CN106744802B - Compound duct carbon material of the one-dimensional micropore-macropore of biology base and preparation method thereof - Google Patents
Compound duct carbon material of the one-dimensional micropore-macropore of biology base and preparation method thereof Download PDFInfo
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Abstract
The compound duct carbon material of the one-dimensional micropore-macropore of biology base of the invention belongs to supercapacitor technologies field, the microscopic appearance of the compound duct carbon material of the one-dimensional micropore-macropore of biology base is tubulose, states the compound duct carbon material of the one-dimensional micropore-macropore of biology base and is made of agraphitic carbon and graphitized carbon;The preparation method of the compound duct carbon material of the one-dimensional micropore-macropore of biology base is that trailing plants Japonica progress carbonization-activation is obtained one-dimensional micropore-macropore compound pore passage structure carbon material.The compound duct carbon material of the one-dimensional micropore-macropore of biology base of the invention achieves that treatment process is simple and convenient, and raw material green is cheap and easy to get, environmentally friendly, the good beneficial effect of chemical property.The compound duct carbon material of the one-dimensional micropore-macropore of gained biology base has huge potentiality application in terms of super capacitor material.
Description
Technical field
The present invention relates to super capacitor material technical fields, and in particular to a kind of one-dimensional micropore-macropore of biology base is compound
Duct carbon material and preparation method thereof.
Background technique
With the development of mankind's science and technology, more and more instrument and equipments need portable energy storage device, as wind-driven generator,
Mobile phone, laptop, unmanned plane and lithium battery automobile etc..Supercapacitor not only has the specific surface area, extra small of super large
Charge gap and itself do not occur chemical reaction etc. features, also have better than other energy storage devices advantage: (1) charging rate
Fastly, charging 10 seconds~10 minutes can achieve 95% of its rated capacity or more;(2) service life cycle is long, depth charge and discharge
Number is recycled up to 1~500,000 times;(3) energy conversion efficiency is high, and process losses are small, and high current energy circulation efficiency >=
90%;(4) power density is high, up to 300W/kg~5000W/kg, is equivalent to 5~10 times of battery;(5) product raw material structure
It is not polluted at, production, use, storage and dismantling process, is ideal environmentally protective power supply;(6) safety coefficient is high, makes for a long time
With can be non-maintaining;(7) easy to detect, remaining capacity can directly be read.Currently, the predecessor of preparation supercapacitor has polypyrrole
(European Polymer Journal.2013,49,3651-3656), graphene oxide (Nanoscale Research
) and MnO Letters.2014,9,535-5452(ACS Appl.Mater.Interfaces,2014 6(13),10506-
10515) etc., these methods are cumbersome, higher cost.And in terms of biomass carbonization, one-dimensional carbon material product report compared with
Few, pattern is destroyed most of biomass after treatment, and one-dimensional microstructure is conducive to the transmission diffusion of charge.Separately
Outside, from environmental protection from the point of view of cost, it is desired to prepare predecessor used in product is low in cost, preferably waste benefit
With.Therefore, it is suitable to find pattern, low-cost biomass material, by simply handling the good electrochemistry of processability
Material is of great significance.
Summary of the invention
The technical problem to be solved by the present invention is to biomass carbonization material feedstock is at high cost.To solve this problem, this hair
It is bright to provide a kind of compound duct carbon material of one-dimensional micropore-macropore of biology base, while it is big to provide the one-dimensional micropore-of the biology base
The preparation method of the compound duct carbon material in hole.The technical solution adopted by the present invention is that the one-dimensional micropore-macropore of biology base is compound
Duct carbon material is made of agraphitic carbon and graphitized carbon;The system of the compound duct carbon material of the one-dimensional micropore-macropore of biology base
Preparation Method is that trailing plants Japonica progress carbonization-activation is obtained one-dimensional micropore-macropore compound pore passage structure carbon material.
The specific technical solution that the present invention uses is the compound duct carbon material of a kind of one-dimensional micropore-macropore of biology base, by nothing
Sizing carbon and graphitized carbon composition, characterized in that the compound duct carbon material of the one-dimensional micropore-macropore of biology base is one-dimensional tubulose
Structure, length are 100~300 μm, and about 2~8 μm of caliber, 0.2~0.5 μm of thickness of pipe wall, there are a large amount of micropores in tube wall;Wherein without
The mass ratio of sizing carbon and graphitized carbon is about 3.5~4.5:1.
