CN105374568B - Graphite-phase C3N4The preparation method of/CNT combined counter electrode - Google Patents
Graphite-phase C3N4The preparation method of/CNT combined counter electrode Download PDFInfo
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- CN105374568B CN105374568B CN201510736774.5A CN201510736774A CN105374568B CN 105374568 B CN105374568 B CN 105374568B CN 201510736774 A CN201510736774 A CN 201510736774A CN 105374568 B CN105374568 B CN 105374568B
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Abstract
The invention discloses a kind of graphite-phase C3N4The preparation method of/CNT combined counter electrode, including step are as follows：CNT is added in cyanamide or dicyandiamide solution, filtered after being heated to reflux, and is dried, obtaining adsorption has the CNT of cyanamide or dicyandiamide；The CNT of preparation is put into tube furnace, heats up, is heat-treated in a nitrogen atmosphere；Room temperature is cooled to, obtains graphite-phase C3N4/ carbon nano tube compound material；Obtained composite is mixed with solvent and additive, forms dispersion liquid；Homogeneous dispersion is coated onto electrode basement surface, surface covering graphite-phase C is made3N4The electrode base board of/carbon nano tube compound material film；By electrode base board drying process under vacuum, the graphite-phase C is prepared3N4/ CNT combined counter electrode.Beneficial effect is：Be advantageous to the transmission of electronics；CNT and graphite-phase C can effectively be reduced3N4Aggregation, improve its catalytic surface product.Preparation process is simple, it is not necessary to complex device, is easy to industrial a large amount of productions.
Description
Technical field
The present invention relates to solar battery technology, more particularly to a kind of graphite-phase for DSSC
C3N4The preparation method of/CNT combined counter electrode.
Background technology
DSSC due to manufacture craft is simple, cost is low, high conversion efficiency and receive significant attention, and
It is the chief component of DSSC to electrode, its major function is to receive the electronics of external circuit and urge
Change the I gone back in original electrolyte3 -For I-.At present DSSC be mainly to electrode platinum to electrode, but platinum is rare
Noble metal, price is too high, and is containing I-/I3 -Stability is bad in the electrolyte of redox couple, therefore hinders dyestuff
Sensitization solar battery large-scale industrial production and business application.So with price is low, electro catalytic activity is high, easily prepared and material
Material prepares DSSC instead of Pt turns into current study hotspot to electrode.
In recent years, occur using carbon material, the carbon material for particularly adulterating nitrogen replaces platinum to prepare low price, high-performance to electricity
The report of pole.Graphite-phase C3N4It is a kind of very high carbon material of nitrogen content, there is unique electronic structure and excellent chemically stable
Property；And graphite-phase C3N4Prepare simply, it is cheap.Therefore in field tables such as light hydrogen production by water decomposition, electrocatalytic oxidation reduction reactions
Reveal greater catalytic performance.But due to graphite-phase C3N4The electrical conductivity of itself is relatively low, therefore uses pure graphite-phase C3N4As dyestuff
Sensitization solar battery to electrode, reduce electronics transports speed, causes the DSSC light being prepared into
Photoelectric transformation efficiency is not high.
The content of the invention
The technical problems to be solved by the invention, which are to provide one kind, can improve graphite-phase C3N4Conductivity, improvement urges
Change performance, improve the graphite-phase C of photoelectric transformation efficiency3N4The preparation method of/CNT combined counter electrode.
