CN1935639A - Spherical acetylene black light cathode material, and its preparing method and use - Google Patents
Spherical acetylene black light cathode material, and its preparing method and use Download PDFInfo
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- CN1935639A CN1935639A CN 200610016154 CN200610016154A CN1935639A CN 1935639 A CN1935639 A CN 1935639A CN 200610016154 CN200610016154 CN 200610016154 CN 200610016154 A CN200610016154 A CN 200610016154A CN 1935639 A CN1935639 A CN 1935639A
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Abstract
The invention relates to a spherical acetylene black electrode material and its preparation and application as photocathode in dye sensitized solar batteries. And it is composed of spherical grains, diameter 50-100nm and specific surface area 280-300m2/g. And the preparing method adopts spin-coating technique to uniformly coat spherical acetylene black on conductive glass and makes porous acetylene black photocathode. And the photocathode has larger specific surface area, able to increase contact between electrolyte and electrode, reduce internal resistance of a battery, improve the electrocatalytic performance, and obtain higher photoelectric conversion performance when applied to dye sensitized solar energy batteries. And it has characters of simple preparing course and low cost, showing a potential application prospect of replacing Pt photocathode.
Description
Technical field
The present invention relates to the manufacturing of solar cell, particularly a kind of preparation method and application thereof that is applied to the porous acetylene black light cathode in the dye-sensitized solar cell.Specifically, it is by the spherical acetylene black electrode material with high conductivity and bigger serface, adopt spin coating technique, evenly be coated on the conductive glass, photocathode as dye sensitization solar battery, can increase ionogen with time interpolar contact, reduce the internal resistance of cell, obtain higher electro catalytic activity and opto-electronic conversion performance.
Background technology
Along with becoming increasingly conspicuous of shortage of resources and problem of environmental pollution, sun power more and more receives common people's concern as a kind of clean reproducible energy.Current, carrying out opto-electronic conversion by solar cell is one of main path of human use's sun power.In solar cell, high and technology maturation has occupied the share of solar cell 90% to silicon solar cell because of its turnover ratio, however silicon be solar cell because of its complex process, cost an arm and a leg material requirements harshness and be difficult to popularize.How to improve the photoelectric transformation efficiency of solar cell and effectively reduce its manufacturing cost, become the target that many solar cell working persons constantly pursue.
From Switzerland Gratzel in 1991 professor since making a breakthrough aspect dye sensitization solar battery (DSSC) research (O ' Regan, B.; Gr tzel, M.Nature 1991,353,737.), such battery demonstrates powerful commercial application prospect owing to have efficient, low cost, less energy-consumption, advantages of environment protection, becomes the focus that countries in the world are studied gradually.For this reason, both at home and abroad at time anode, ionogen to DSSC, continuous exploration has all been carried out in aspects such as production technique and battery structure.Wherein, the photocathode as the DSSC important component part plays catalytic reduction I
3 -With the effect of transfer transport, its electrocatalysis characteristic is to the opto-electronic conversion performance important influence of whole DSSC.At present, the DSSC photocathode mainly is to adopt precious metal material Pt to make catalysis electrode.Chinese patent CN1512599A announced and a kind ofly utilized organic surface active agent that the Pt particle is closely arranged in order at conductive glass surface, forms strong adhesive force again behind further sintering and has the nanostructure Pt catalysis electrode of high electrochemical activity.It is good that platinum electrode has a catalytic performance, the advantage that specific conductivity is high, yet its expensive price limit its practical application.Therefore, in recent years the research and development of low-cost and high-performance photocathode have been become the focus of people's concern.Chinese patent CN1697200A announced a kind of on a side of substrate an affixed nickel base alloy layer, an affixed again super thin metal layer provides a kind of catalytic counter electrodes with high catalytic activity, high conductivity, high light reflectivity, corrosion resistance and good on the outer side of nickel base alloy layer.Chinese patent CN1770401A has announced the mesoporous metal counter electrode of a kind of DSSC of being applied to, has improved efficient, has reduced cost, helps promoting the commercialization of this battery.
In recent years, the carbon material of high efficiency, low cost as: graphite, activated carbon, carbon nanotube etc. are because its high electroconductibility, and to I
-/ I
3 -Advantages of high catalytic activity, people's attention [N.Papageorgiou, Counter-electrode function in nanocrystalline photoelectrochemical cellconfigurations, Coord.Chem.Rev.2004 have been caused gradually, 248,1421-1446.].But yet there are no report both at home and abroad as the preparation of photocathode and the research and being applied in DSSC of electrocatalysis characteristic about spherical acetylene black.The spherical acetylene black that obtains through Pintsch process, have high electroconductibility and big specific surface area, adopt spin coating technique, evenly be coated in spherical acetylene black on the conductive glass, as the photocathode of DSSC, help increasing ionogen with time interpolar contact, reduce the internal resistance of cell, can improve its electro catalytic activity effectively, thereby obtain higher photoelectric transformation efficiency.Therefore: explore the preparation method of porous spherical acetylene black light cathode, and over-all properties and reduction battery cost that its electrocatalysis characteristic is studied for the raising dye sensitization solar battery have crucial meaning.
Summary of the invention
The purpose of this invention is to provide a kind of spherical acetylene black light cathode material and preparation method and application thereof.This acetylene black electrode material is a globosity, has bigger specific surface area, has increased ionogen and has contacted with interelectrode, reduces the internal resistance of cell, has improved electrocatalysis characteristic.
