CN105374568A - Graphite phase C3N4/carbon nanotube composite counter electrode preparation method - Google Patents
Graphite phase C3N4/carbon nanotube composite counter electrode preparation method Download PDFInfo
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- CN105374568A CN105374568A CN201510736774.5A CN201510736774A CN105374568A CN 105374568 A CN105374568 A CN 105374568A CN 201510736774 A CN201510736774 A CN 201510736774A CN 105374568 A CN105374568 A CN 105374568A
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Abstract
The invention discloses a graphite phase C3N4/carbon nanotube composite counter electrode preparation method, comprising the steps of: adding a carbon nanotube into a cyanamide or dicyandiamide solution, and performing heating circumfluence, filtering, and drying to obtain a carbon nanotube having the surface adsorbing cyanamide or dicyandiamide; putting the prepared carbon nanotube in a tubular furnace for heating, and performing heat treatment in a nitrogen atmosphere; cooling the carbon nanotube to a room temperature to obtain a graphite phase C3N4/carbon nanotube composite material; mixing the obtained composite material and an additive in a solvent to form a dispersion liquid; uniformly coating the dispersion liquid on the surface of an electrode substrate to prepare an electrode substrate having the surface being covered by a C3N4/carbon nanotube composite material film; and performing drying treatment on the prepared electrode substrate under a vacuum condition to prepare a C3N4/carbon nanotube composite counter electrode. The method is in favor of electronic transmission, and can effectively reduce carbon nanotube and graphite phase C3N4 aggregation, and increase a catalysis surface; the method has a simple preparation process, does not require complex equipment, and is easy to realize industrial mass production.
Description
Technical field
The present invention relates to solar battery technology, particularly a kind of graphite-phase C for DSSC
3n
4the preparation method of/carbon nano-tube combined counter electrode.
Background technology
DSSC is subject to extensive concern because manufacture craft is simple, cost is low, conversion efficiency is high, and be the chief component of DSSC to electrode, its major function accepts the electronics of external circuit and the I in catalytic reduction electrolyte
3 -for I
-.Mainly platinum is to electrode to electrode for current DSSC, but platinum is rare precious metals, and price is too high, and containing I
-/ I
3 -in the electrolyte of redox couple, stability is bad, therefore hinders DSSC large-scale industrial production and business application.So low by price, electro catalytic activity is high, be easy to preparation and material replaces Pt to prepare DSSC and become current study hotspot to electrode.
In recent years, occurred employing material with carbon element, the material with carbon element of the nitrogen that particularly adulterates replaces platinum preparation low price, high-performance to the report of electrode.Graphite-phase C
3n
4be the material with carbon element that a kind of nitrogen content is very high, there is unique electronic structure and excellent chemical stability; And graphite-phase C
3n
4preparation is simple, low price.Therefore greater catalytic performance is shown in fields such as light hydrogen production by water decomposition, electrocatalytic oxidation reduction reactions.But due to graphite-phase C
3n
4the conductivity of itself is lower, therefore uses pure graphite-phase C
3n
4as DSSC to electrode, what reduce electronics transports speed, causes the DSSC photoelectric conversion efficiency that is prepared into not high.
Summary of the invention
Technical problem to be solved by this invention is to provide one can improve graphite-phase C
3n
4conductivity, improve catalytic performance, improve the graphite-phase C of photoelectric conversion efficiency
3n
4the preparation method of/carbon nano-tube combined counter electrode.