The preparation method of the compound duct carbon material of the one-dimensional micropore-macropore of biology base, synthesis process are as follows:
Trailing plants Japonica is peeled off deseeding, obtains trailing plants Japonica silk within dry 12~24 hours in 100~140 DEG C after being washed with deionized water;
Under nitrogen protection, trailing plants Japonica silk is carbonized 0.5~3 hour in 500~700 DEG C, obtains carbonization trailing plants Japonica silk;Carbonization trailing plants Japonica silk is set
In the distilled water dissolved with sodium hydroxide, heated 1~5 hour in 100~140 DEG C, in 100~140 after being washed with deionized
DEG C dry 12~24 hours, obtain the carbonization trailing plants Japonica silk without metallic element, the mistake recycled to avoid metallic element in electrochemistry
The unstable of material is caused in journey;The mass ratio of carbonization trailing plants Japonica silk, sodium hydroxide and water is 1:4~30:200~400;
Carbonization trailing plants Japonica silk without metallic element is immersed and is stirred 30~90 minutes dissolved in the distilled water of potassium hydroxide, is taken out
Filter obtains the carbonization trailing plants Japonica silk of load potassium hydroxide in 100~140 DEG C to drying 12~24 hours;Under nitrogen protection, will
The carbonization trailing plants Japonica silk for loading potassium hydroxide activates 0.5~2 hour in 600~1000 DEG C;In 100~140 DEG C after being washed with boiling water
It is 12~24 hours dry, obtain the compound duct carbon material of one-dimensional micropore-macropore;Wherein without metallic element carbonization trailing plants Japonica silk,
The mass ratio of potassium hydroxide and water is 1:4~8:200~600.
The compound duct carbon material of the one-dimensional micropore-macropore of biology base of the invention, microscopic appearance are tubulose, and length is 100 μ
M~300 μm, about 2~8 μm of caliber, 0.2~0.5 μm of thickness of pipe wall, 1385~1395m of specific surface area2/ g, capacitance reaches 245~
265F/g, equivalent series resistance only have 0.16~0.18 Ω;By controlling the pattern of product, make that there is good charge-transporting
Can, there is huge potentiality application in terms of super capacitor material.It is one-dimensional micro- prepared by the present invention for the prior art
The compound duct carbon material of hole-macropore, synthetic method is simple, and morphology controllable, synthesis cycle is short, and capacitance is higher and equivalent series
Resistance very little, low in cost, raw material is easy to get, green non-pollution.Experimentation only needs to calcine twice, centre potassium hydroxide solution
It impregnates, final product can be obtained.The one-dimensional micropore of biology base-macropore compound pore passage structure carbon material, on the one hand can provide compared with
Big specific surface area allows a large amount of charge to be attached to the surfaces externally and internally of carbon material, thus reach biggish capacitance, another aspect one
Structure of dimension itself is good charge transmission bridge again, is conducive to the quick transmission of charge, be greatly reduced material etc.
Imitate series resistance.Entire technical process is simple, and at low cost, effect is good, and waste utilization is environmentally protective, is conducive to industrialization production.
Detailed description of the invention
The untreated optical photograph of Fig. 1 trailing plants Japonica (A) and transmission electron microscope photo (B).
The scanning electricity of the different amplification of the compound duct carbon material 1 of the one-dimensional micropore-macropore of the biology base of Fig. 2 embodiment 1
Sub- microscope photo.
The nitrogen adsorption curve of the compound duct carbon material 1 of the one-dimensional micropore-macropore of the biology base of Fig. 3 embodiment 1.
The pore size distribution curve of the compound duct carbon material 1 of the one-dimensional micropore-macropore of the biology base of Fig. 4 embodiment 1.
The cyclic voltammetry curve of the compound duct carbon material 1 of the one-dimensional micropore-macropore of the biology base of Fig. 5 embodiment 1.
The impedance curve of the compound duct carbon material 1 of the one-dimensional micropore-macropore of the biology base of Fig. 6 embodiment 1.
The Raman curve of the compound duct carbon material 1 of the one-dimensional micropore-macropore of the biology base of Fig. 7 embodiment 1.
Specific embodiment
The present invention is illustrated with specific embodiment below, purpose, which is only that, to be best understood from the contents of the present invention rather than limit
Protection scope of the present invention.