To solve the above problems, the present invention adopts the following technical scheme that：
A kind of graphite-phase C3N4The preparation method of/CNT combined counter electrode, including step are as follows：
(1) CNT is added in cyanamide or dicyandiamide solution, the CNT and cyanamide or dicyandiamide are molten
Cyanamide or dicyandiamide weight ratio in liquid are 1:10~1:30, filtered after being heated to reflux, and dry under vacuum, obtain
Adsorption has the CNT of cyanamide or dicyandiamide；
(2) CNT prepared by step (1) is put into tube furnace, 500 DEG C~600 DEG C is warming up to, in nitrogen gas
It is heat-treated 2 hours~6 hours under atmosphere；Room temperature is cooled to, obtains graphite-phase C3N4/ carbon nano tube compound material；
(3) composite that step (2) obtains is mixed with solvent and additive, forms dispersion liquid；The solvent is second
Alcohol, n-butanol, one kind or the mixed solution of one of which and water in isopropanol；The additive is butyl titanate, isopropyl oxygen
The mixture of one kind or two kinds of arbitrary proportions in alcohol titanium, titanium tetrachloride, graphite-phase C in dispersion liquid3N4/ carbon nanotube composite
The mass fraction of material is 20~60 parts, and the mass fraction of additive is 0.1 part~1 part, and remaining is solvent；
(4) homogeneous dispersion formed in step (3) is coated onto electrode basement surface, surface covering graphite-phase C is made3N4/
The electrode base board of carbon nano tube compound material film；
(5) by after the electrode base board prepared in step (4) under vacuum drying process 0.5 hour~2 hours, prepare
Go out the graphite-phase C3N4/ CNT combined counter electrode.
As further preferred, heating-up temperature is 90 DEG C~100 DEG C in the step (1), is heated to reflux the time as 1 hour
~6 hours.
As further preferred, the heating rate in the step (2) is 2 DEG C/min~6 DEG C/min.
As further preferred, the method for mixing is grinding or stirring in the step (3).
As further preferred, dispersion liquid coating layer thickness is 3 μm~15 μm in the step (4).
As further preferred, the drying process temperature in the step (5) is 100 DEG C~200 DEG C.
As further preferred, the concentration of cyanamide or dicyandiamide solution described in the step (1) be 20wt%~
50wt%.
As further preferred, the weight/mass percentage composition of mixed solution reclaimed water is 2%~10% in the step (3).
Graphite-phase C of the present invention3N4/ CNT combined counter electrode takes full advantage of graphite-phase C3N4Electro-catalysis is lived
Property point it is more the characteristics of, by compound with CNT, hence it is evident that improve its conductivity, it is prepared to electrode so as to greatly improve
Catalytic performance.Graphite-phase C3N4/ carbon nano-tube combination electrode can make as DSSC to electrode
With.
The beneficial effects of the invention are as follows：
1st, C is made3N4Good interface cohesion is formed with CNT, is advantageous to the transmission of electronics；
2nd, CNT and graphite-phase C can effectively be reduced3N4Aggregation, improve its catalytic surface product.
3rd, preparation process is simple, it is not necessary to complex device, is easy to industrial a large amount of productions
4th, graphite-phase C prepared by this method3N4/ carbon nano-tube combination electrode catalytic activity is high, and electrochemical impedance spectroscopy shows it
It is 2.1 Ω cm that electric charge, which moves jump resistance,2Left and right.Applied in DSSC, photoelectric transformation efficiency is more than 6.34%.
Brief description of the drawings
Fig. 1 is the graphite-phase C prepared by the embodiment of the present invention 33N4The SEM photograph of/carbon nano tube compound material.
Fig. 2 is the graphite-phase C prepared by the embodiment of the present invention 43N4The SEM figures of/carbon nano tube compound material.
Fig. 3 is the graphite-phase C prepared by the embodiment of the present invention 53N4The SEM figures of/carbon nano tube compound material.
Embodiment
A kind of graphite-phase C of the present invention3N4The preparation method of/CNT combined counter electrode, including step are as follows：
(1) CNT is added in cyanamide or dicyandiamide solution, be heated to reflux 1~6 hour, heating-up temperature is preferably extremely
90~100 DEG C, then filter, and dry under vacuum, obtaining adsorption has the CNT of cyanamide or dicyandiamide；
The concentration of the cyanamide or dicyandiamide solution is 20~50wt%, CNT and single cyanogen in cyanamide or dicyandiamide solution
Amine or dicyandiamide weight ratio are 1:10~1:30.
(2) CNT prepared by step (1) is put into tube furnace, it is 2~6 DEG C/min to control heating rate, is risen
Temperature is heat-treated 2~6 hours in a nitrogen atmosphere to 500~600 DEG C；Room temperature is cooled to, obtains graphite-phase C3N4/ CNT is multiple
Condensation material.