For solving the problem, the present invention adopts following technical scheme:
A kind of graphite-phase C
3n
4the preparation method of/carbon nano-tube combined counter electrode, comprises step as follows:
(1) carbon nano-tube is added in cyanamide or dicyandiamide solution, cyanamide in described carbon nano-tube and cyanamide or dicyandiamide solution or dicyandiamide weight ratio are 1:10 ~ 1:30, filter after adding hot reflux, and dry under vacuum, obtain the carbon nano-tube that adsorption has cyanamide or dicyandiamide;
(2) carbon nano-tube prepared by step (1) is put into tube furnace, be warmed up to 500 DEG C ~ 600 DEG C, in a nitrogen atmosphere heat treatment 2 hours ~ 6 hours; Cool to room temperature, obtains graphite-phase C
3n
4/ carbon nano tube compound material;
(3) composite material that step (2) obtains is mixed with solvent and additive, form dispersion liquid; Described solvent is ethanol, n-butanol, a kind of in isopropyl alcohol or wherein a kind of mixed solution with water; Described additive is the mixture of a kind of or two kinds of arbitrary proportions in butyl titanate, isopropyl oxygen alcohol titanium, titanium tetrachloride, graphite-phase C in dispersion liquid
3n
4the mass fraction of/carbon nano tube compound material is 20 ~ 60 parts, and the mass fraction of additive is 0.1 part ~ 1 part, and all the other are solvent;
(4) homogeneous dispersion formed in step (3) is coated onto electrode basement surface, makes surface coverage graphite-phase C
3n
4the electrode base board of/carbon nano tube compound material film;
(5), after drying processes 0.5 hour ~ 2 hours under vacuum by the electrode base board of preparation in step (4), described graphite-phase C is prepared
3n
4/ carbon nano-tube combined counter electrode.
As preferred further, in described step (1), heating-up temperature is 90 DEG C ~ 100 DEG C, and heating return time is 1 hour ~ 6 hours.
As further preferably, the heating rate in described step (2) is 2 DEG C/min ~ 6 DEG C/min.
As preferred further, the method for mixing in described step (3) is grinding or stirring.
As preferred further, in described step (4), dispersion liquid coating layer thickness is 3 μm ~ 15 μm.
As preferred further, the dry treatment temperature in described step (5) is 100 DEG C ~ 200 DEG C.
As preferred further, described in described step (1), the concentration of cyanamide or dicyandiamide solution is 20wt% ~ 50wt%.
As preferred further, in described step (3), in mixed solution, the mass percentage of water is 2% ~ 10%.
The graphite-phase C that the present invention relates to
3n
4/ carbon nano-tube combined counter electrode takes full advantage of graphite-phase C
3n
4the feature that electro catalytic activity point is many, by the compound with carbon nano-tube, significantly improves its conductivity, thus greatly improves the prepared catalytic performance to electrode.This graphite-phase C
3n
4/ carbon nano-tube combination electrode can using electrode as DSSC.
The invention has the beneficial effects as follows:
1, C is made
3n
4form good interface cohesion with carbon nano-tube, be conducive to the transmission of electronics;
2, carbon nano-tube and graphite-phase C can effectively be reduced
3n
4gathering, improve its catalytic surface amass.
3, preparation process is simple, does not need complex device, is easy to a large amount of production of industry
4, the graphite-phase C for preparing of the method
3n
4/ carbon nano-tube combination electrode catalytic activity is high, and it is 2.1 Ω cm that electrochemical impedance spectroscopy shows that its electric charge moves the resistance that jumps
2left and right.Be applied in DSSC, photoelectric conversion efficiency is more than 6.34%.
Accompanying drawing explanation
Fig. 1 is the graphite-phase C prepared by the embodiment of the present invention 3
3n
4the SEM photo of/carbon nano tube compound material.
Fig. 2 is the graphite-phase C prepared by the embodiment of the present invention 4
3n
4the SEM figure of/carbon nano tube compound material.
Fig. 3 is the graphite-phase C prepared by the embodiment of the present invention 5
3n
4the SEM figure of/carbon nano tube compound material.
Embodiment
A kind of graphite-phase C that the present invention relates to
3n
4the preparation method of/carbon nano-tube combined counter electrode, comprises step as follows:
(1) carbon nano-tube added in cyanamide or dicyandiamide solution, add hot reflux 1 ~ 6 hour, heating-up temperature preferably to 90 ~ 100 DEG C, then filter, and dry under vacuum, obtain the carbon nano-tube that adsorption has cyanamide or dicyandiamide; The concentration of described cyanamide or dicyandiamide solution is 20 ~ 50wt%, and the cyanamide in carbon nano-tube and cyanamide or dicyandiamide solution or dicyandiamide weight ratio are 1:10 ~ 1:30.
(2) carbon nano-tube prepared by step (1) is put into tube furnace, controlling heating rate is 2 ~ 6 DEG C/min, is warmed up to 500 ~ 600 DEG C, in a nitrogen atmosphere heat treatment 2 ~ 6 hours; Cool to room temperature, obtains graphite-phase C
3n
4/ carbon nano tube compound material.