Embodiment 1
Trailing plants Japonica is peeled off deseeding, obtains trailing plants Japonica silk within dry 12 hours in 100 DEG C after being washed with deionized water;In nitrogen protection
Under, 500mg trailing plants Japonica silk is carbonized 0.5 hour in 500 DEG C, obtains 250mg carbonization trailing plants Japonica silk;250mg carbonization trailing plants Japonica silk is placed in
Dissolved in the 100g distilled water of 1g sodium hydroxide, heated 1 hour in 100 DEG C, it is small in 100 DEG C of dryings 12 after being washed with deionized
When, the carbonization trailing plants Japonica silk that 250mg is free of metallic element is obtained, causes material during electrochemistry recycles to avoid metallic element
That expects is unstable;
Carbonization trailing plants Japonica silk by 250mg without metallic element is immersed dissolved with 50g stirring 0.5 in the distilled water of 1g potassium hydroxide
Hour, it filters, it is 12 hours dry in 100 DEG C, obtain the carbonization trailing plants Japonica silk of 120mg load potassium hydroxide;Under nitrogen protection, will
The carbonization trailing plants Japonica silk that 120mg loads potassium hydroxide activates 0.5 hour in 800 DEG C;It is small in 120 DEG C of dryings 24 after being washed with boiling water
When, obtain the compound duct carbon material 1 of one-dimensional micropore-macropore.
Fig. 1 (A) provides the optical photograph of untreated trailing plants Japonica, and trailing plants Japonica has a shell, and surface splits and internal has very thin hair
Silk leaks out, and a sheet seed is arranged at the bottom of every Shu Maosi, and Fig. 1 (B) is that the transmission electron microscope of untreated trailing plants Japonica silk shines
Piece, it is seen then that trailing plants Japonica silk be tubular structure, 29 μm of outer diameter, 25 μm of internal diameter, 2 μm of tube wall.
Fig. 2 is the electron scanning micrograph of the compound duct carbon material 1 of the one-dimensional micropore-macropore of biology base of embodiment 1.
From Figure 2 it can be seen that the compound duct carbon material 1 of the one-dimensional micropore-macropore of 1 gained biology base of embodiment is one-dimensional tubular structure, compared to not
The material of processing has an apparent contraction, and about 4 μm of caliber, thickness of pipe wall about 250nm, 100 μm of length;It is one-dimensional micro- that Fig. 3 provides biology base
The nitrogen adsorption curve of the compound duct carbon material 1 of hole-macropore, is I type adsorption curve, and specific surface area (BET) is 1394m2/g.Figure
4 provide the pore-size distribution of the compound duct carbon material 1 of the one-dimensional micropore-macropore of biology base, from fig. 4, it can be seen that duct contained by material is main
For micropore, also there is an apparent peak in big porose area.Fig. 5 provides following for the one-dimensional compound duct carbon material 1 of micropore-macropore of biology base
Ring volt-ampere curve is typical electric double layer capacitance cyclic voltammetry curve, is 265F/ according to the capacitance that product is calculated in Fig. 5
g.Fig. 6 provides the impedance curve of the compound duct carbon material 1 of the one-dimensional micropore-macropore of biology base, and the radius of the semicircle of high frequency region indicates
Charge transfer resistance, the slope of the straight line of low frequency range represent electrolyte diffusion resistance, and it is one-dimensional micro- that biology base is calculated according to Fig. 6
The equivalent series resistance of the compound duct carbon material 1 of hole-macropore is 0.16 Ω;Fig. 7 provides the one-dimensional micropore of biology base-macropore composite holes
The Raman spectrum of road carbon material 1, primitive curve can be divided into D band and G band, wherein D band represents agraphitic carbon in material, G band generation
Graphitized carbon in table material, is fitted by swarming, and the ratio that can calculate agraphitic carbon and graphitized carbon is 64:18.
According to result above it was determined that the compound duct carbon material 1 of the one-dimensional micropore-macropore of biology base is one-dimensional tubulose knot
Structure, length are 100 μm, 4 μm of caliber, 0.25 μm of thickness of pipe wall;Wherein the mass ratio of agraphitic carbon and graphitized carbon is about 64:18.