(3) composite that step (2) obtains is mixed with appropriate solvent and additive successively, by ultrasound, grinding or
The mixed method of person's stirring forms dispersion liquid；Graphite-phase C in the dispersion liquid3N4The mass fraction of/carbon nano tube compound material is 20
~60 parts, the mass fraction of additive is 0.1~1 part, and remaining is solvent.
The solvent is ethanol, n-butanol, one kind or the mixed solution of one of which and water in isopropanol, its reclaimed water
Weight/mass percentage composition is 2~10%；The additive is butyl titanate, isopropyl oxygen alcohol titanium, one kind in titanium tetrachloride or two kinds
The mixture of arbitrary proportion.
(4) dispersion liquid formed in step (3) is uniformly coated onto electricity by spin coating, drop coating, spraying, blade coating or printing process
Pole substrate surface, it is 3~15 μm to control dispersion liquid coating layer thickness, and surface covering graphite-phase C is made3N4/ carbon nano tube compound material
The electrode base board of film.
(5) by the middle electrode base board prepared drying process 0.5~2 hour under vacuum condition and certain temperature of step (4)
Afterwards, wherein drying process temperature is 100~200 DEG C, prepares the graphite-phase C3N4/ CNT combined counter electrode.
Embodiment 1
A kind of graphite-phase C of the present invention3N4The preparation method of/CNT combined counter electrode, including step are as follows：
(1) 200mg CNTs are added in 12mL, 50wt% cyanamide solution and are heated to reflux at 100 DEG C 1 hour,
Then filter, and 60 DEG C of dryings under vacuum, obtaining adsorption has the CNT of cyanamide.
(2) CNT prepared by step (1) is put into tube furnace, it is 2 DEG C/min to control heating rate, is warming up to
500 DEG C, it is heat-treated 6 hours in a nitrogen atmosphere；Room temperature is cooled to, obtains graphite-phase C3N4/ carbon nano tube compound material.
(3) composite that step (2) obtains is distributed in 10mL n-butanol solvents, then adds butyl titanate, led to
Cross stirring and form uniform dispersion liquid.The mass fraction of composite described in the dispersion liquid is 20 parts, additive butyl titanate
Mass fraction be 0.1 part.
(4) it is using the titanium sheet cleaned up as electrode basement, the dispersion liquid formed in step (3) is equal by spraying method
Even to deposit to titanium plate surface, it is 3 μm to control dispersion liquid coating layer thickness, and surface covering graphite-phase C is made3N4/ carbon nanotube composite
Expect the electrode base board of film.
(5) by the electrode base board prepared in step (4) 100 DEG C of drying process 2 hours under vacuum, can prepare
The graphite-phase C3N4/ CNT combined counter electrode.
Embodiment 2
A kind of graphite-phase C of the present invention3N4The preparation method of/CNT combined counter electrode, including step are as follows：
(1) 500mg CNTs are added in 25mL, 20wt% cyanamide solution and is heated to reflux 6 hours at 90 DEG C, so
After filter, and 60 DEG C of dryings under vacuum, obtaining adsorption has the CNT of cyanamide.
(2) CNT prepared by step (1) is put into tube furnace, it is 6 DEG C/min to control heating rate, is warming up to
600 DEG C, it is heat-treated 2 hours in a nitrogen atmosphere；Room temperature is cooled to, obtains graphite-phase C3N4/ carbon nano tube compound material.
(3) composite that step (2) obtains is distributed in 10mL isopropanol solvents, then adds isopropyl oxygen alcohol titanium,
Uniform dispersion liquid is formed by grinding.The mass fraction of composite described in the dispersion liquid is 60 parts, additive isopropyl oxygen
The mass fraction of alcohol titanium is 1 part.
(4) using the electro-conductive glass cleaned up as electrode basement, the dispersion liquid formed in step (3) is passed through into blade coating side
For method uniform deposition to conductive glass surface, it is 15 μm to control dispersion liquid coating layer thickness, and surface covering graphite-phase C is made3N4/ carbon is received
The electrode base board of mitron composite material film.