(3) composite material that step (2) obtains is mixed with appropriate solvent and additive successively, form dispersion liquid by mixed method that is ultrasonic, that grind or stir; Graphite-phase C in this dispersion liquid
3n
4the mass fraction of/carbon nano tube compound material is 20 ~ 60 parts, and the mass fraction of additive is 0.1 ~ 1 part, and all the other are solvent.
Described solvent is ethanol, n-butanol, a kind of in isopropyl alcohol or wherein a kind of mixed solution with water, and wherein the mass percentage of water is 2 ~ 10%; Described additive is the mixture of a kind of or two kinds of arbitrary proportions in butyl titanate, isopropyl oxygen alcohol titanium, titanium tetrachloride.
(4) dispersion liquid formed in step (3) is evenly coated onto electrode basement surface by spin coating, a painting, spraying, blade coating or printing process, controlling dispersion liquid coating layer thickness is 3 ~ 15 μm, makes surface coverage graphite-phase C
3n
4the electrode base board of/carbon nano tube compound material film.
(5) by the electrode base board of preparation in step (4), under vacuum condition and uniform temperature, dry process is after 0.5 ~ 2 hour, and wherein dry treatment temperature is 100 ~ 200 DEG C, prepares described graphite-phase C
3n
4/ carbon nano-tube combined counter electrode.
Embodiment 1
A kind of graphite-phase C that the present invention relates to
3n
4the preparation method of/carbon nano-tube combined counter electrode, comprises step as follows:
(1) 200mg carbon nano-tube is added in 12mL, 50wt% cyanamide solution at 100 DEG C, add hot reflux 1 hour, then filter, and 60 DEG C of dryings under vacuum, obtain the carbon nano-tube that adsorption has cyanamide.
(2) carbon nano-tube prepared by step (1) is put into tube furnace, controlling heating rate is 2 DEG C/min, is warmed up to 500 DEG C, in a nitrogen atmosphere heat treatment 6 hours; Cool to room temperature, obtains graphite-phase C
3n
4/ carbon nano tube compound material.
(3) composite material that step (2) obtains being distributed in 10mL n-butanol solvent, then adding butyl titanate, forming uniform dispersion liquid by stirring.The mass fraction of composite material described in this dispersion liquid is 20 parts, and the mass fraction of additive butyl titanate is 0.1 part.
(4) using the titanium sheet that cleans up as electrode basement, by the dispersion liquid that formed in step (3) by spraying method uniform deposition to titanium plate surface, control dispersion liquid coating layer thickness is 3 μm, makes surface coverage graphite-phase C
3n
4the electrode base board of/carbon nano tube compound material film.
(5) by the 100 DEG C of dry process 2 hours under vacuum of the electrode base board of preparation in step (4), described graphite-phase C can just be prepared
3n
4/ carbon nano-tube combined counter electrode.
Embodiment 2
A kind of graphite-phase C that the present invention relates to
3n
4the preparation method of/carbon nano-tube combined counter electrode, comprises step as follows:
(1) 500mg carbon nano-tube is added in 25mL, 20wt% cyanamide solution at 90 DEG C, add hot reflux 6 hours, then filter, and 60 DEG C of dryings under vacuum, obtain the carbon nano-tube that adsorption has cyanamide.
(2) carbon nano-tube prepared by step (1) is put into tube furnace, controlling heating rate is 6 DEG C/min, is warmed up to 600 DEG C, in a nitrogen atmosphere heat treatment 2 hours; Cool to room temperature, obtains graphite-phase C
3n
4/ carbon nano tube compound material.
(3) composite material that step (2) obtains is distributed in 10mL isopropanol solvent, then adds isopropyl oxygen alcohol titanium, form uniform dispersion liquid by grinding.The mass fraction of composite material described in this dispersion liquid is 60 parts, and the mass fraction of additive isopropyl oxygen alcohol titanium is 1 part.
(4) using the electro-conductive glass that cleans up as electrode basement, by the dispersion liquid that formed in step (3) by knife coating procedure uniform deposition to conductive glass surface, control dispersion liquid coating layer thickness is 15 μm, makes surface coverage graphite-phase C
3n
4the electrode base board of/carbon nano tube compound material film.
