) is uniformly mixed according to mass ratio 80:10:10, and solvent (N-Methyl pyrrolidone) is added and is ground into uniform slurry,
It scratches on aluminium foil, disk of the dry backlash at diameter 15mm, tabletting is weighed after drying again, and being then assembled into specification is
The button battery of CR2016, wherein cathode is metal lithium sheet, and electrolyte is general lithium-sulfur cell electrolyte, charge-discharge test
Electric current is 0.167mA/g, and measuring its first discharge specific capacity is 1257mAh/g, first charge discharge efficiency 91%, specific volume after recycling 50 times
Amount is 931mAh/g.
Example IV
1, polyaniline and nano strip phenolic resin based polyalcohol In-situ reaction: take 0.384g citric acid that water is added to be made into
200mL solution, is added 0.744g aniline and 3.2g nano strip phenolic resin based polyalcohol, and stirring or ultrasound keep its dispersion equal
It is even, it is then placed into 0 DEG C of environment and freezes 30 minutes, add the solution that 1.824g ammonium persulfate and 40g water are made into, magnetic force stirs
Filtration drying after mixing 12 hours, obtains composition polymer.In the composition polymer finally obtained, polyaniline and nano strip phenolic aldehyde tree
The mass ratio of aliphatic radical polymer is 1:5.
2, above-mentioned polyaniline and nano strip phenolic resin based polyalcohol the preparation of the band-like porous carbon of nitrogen-doped nanometer: are taken
Compound 1.2g is heated to 950 DEG C under an argon atmosphere, then passes to CO2 and keeps the temperature 40 minutes, it is band-like more to obtain nitrogen-doped nanometer
Hole carbon.
3, the band-like porous carbon of nitrogen-doped nanometer and elemental sulfur are compound: the band-like porous carbon 0.08g of above-mentioned nitrogen-doped nanometer is taken, then
Elemental sulfur 0.12g is taken, the grinding of 2mL dehydrated alcohol is added after mixing uniformly, adds 1mL carbon tetrachloride to promote the molten of elemental sulfur
Solution is placed in 155 DEG C of baking oven after it is spontaneously dried and keeps the temperature 12 hours, obtains the band-like porous carbon of nitrogen-doped nanometer and sulphur
Composite material.
4, the electrochemical property test of lithium-sulfur cell: by gained positive electrode, binder (Kynoar), conductive agent
(acetylene black) is uniformly mixed according to mass ratio 80:10:10, and solvent (N-Methyl pyrrolidone) is added and is ground into uniform slurry,
It scratches on aluminium foil, disk of the dry backlash at diameter 15mm, tabletting is weighed after drying again, and being then assembled into specification is
The button battery of CR2016, wherein cathode is metal lithium sheet, and electrolyte is general lithium-sulfur cell electrolyte, charge-discharge test
Electric current is 0.167mA/g, and measuring its first discharge specific capacity is 1266mAh/g, first charge discharge efficiency 93%, specific volume after recycling 50 times
Amount is 938mAh/g.
Comparative example one
1, the preparation of nano strip phenolic resin based polyalcohol: by 1.65g hydroquinone, 37% formalin of 2.5mL and
10% hydrochloric acid of 110mL is sufficiently mixed in the 200mL polytetrafluoroethyllining lining of autoclave, simultaneously by autoclave sealing
It is placed in 180 DEG C of baking ovens and keeps the temperature 12 hours, it is 6-7 that products therefrom, which is filtered, and is washed to pH, then is placed in 110 DEG C of oven dryings 12
Hour obtains 2g phenolic resin base nano strip polymer.
2, the preparation of nano strip porous carbon: take the compound 1.2g of above-mentioned nano strip phenolic resin based polyalcohol in argon
It is heated to 950 DEG C under gas atmosphere, then passes to CO2 and keeps the temperature 40 minutes, obtain nano strip porous carbon.
3, nano strip porous carbon and elemental sulfur are compound: taking above-mentioned nano strip porous carbon 0.08g, then take elemental sulfur
0.12g is added the grinding of 2mL dehydrated alcohol uniformly, adds 1mL carbon tetrachloride to promote the dissolution of elemental sulfur, to it after mixing
It is placed in after natural drying in 155 DEG C of baking oven and keeps the temperature 12 hours, obtain the composite material of nano strip porous carbon and sulphur.
4, the electrochemical property test of lithium-sulfur cell: by gained positive electrode, binder (Kynoar), conductive agent
(acetylene black) is uniformly mixed according to mass ratio 80:10:10, and solvent (N-Methyl pyrrolidone) is added and is ground into uniform slurry,
It scratches on aluminium foil, disk of the dry backlash at diameter 15mm, tabletting is weighed after drying again, and being then assembled into specification is
The button battery of CR2016, wherein cathode is metal lithium sheet, and electrolyte is general lithium-sulfur cell electrolyte, charge-discharge test
Electric current is 0.167mA/g, and measuring its first discharge specific capacity is 1371mAh/g, first charge discharge efficiency 89%, specific volume after recycling 50 times
Amount is 801mAh/g.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (4)
1. a kind of preparation method of the band-like porous carbon of nitrogen-doped nanometer, which is characterized in that the preparation method the following steps are included:
Step 1: polyaniline and nano strip phenolic resin based polyalcohol In-situ reaction, the monomer aniline of polyaniline is added to
Stirring and dissolving in 200mL citric acid solution, adds nano strip phenolic resin based polyalcohol, and stirring or ultrasound keep its dispersion equal
It is even, it is then placed into 0 DEG C of environment and freezes 30 minutes, be then added configured 40mL ammonium persulfate solution, after magnetic agitation
Filtration drying, obtains the compound of polyaniline Yu nano strip phenolic resin based polyalcohol, in the composition polymer finally obtained,
The mass ratio of polyaniline and nano strip phenolic resin based polyalcohol is between 1:2-1:5.
Step 2: the preparation of the band-like porous carbon of nitrogen-doped nanometer, by above-mentioned polyaniline and nano strip phenolic resin based polyalcohol
Compound heat under an argon atmosphere, then pass to CO2Heat preservation 40 minutes forms the band-like porous carbon of nitrogen-doped nanometer.
Step 3: the band-like porous carbon of nitrogen-doped nanometer and elemental sulfur are compound, by the band-like porous carbon of above-mentioned nitrogen-doped nanometer and simple substance
Sulphur is 2:3 mixing according to mass ratio, and the grinding of 2mL dehydrated alcohol is added uniformly, adds 1mL carbon tetrachloride to promote elemental sulfur
Dissolution keeps the temperature in the baking oven for being placed in 155 DEG C after it is spontaneously dried, obtains the compound of the band-like porous carbon of nitrogen-doped nanometer and sulphur
Material.
2. a kind of preparation method of the band-like porous carbon of nitrogen-doped nanometer according to claim 1, it is characterised in that: step 1
The middle magnetic agitation time is 12 hours.
3. a kind of preparation method of the band-like porous carbon of nitrogen-doped nanometer according to claim 1, it is characterised in that: N doping
In the preparation step of nano strip porous carbon, by the compound of polyaniline and nano strip phenolic resin based polyalcohol in argon gas gas
950 DEG C are added under atmosphere.
4. a kind of preparation method of the band-like porous carbon of nitrogen-doped nanometer according to claim 1, it is characterised in that: the nitrogen
The soaking time of baking oven is 12 hours in the band-like porous carbon of dopen Nano and elemental sulfur recombination process.
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Application publication date: 20190510 |