(5) by the electrode base board prepared in step (4) at a temperature of vacuum condition and 200 DEG C drying process 0.5 hour, just
The graphite-phase C can be prepared3N4/ CNT combined counter electrode.
Embodiment 3
A kind of graphite-phase C of the present invention3N4The preparation method of/CNT combined counter electrode, including step are as follows：
(1) 250mg CNTs are added in 10mL, 50wt% cyanamide solution and is heated to reflux 4 hours at 95 DEG C, so
After filter, and 60 DEG C of dryings under vacuum, obtaining adsorption has the CNT of cyanamide.
(2) CNT prepared by step (1) is put into tube furnace, it is 3 DEG C/min to control heating rate, is warming up to
550 DEG C, it is heat-treated 4 hours in a nitrogen atmosphere；Room temperature is cooled to, obtains graphite-phase C3N4/ carbon nano tube compound material, its SEM
Photo is as shown in Figure 1.Fig. 1 shows CNT and graphite-phase C3N4Uniformly it is combined with each other, forms porous compound.
CNT can form effective conductive network in compound, so as to improve its electrocatalysis characteristic.
(3) composite that step (2) obtains is distributed in 10mL solvents, the solvent is the mixing of n-butanol and water
Solution, the weight/mass percentage composition of mixed solution reclaimed water is 5%；Then isopropyl oxygen alcohol titanium is added, uniform point is formed by grinding
Dispersion liquid.The mass fraction of composite described in the 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 cleaned up as electrode basement, the dispersion liquid formed in step (3) is passed through into blade coating side
For method uniform deposition to conductive glass surface, it is 10 μm to control dispersion liquid coating layer thickness, and surface covering graphite-phase C is made3N4/ carbon is received
The electrode base board of mitron composite material film.
(5) by the middle electrode base board prepared drying process 1 hour at vacuum condition and 150 DEG C of step (4), can prepare
Go out the graphite-phase C3N4/ CNT combined counter electrode.
Embodiment 4
A kind of graphite-phase C of the present invention3N4/ CNT combined counter electrode, preparation method, including step is as follows：
(1) 300mg CNTs are added in 15mL, 50wt% cyanamide solution and are heated to reflux at 95 DEG C 1.5 hours,
Then filter, and 60 DEG C of dryings under vacuum, obtaining adsorption has the CNT of cyanamide.
(2) CNT prepared by step (1) is put into tube furnace, it is 4 DEG C/min to control heating rate, is warming up to
520 DEG C, it is heat-treated 5 hours in a nitrogen atmosphere；Room temperature is cooled to, obtains graphite-phase C3N4/ carbon nano tube compound material, its SEM
Photo is as shown in Figure 2.
(3) composite that step (2) obtains is distributed in 10mL solvents, the solvent is molten for the mixing of ethanol and water
Liquid, the weight/mass percentage composition of mixed solution reclaimed water is 6%；Then titanium tetrachloride is added, uniform dispersion liquid is formed by grinding.
The mass fraction of composite described in the dispersion liquid is 55 parts, and the mass fraction of additive titanium tetrachloride is 0.7 part.
(4) it is using the titanium sheet cleaned up as electrode basement, the dispersion liquid formed in step (3) is equal by knife coating procedure
Even to deposit to titanium plate surface, it is 8 μm to control dispersion liquid coating layer thickness, and surface covering graphite-phase C is made3N4/ carbon nanotube composite
Expect the electrode base board of film.
(5) by the electrode base board prepared in step (4) at vacuum condition and 180 DEG C drying process 1.5 hours,
Prepare the graphite-phase C3N4/ CNT combined counter electrode.
Embodiment 5
A kind of graphite-phase C of the present invention3N4The preparation method of/CNT combined counter electrode, including step are as follows：
(1) 200mg CNTs are added in 10mL, 30wt% dicyandiamide solution and are heated to reflux at 95 DEG C 1.5 hours,
Then filter, and 60 DEG C of dryings under vacuum, obtaining adsorption has the CNT of dicyandiamide.