(5) process 0.5 hour by dry under vacuum condition and 200 DEG C of temperature for the electrode base board of preparation in step (4), just can prepare described graphite-phase C
3n
4/ carbon nano-tube combined counter electrode.
Embodiment 3
A kind of graphite-phase C that the present invention relates to
3n
4the preparation method of/carbon nano-tube combined counter electrode, comprises step as follows:
(1) 250mg carbon nano-tube is added in 10mL, 50wt% cyanamide solution at 95 DEG C, add hot reflux 4 hours, then filter, and 60 DEG C of dryings under vacuum, obtain the carbon nano-tube that adsorption has cyanamide.
(2) carbon nano-tube prepared by step (1) is put into tube furnace, controlling heating rate is 3 DEG C/min, is warmed up to 550 DEG C, in a nitrogen atmosphere heat treatment 4 hours; Cool to room temperature, obtains graphite-phase C
3n
4/ carbon nano tube compound material, its SEM photo as shown in Figure 1.Fig. 1 demonstrates carbon nano-tube and graphite-phase C
3n
4be combined with each other uniformly, form the compound of porous.Carbon nano-tube can form effective conductive network in compound, thus improves its electrocatalysis characteristic.
(3) be distributed in 10mL solvent by the composite material that step (2) obtains, described solvent is the mixed solution of n-butanol and water, and in mixed solution, the mass percentage of water is 5%; Then add isopropyl oxygen alcohol titanium, form uniform dispersion liquid by grinding.The mass fraction of composite material described in this dispersion liquid is 50 parts, and the mass fraction of additive isopropyl oxygen alcohol titanium is 0.5 part.
(4) using the electro-conductive glass that cleans up as electrode basement, by the dispersion liquid that formed in step (3) by knife coating procedure uniform deposition to conductive glass surface, control dispersion liquid coating layer thickness is 10 μm, makes surface coverage graphite-phase C
3n
4the electrode base board of/carbon nano tube compound material film.
(5) process 1 hour by dry at vacuum condition and 150 DEG C for the electrode base board of preparation in step (4), just can prepare described graphite-phase C
3n
4/ carbon nano-tube combined counter electrode.
Embodiment 4
A kind of graphite-phase C that the present invention relates to
3n
4/ carbon nano-tube combined counter electrode, preparation method, comprise step as follows:
(1) 300mg carbon nano-tube is added in 15mL, 50wt% cyanamide solution at 95 DEG C, add hot reflux 1.5 hours, then filter, and 60 DEG C of dryings under vacuum, obtain the carbon nano-tube that adsorption has cyanamide.
(2) carbon nano-tube prepared by step (1) is put into tube furnace, controlling heating rate is 4 DEG C/min, is warmed up to 520 DEG C, in a nitrogen atmosphere heat treatment 5 hours; Cool to room temperature, obtains graphite-phase C
3n
4/ carbon nano tube compound material, its SEM photo as shown in Figure 2.
(3) be distributed in 10mL solvent by the composite material that step (2) obtains, described solvent is the mixed solution of ethanol and water, and in mixed solution, the mass percentage of water is 6%; Then add titanium tetrachloride, form uniform dispersion liquid by grinding.The mass fraction of composite material described in this dispersion liquid is 55 parts, and the mass fraction of additive titanium tetrachloride is 0.7 part.
(4) using the titanium sheet that cleans up as electrode basement, by the dispersion liquid that formed in step (3) by knife coating procedure uniform deposition to titanium plate surface, control dispersion liquid coating layer thickness is 8 μm, makes surface coverage graphite-phase C
3n
4the electrode base board of/carbon nano tube compound material film.
(5) process 1.5 hours by dry at vacuum condition and 180 DEG C for the electrode base board of preparation in step (4), just can prepare described graphite-phase C
3n
4/ carbon nano-tube combined counter electrode.
Embodiment 5
A kind of graphite-phase C that the present invention relates to
3n
4the preparation method of/carbon nano-tube combined counter electrode, comprises step as follows:
(1) 200mg carbon nano-tube is added in 10mL, 30wt% dicyandiamide solution at 95 DEG C, add hot reflux 1.5 hours, then filter, and 60 DEG C of dryings under vacuum, obtain the carbon nano-tube that adsorption has dicyandiamide.