Embodiment 2
Trailing plants Japonica is peeled off deseeding, obtains trailing plants Japonica silk within dry 24 hours in 120 DEG C after being washed with deionized water;In nitrogen protection
Under, 500mg trailing plants Japonica silk is carbonized 1 hour in 600 DEG C, obtains 250mg carbonization trailing plants Japonica silk;250mg carbonization trailing plants Japonica silk is placed in molten
Have in the 50mL distilled water of 2.5g sodium hydroxide, is heated 5 hours in 120 DEG C, it is small in 120 DEG C of dryings 24 after being washed with deionized
When, the carbonization trailing plants Japonica silk that 250mg is free of metallic element is obtained, causes material during electrochemistry recycles to avoid metallic element
That expects is unstable;
Carbonization trailing plants Japonica silk immersion by 250mg without metallic element in the 100mL distilled water of 2g potassium hydroxide dissolved with stirring
60 minutes;It filters, it is 24 hours dry in 120 DEG C, obtain the carbonization trailing plants Japonica silk of 120mg load potassium hydroxide;Under nitrogen protection,
The carbonization trailing plants Japonica silk of 120mg load potassium hydroxide is activated 1 hour in 600 DEG C;It is small in 100 DEG C of dryings 12 after being washed with boiling water
When, obtain the compound duct carbon material 2 of the one-dimensional micropore-macropore of biology base.
The compound duct carbon material 2 of the one-dimensional micropore-macropore of 2 gained biology base of embodiment is one-dimensional tubular structure compared to untreated
Material have an apparent contraction, about 2 μm of caliber, about 0.230 μm of thickness of pipe wall, 200 μm of length;One-dimensional micropore-the macropore of biology base is multiple
The nitrogen adsorption curve for closing duct carbon material 1 is similar with Fig. 3, is I type adsorption curve, and specific surface area (BET) is 1385m2/g;It is raw
The pore-size distribution of the compound duct carbon material 2 of the one-dimensional micropore-macropore of object base is similar with Fig. 4, and duct contained by material is mainly micropore,
Big porose area also has an apparent peak.The cyclic voltammetry curve and Fig. 5 of the compound duct carbon material 2 of the one-dimensional micropore-macropore of biology base
It is similar, it is typical electric double layer capacitance cyclic voltammetry curve, the capacitance that product is calculated is 255F/g;Biology base is one-dimensional micro-
The impedance curve of the compound duct carbon material 2 of hole-macropore is similar with Fig. 6, and the radius of the semicircle of high frequency region indicates charge transfer resistance,
The slope of the straight line of low frequency range represents electrolyte diffusion resistance, and the compound duct carbon materials of the one-dimensional micropore-macropore of biology base are calculated
The equivalent series resistance of material 2 is 0.17 Ω;The Raman spectrum and Fig. 7 class of the compound duct carbon material 2 of the one-dimensional micropore-macropore of biology base
Seemingly, primitive curve can be divided into D band and G band, wherein and D band represents agraphitic carbon in material, and G band represents graphitized carbon in material,
It is fitted by swarming, the ratio that can calculate agraphitic carbon and graphitized carbon is about 62:15.
According to result above it was determined that the compound duct carbon material 1 of the one-dimensional micropore-macropore of biology base is one-dimensional tubulose knot
Structure, length are 200 μm, and caliber is 2 μm, 0.23 μm of thickness of pipe wall;Wherein the mass ratio of agraphitic carbon and graphitized carbon is about 62:
15。
Embodiment 3
Trailing plants Japonica is peeled off deseeding, obtains trailing plants Japonica silk within dry 18 hours in 140 DEG C after being washed with deionized water;In nitrogen protection
Under, 500mg trailing plants Japonica silk is carbonized 3 hours in 700 DEG C, obtains 250mg carbonization trailing plants Japonica silk;250mg carbonization trailing plants Japonica silk is placed in molten
Have in the 75mL distilled water of 7.5g sodium hydroxide, is heated 3 hours in 140 DEG C, it is small in 140 DEG C of dryings 18 after being washed with deionized
When, the carbonization trailing plants Japonica silk that 250mg is free of metallic element is obtained, causes material during electrochemistry recycles to avoid metallic element
That expects is unstable;
Carbonization trailing plants Japonica silk immersion by 250mg without metallic element in the 150mL distilled water of 1.5g potassium hydroxide dissolved with stirring
It mixes 90 minutes, filters, it is 18 hours dry in 140 DEG C, obtain the carbonization trailing plants Japonica silk of 120mg load potassium hydroxide;In nitrogen protection
Under, the carbonization trailing plants Japonica silk of 120mg load potassium hydroxide is activated 2 hours in 1000 DEG C;In 140 DEG C dry 18 after being washed with boiling water
Hour, obtain the compound duct carbon material 3 of one-dimensional micropore-macropore.