(2) CNT prepared by step (1) is put into tube furnace, it is 3 DEG C/min to control heating rate, is warming up to
570 DEG C, it is heat-treated 2 hours in a nitrogen atmosphere；Room temperature is cooled to, obtains graphite-phase C3N4/ carbon nano tube compound material, its SEM
Photo is as shown in Figure 3.
(3) composite that step (2) obtains is distributed in 10mL solvents, the solvent is the mixing of n-butanol and water
Solution, the weight/mass percentage composition of mixed solution reclaimed water is 8%；Then isopropyl oxygen alcohol titanium is added, uniform point is formed by grinding
Dispersion liquid.The mass fraction of composite described in the dispersion liquid is 40 parts, and the mass fraction of additive isopropyl oxygen alcohol titanium is 0.5
Part.
(4) using the deposition ITO cleaned up polyester piece as electrode basement, the dispersion liquid formed in step (3) is led to
Printing process uniform deposition is crossed to the polyester piece surface, it is 7 μm to control dispersion liquid coating layer thickness, and surface covering graphite-phase is made
C3N4The electrode base board of/carbon nano tube compound material film.
(5) by the middle electrode base board prepared drying process 1 hour at vacuum condition and 100 DEG C of step (4), can prepare
Go out the graphite-phase C3N4/ CNT combined counter electrode.
Embodiment 6
A kind of graphite-phase C of the present invention3N4The preparation method of/CNT combined counter electrode, including step are as follows：
(1) 250mg CNTs are added in 10mL, 50wt% dicyandiamide solution.It is small that 1.5 are heated to reflux at 95 DEG C
When, then filter, and 60 DEG C of dryings under vacuum, obtaining adsorption has the CNT of dicyandiamide.
(2) CNT prepared by step (1) is put into tube furnace, it is 3 DEG C/min to control heating rate, is warming up to
550 DEG C, it is heat-treated 4 hours in a nitrogen atmosphere；Room temperature is cooled to, obtains graphite-phase C3N4/ carbon nano tube compound material.
(3) composite that step (2) obtains is distributed in 10mL solvents, the solvent is the mixing of n-butanol and water
Solution, the weight/mass percentage composition of mixed solution reclaimed water is 3%；Then titanium tetrachloride is added, uniform disperse is formed by grinding
Liquid.The mass fraction of composite described in the dispersion liquid is 50 parts, and the mass fraction of additive titanium tetrachloride is 0.6 part.
(4) using the electro-conductive glass cleaned up as electrode basement, the dispersion liquid formed in step (3) is passed through into spin coating side
For method uniform deposition to the conductive glass surface, it is 6 μm to control dispersion liquid coating layer thickness, and surface covering graphite-phase C is made3N4/ carbon
The electrode base board of nanometer tube composite materials film.
(5) by the electrode base board prepared in step (4) at a temperature of vacuum condition and 200 DEG C drying process 0.5 hour, just
The graphite-phase C can be prepared3N4/ CNT combined counter electrode.
The graphite-phase C of the present invention3N4/ CNT combined counter electrode can be as DSSC to electricity
Pole uses.Utilize the graphite-phase C of 3~embodiment of the embodiment of the present invention 53N4/ CNT combined counter electrode prepares dye sensitization too
Step is as follows during positive energy battery：
1st, electro-conductive glass is pre-processed first；
2 and then titania slurry is coated on the electro-conductive glass handled well, 10 μm of thickness control, 450 degree are heat-treated
Immerse afterwards in dyestuff and adsorb the working electrode for forming battery overnight；
3rd, the graphite-phase C is pressed on the working electrode3N4/ CNT combined counter electrode, two interelectrode gaps
Filling contains I-/I3 -Redox couple (0.5MI2,0.05MI3 -) electrolyte, be prepared into DSSC.
The graphite-phase C that measurement is prepared using 3~embodiment of embodiment 53N4Made of/CNT combined counter electrode
The electricity conversion of DSSC, and contrasted with traditional Pt electrodes, data such as table 1.