(2) carbon nano-tube prepared by step (1) is put into tube furnace, controlling heating rate is 3 DEG C/min, is warmed up to 570 DEG C, in a nitrogen atmosphere heat treatment 2 hours; Cool to room temperature, obtains graphite-phase C
3n
4/ carbon nano tube compound material, its SEM photo as shown in Figure 3.
(3) be distributed in 10mL solvent by the composite material that step (2) obtains, described solvent is the mixed solution of n-butanol and water, and in mixed solution, the mass percentage of water is 8%; Then add isopropyl oxygen alcohol titanium, form uniform dispersion liquid by grinding.The mass fraction of composite material described in this dispersion liquid is 40 parts, and the mass fraction of additive isopropyl oxygen alcohol titanium is 0.5 part.
(4) using the polyester sheet of deposition ITO that cleans up as electrode basement, by surperficial to described polyester sheet by printing process uniform deposition for the dispersion liquid formed in step (3), controlling dispersion liquid coating layer thickness is 7 μm, makes surface coverage graphite-phase C
3n
4the electrode base board of/carbon nano tube compound material film.
(5) process 1 hour by dry at vacuum condition and 100 DEG C for the electrode base board of preparation in step (4), just can prepare described graphite-phase C
3n
4/ carbon nano-tube combined counter electrode.
Embodiment 6
A kind of graphite-phase C that the present invention relates to
3n
4the preparation method of/carbon nano-tube combined counter electrode, comprises step as follows:
(1) 250mg carbon nano-tube is added in 10mL, 50wt% dicyandiamide solution.At 95 DEG C, add hot reflux 1.5 hours, then filter, and 60 DEG C of dryings under vacuum, obtain the carbon nano-tube that adsorption has dicyandiamide.
(2) carbon nano-tube prepared by step (1) is put into tube furnace, controlling heating rate is 3 DEG C/min, is warmed up to 550 DEG C, in a nitrogen atmosphere heat treatment 4 hours; Cool to room temperature, obtains graphite-phase C
3n
4/ carbon nano tube compound material.
(3) be distributed in 10mL solvent by the composite material that step (2) obtains, described solvent is the mixed solution of n-butanol and water, and in mixed solution, the mass percentage of water is 3%; Then add titanium tetrachloride, form uniform dispersion liquid by grinding.The mass fraction of composite material described in this dispersion liquid is 50 parts, and the mass fraction of additive titanium tetrachloride is 0.6 part.
(4) using the electro-conductive glass that cleans up as electrode basement, by the dispersion liquid that formed in step (3) by spin coating method uniform deposition to described conductive glass surface, control dispersion liquid coating layer thickness is 6 μm, makes surface coverage graphite-phase C
3n
4the electrode base board of/carbon nano tube compound material film.
(5) process 0.5 hour by dry under vacuum condition and 200 DEG C of temperature for the electrode base board of preparation in step (4), just can prepare described graphite-phase C
3n
4/ carbon nano-tube combined counter electrode.
Graphite-phase C of the present invention
3n
4/ carbon nano-tube combined counter electrode all can using electrode as DSSC.Utilize the graphite-phase C of the embodiment of the present invention 3 ~ embodiment 5
3n
4when/carbon nano-tube combined counter electrode prepares DSSC, step is as follows:
1, first preliminary treatment is carried out to electro-conductive glass;
2, then titania slurry is coated on the electro-conductive glass handled well, THICKNESS CONTROL 10 μm, immerses attach overnight in dyestuff after 450 degree of heat treatments and form the work electrode of battery;
3, on described work electrode, described graphite-phase C is pressed
3n
4/ carbon nano-tube combined counter electrode, two interelectrode gap fillings contain I
-/ I
3 -redox couple (0.5MI
2, 0.05MI
3 -) electrolyte, be prepared into DSSC.
Measure the described graphite-phase C adopting embodiment 3 ~ embodiment 5 to prepare
3n
4the electricity conversion of the DSSC that/carbon nano-tube combined counter electrode is made, and contrast with conventional P t electrode, data are as table 1.