The electron scanning micrograph and Fig. 2 of the compound duct carbon material 3 of the one-dimensional micropore-macropore of the biology base of embodiment 3
Similar, the compound duct carbon material 3 of the one-dimensional micropore-macropore of 3 gained biology base of embodiment is one-dimensional tubular structure compared to untreated
Material has an apparent contraction, and about 8 μm of caliber, about 0.450 μm of thickness of pipe wall, 300 μm of length;One-dimensional micropore-the macropore of biology base is compound
The nitrogen adsorption curve of duct carbon material 3 is similar with Fig. 3, is I type adsorption curve, and specific surface area (BET) is 1395m2/g;Biology
The pore-size distribution of the compound duct carbon material 3 of the one-dimensional micropore-macropore of base is similar with Fig. 4, and duct contained by material is mainly micropore, big
Porose area also has an apparent peak.The cyclic voltammetry curve and Fig. 5 class of the compound duct carbon material 3 of the one-dimensional micropore-macropore of biology base
It seemingly, is typical electric double layer capacitance cyclic voltammetry curve, the capacitance that product is calculated is 245F/g;Biology base is one-dimensional micro-
The impedance curve of the compound duct carbon material 3 of hole-macropore is similar with Fig. 6, and the radius of the semicircle of high frequency region indicates charge transfer resistance,
The slope of the straight line of low frequency range represents electrolyte diffusion resistance, and the compound duct carbon materials of the one-dimensional micropore-macropore of biology base are calculated
The equivalent series resistance of material 1 is 0.18 Ω;The Raman spectrum and Fig. 7 class of the compound duct carbon material 1 of the one-dimensional micropore-macropore of biology base
Seemingly, primitive curve can be divided into D band and G band, wherein and D band represents agraphitic carbon in material, and G band represents graphitized carbon in material,
It is fitted by swarming, the ratio that can calculate agraphitic carbon and graphitized carbon is about 64:17.
According to result above it was determined that the compound duct carbon material 1 of the one-dimensional micropore-macropore of biology base is one-dimensional tubulose knot
Structure, length are 300 μm, and caliber is 8 μm, 0.45 μm of thickness of pipe wall;Wherein the mass ratio of agraphitic carbon and graphitized carbon is about 64:
17。
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
Specific implementation of the invention is only limited to these instructions.It for those of ordinary skill in the art, can be according to the present invention
Technical solution and inventive concept, make it is corresponding change and substitution, and performance or use is identical, all should be considered as of the invention
Protection scope.
Claims (2)
1. a kind of compound duct carbon material of one-dimensional micropore-macropore of biology base, is made of, feature agraphitic carbon and graphitized carbon
It is that the compound duct carbon material of the one-dimensional micropore-macropore of biology base is one-dimensional tubular structure, length is 100~300 μm, caliber
It is 2~8 μm, 0.2~0.5 μm of thickness of pipe wall, there are a large amount of micropores in tube wall;Wherein the mass ratio of agraphitic carbon and graphitized carbon is
3.5~4.5:1.
2. a kind of preparation method of the compound duct carbon material of one-dimensional micropore-macropore of the biology base of claim 1, synthesis process is such as
Under:
Trailing plants Japonica is peeled off deseeding, obtains trailing plants Japonica silk within dry 12~24 hours in 100~140 DEG C after being washed with deionized water;In nitrogen
Under gas shielded, trailing plants Japonica silk is carbonized 0.5~3 hour in 500~700 DEG C, obtains carbonization trailing plants Japonica silk;Carbonization trailing plants Japonica silk is placed in molten
Have in the distilled water of sodium hydroxide, is heated 1~5 hour in 100~140 DEG C, it is dry in 100~140 DEG C after being washed with deionized
Dry 12~24 hours, the carbonization trailing plants Japonica silk without metallic element is obtained, to avoid metallic element during electrochemistry recycles
Cause the unstable of material;The mass ratio of carbonization trailing plants Japonica silk, sodium hydroxide and water is 1:4~30:200~400;
Carbonization trailing plants Japonica silk without metallic element is immersed and is stirred 30~90 minutes dissolved in the distilled water of potassium hydroxide, is filtered,
In 100~140 DEG C to drying 12~24 hours, the carbonization trailing plants Japonica silk of load potassium hydroxide is obtained;Under nitrogen protection, it will load
The carbonization trailing plants Japonica silk of potassium hydroxide activates 0.5~2 hour in 600~1000 DEG C;In 100~140 DEG C of dryings after being washed with boiling water
12~24 hours, obtain the compound duct carbon material of one-dimensional micropore-macropore;Wherein be free of carbonization trailing plants Japonica silk, the hydrogen-oxygen of metallic element
The mass ratio for changing potassium and water is 1:4~8:200~600.
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