The test of battery performance is by being connected to battery from the working electrode of battery and to drawing two wires on electrode
On performance testing device.The work area of battery is 0.2cm-2, intensity of illumination is 100mw/cm2.Fill factor, curve factor (ff) refers to
Current Voltage product (the I on the point of peak power output can be obtained in I-V curveopt×Vopt) and Isc×Voc(IscFor short-circuit light
Electric current, VocThe ratio between for open-circuit photovoltage), it embodies the power output of battery with the change dynamic characteristic of load.Photoelectric transformation efficiency (η)
It is then Iopt×VoptWith the luminous power P of inputinThe ratio between.
Table 1 assembles the photoelectric parameter of DSSC
Therefore graphite-phase C3N4/ CNT combined counter electrode can be used for DSSC instead of Pt.
Although embodiment of the present invention is disclosed as above, it is not restricted in specification and embodiment listed
With it can be applied to various suitable the field of the invention completely, can be easily for those skilled in the art
Other modification is realized, therefore under the universal limited without departing substantially from claim and equivalency range, it is of the invention and unlimited
In specific details and shown here as the legend with description.
Claims (8)
- A kind of 1. graphite-phase C3N4The preparation method of/CNT combined counter electrode, it is characterized in that as follows including step：(1) CNT is added in cyanamide or dicyandiamide solution, in the CNT and cyanamide or dicyandiamide solution Cyanamide or dicyandiamide weight ratio be 1:10~1:30, filtered after being heated to reflux, and dry under vacuum, obtain surface It is adsorbed with the CNT of cyanamide or dicyandiamide；(2) CNT prepared by step (1) is put into tube furnace, is warming up to 500 DEG C~600 DEG C, in a nitrogen atmosphere Heat treatment 2 hours~6 hours；Room temperature is cooled to, obtains graphite-phase C3N4/ carbon nano tube compound material；(3) composite that step (2) obtains is mixed with solvent and additive, forms dispersion liquid；The solvent is ethanol, just The mixed solution of one kind or one of which and water in butanol, isopropanol；The additive be butyl titanate, isopropyl oxygen alcohol titanium, The mixture of one kind or two kinds of arbitrary proportions in titanium tetrachloride, graphite-phase C in dispersion liquid3N4The matter of/carbon nano tube compound material It is 20~60 parts to measure number, and the mass fraction of additive is 0.1 part~1 part, and remaining is solvent；(4) homogeneous dispersion formed in step (3) is coated onto electrode basement surface, surface covering graphite-phase C is made3N4/ carbon is received The electrode base board of mitron composite material film；(5) by after the electrode base board prepared in step (4) under vacuum drying process 0.5 hour~2 hours, institute is prepared State graphite-phase C3N4/ CNT combined counter electrode.
- 2. graphite-phase C according to claim 13N4The preparation method of/CNT combined counter electrode, it is characterized in that described Heating-up temperature is 90 DEG C~100 DEG C in step (1), is heated to reflux the time as 1 hour~6 hours.
- 3. graphite-phase C according to claim 13N4The preparation method of/CNT combined counter electrode, it is characterized in that described Heating rate in step (2) is 2 DEG C/min~6 DEG C/min.
- 4. graphite-phase C according to claim 13N4The preparation method of/CNT combined counter electrode, it is characterized in that described The method of mixing is grinding or stirring in step (3).
- 5. graphite-phase C according to claim 13N4The preparation method of/CNT combined counter electrode, it is characterized in that described Dispersion liquid coating layer thickness is 3 μm~15 μm in step (4).
- 6. graphite-phase C according to claim 13N4The preparation method of/CNT combined counter electrode, it is characterized in that described Drying process temperature in step (5) is 100 DEG C~200 DEG C.
- 7. graphite-phase C according to claim 1 or 23N4The preparation method of/CNT combined counter electrode, it is characterized in that institute It is 20wt%~50wt% to state the concentration of cyanamide or dicyandiamide solution described in step (1).
- 8. the graphite-phase C according to claim 1 or 43N4The preparation method of/CNT combined counter electrode, it is characterized in that institute The weight/mass percentage composition for stating mixed solution reclaimed water in step (3) is 2%~10%.
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| "氧掺杂g-C3N4可见光催化剂的制备及性能研究";李江华;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20140815(第8期);B016-322 * |
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