The test of battery performance be by from battery work electrode with two wires drawn to electrode receive on battery performance test device.The work area of battery is 0.2cm
-2, intensity of illumination is 100mw/cm
2.Fill factor, curve factor (ff) refers to the current/voltage product (I that can to obtain in I-V curve on the point of peak power output
opt× V
opt) and I
sc× V
oc(I
scfor short-circuit photocurrent, V
ocfor open-circuit photovoltage) ratio, its embodies the power output of battery with the variation characteristic of load.Photoelectric conversion efficiency (η) is then I
opt× V
optwith the luminous power P of input
inratio.
The photoelectric parameter of DSSC assembled by table 1
Therefore graphite-phase C3N4/ carbon nano-tube combined counter electrode can replace Pt to be used for DSSC.
Although embodiment of the present invention are open as above, but it is not restricted to listed in specification and execution mode utilization, it can be applied to various applicable the field of the invention completely, for those skilled in the art, can easily realize other amendment, therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details and illustrates here and the legend described.
Claims (8)
1. a graphite-phase C
3n
4the preparation method of/carbon nano-tube combined counter electrode, is characterized in that comprising step as follows:
(1) carbon nano-tube is added in cyanamide or dicyandiamide solution, cyanamide in described carbon nano-tube and cyanamide or dicyandiamide solution or dicyandiamide weight ratio are 1:10 ~ 1:30, filter after adding hot reflux, and dry under vacuum, obtain the carbon nano-tube that adsorption has cyanamide or dicyandiamide;
(2) carbon nano-tube prepared by step (1) is put into tube furnace, be warmed up to 500 DEG C ~ 600 DEG C, in a nitrogen atmosphere heat treatment 2 hours ~ 6 hours; Cool to room temperature, obtains graphite-phase C
3n
4/ carbon nano tube compound material;
(3) composite material that step (2) obtains is mixed with solvent and additive, form dispersion liquid; Described solvent is ethanol, n-butanol, a kind of in isopropyl alcohol or wherein a kind of mixed solution with water; Described additive is the mixture of a kind of or two kinds of arbitrary proportions in butyl titanate, isopropyl oxygen alcohol titanium, titanium tetrachloride, graphite-phase C in dispersion liquid
3n
4the mass fraction of/carbon nano tube compound material is 20 ~ 60 parts, and the mass fraction of additive is 0.1 part ~ 1 part, and all the other are solvent;
(4) homogeneous dispersion formed in step (3) is coated onto electrode basement surface, makes surface coverage graphite-phase C
3n
4the electrode base board of/carbon nano tube compound material film;
(5), after drying processes 0.5 hour ~ 2 hours under vacuum by the electrode base board of preparation in step (4), described graphite-phase C is prepared
3n
4/ carbon nano-tube combined counter electrode.
2. graphite-phase C according to claim 1
3n
4the preparation method of/carbon nano-tube combined counter electrode, it is characterized in that in described step (1), heating-up temperature is 90 DEG C ~ 100 DEG C, heating return time is 1 hour ~ 6 hours.
3. graphite-phase C according to claim 1
3n
4the preparation method of/carbon nano-tube combined counter electrode, the heating rate that it is characterized in that in described step (2) is 2 DEG C/min ~ 6 DEG C/min.
4. graphite-phase C according to claim 1
3n
4the preparation method of/carbon nano-tube combined counter electrode, is characterized in that the method for mixing in described step (3) is for grinding or stirring.
5. graphite-phase C according to claim 1
3n
4the preparation method of/carbon nano-tube combined counter electrode, is characterized in that in described step (4), dispersion liquid coating layer thickness is 3 μm ~ 15 μm.
6. graphite-phase C according to claim 1
3n
4the preparation method of/carbon nano-tube combined counter electrode, is characterized in that the dry treatment temperature in described step (5) is 100 DEG C ~ 200 DEG C.
7. graphite-phase C according to claim 1 and 2
3n
4the preparation method of/carbon nano-tube combined counter electrode, is characterized in that the concentration of cyanamide or dicyandiamide solution described in described step (1) is 20wt% ~ 50wt%.
8. the graphite-phase C according to claim 1 or 4
3n
4the preparation method of/carbon nano-tube combined counter electrode, is characterized in that the mass percentage of water in mixed solution in described step (3) is 2% ~ 10%.
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CN109248706A (en) * | 2018-10-25 | 2019-01-22 | 天津工业大学 | Carbon nanotube nitrogenizes carbon composite and synthetic method |
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