It is photocathode with porous spherical acetylene black film that another object of the present invention provides a kind of, and the dye-sensitized nano titanium dioxide film is the light anode, with I
-/ I
3 -Be the dye sensitization solar battery that ionogen constitutes, this dye sensitization solar battery has higher photoelectric transformation efficiency.
Spherical acetylene black light cathode material provided by the invention, it is by the spherical acetylene black granulometric composition, and its diameter is 50-100nm, and specific surface area is 280-300m
2/ g.
The preparation method of described spherical acetylene black be in tube furnace with high purity acetylene gas through Pintsch process, through following step:
1) at room temperature, being 99.99% argon gas with purity feeds in the tubular reactor with the speed of 5ml/min, is heated to 650 ℃.Be that 99.99% the acetylene gas flow with 5ml/min under 5MPa pressure imports in the tubular reactor subsequently with purity, reacted 2 hours.
2) reaction finishes after cool to room temperature takes out, and stirs 30min at normal temperatures with tensio-active agent ethylene glycol-Polyvinylpyrolidone (PVP) solution, uses absolute ethanol washing 3-5 time then, at 60-80 ℃ of vacuum-drying 2-4 hour, obtains the dispersive spherical acetylene black.The mass ratio of ethylene glycol and Polyvinylpyrolidone (PVP) is 55: 1.
Dye sensitization solar battery provided by the invention, comprise: the dye sensitization titanium dioxide photo anode, (acetonitrile and the methoxypropionitrile preparation in 1: 1 by volume of acetylene black light cathode and electrolytic solution, use 1 of 0.6M, 2-dimethyl-3-propyl imidazole iodine, 0.1M lithium iodide, 0.05M iodine, 0.5M tert .-butylpyridine make supporting electrolyte), it is characterized in that: described dye sensitization titanium dioxide photo anode comprises adulterated tin dioxide transparent conductive glass of fluorine (FTO) and nanocrystalline titanium dioxide film, sensitizing agent is cis-di (thiocyanato) bis (2,2 '-bipyridyl-4,4 '-dicarboxylate) ruthenium (II) (being called for short the N3 dyestuff), described acetylene black light cathode is that diameter is 50-100nm, and specific surface area is 280-300m
2The porous spherical acetylene black film of/g.
A kind of acetylene black light cathode provided by the invention is with spherical acetylene black ultra-sonic dispersion (spherical acetylene black and dehydrated alcohol mass volume ratio: 1: 1, mg/ml), adopt whirler, the uniform porous acetylene black film of formation on conductive glass in dehydrated alcohol.Concrete steps:
At room temperature, the spherical acetylene black ultra-sonic dispersion in dehydrated alcohol, is placed conductive glass on the whirler, drip the central position of this solution to conductive glass, under the rotating speed of 1000-5000r/min, rotation 15-60s, obtain one deck acetylene black film, then at 60 ℃ of dry 5min; Repeat rotation-drying process repeatedly, can obtain thickness is the acetylene black film of 0.1-50 μ m.
A kind of nanocrystalline titanium dioxide film of the present invention is to adopt the method for silk screen printing that titania slurry is coated on the FTO, through high temperature sintering, and the about 10 μ m of thickness.Subsequently the nanocrystalline titanium dioxide film that makes is immersed in 3 * 10
-4In the ethanolic soln of the N3 dyestuff of M.
DSSC among the present invention is the sandwich structure battery, its making method: between dye sensitization titanium dioxide photo anode and acetylene black light cathode, add sealing membrane (for example " surlyn " thermoplastic polymer film), by dull and stereotyped pressing machine heating and pressurization, two electrodes are bonded together fully, utilize vacuum or manual method to inject electrolyte solution at the photocathode dorsal pore then, and hermetic electrolyte matter is injected aperture.This battery is at AM1.5-100mW/cm
2Light intensity under test, gather photoelectric current, photovoltage with U.S. Keithley2400 digital source table.
Prepared porous spherical acetylene black electrode is assembled into the sheet cell structure among the present invention, and two identical electrodes separate with sealing membrane, and spacing is 60 μ m.Electro-chemical test carries out under 25 ℃ of room temperatures.Electro catalytic activity is measured and is used U.S. PARSTAT2273 impedance test system.
The invention has the advantages that and adopt cheap spherical acetylene black to substitute the catalysis photocathode of precious metals pt as DSSC, because spherical acetylene black has higher electroconductibility and bigger specific surface area, can increase ionogen effectively and contact, reduce the internal resistance of cell, I with interelectrode
-/ I
3 -Have higher electrocatalysis characteristic, and have higher photoelectric transformation efficiency, demonstrate the application prospect that potential substitutes the Pt photocathode.
Description of drawings
The Electronic Speculum figure of the porous spherical acetylene black light cathode that Fig. 1 makes for embodiment 2; (a) low range scanning electron microscope analysis (b), (c) high magnification scanning electron microscope analysis (d) TEM (transmission electron microscope) analysis.
Fig. 2 is the Electronic Speculum figure of the titanium dioxide film of embodiment 4 making; (a) cross section scanning electron microscope analysis (b) film surface scan electronic microscope photos.
Fig. 3 is the dye sensitization solar battery structural representation that embodiment 5 makes.
Fig. 4 is the I-V curve of dye sensitization solar battery under different catalytic carriers that embodiment 5 makes.
Fig. 5 is the testing impedance battery structure synoptic diagram that embodiment 8 makes.
Fig. 6 is the impedance spectrogram of the testing impedance battery of embodiment 8 making at different acetylene black thickness.
Fig. 7 is the impedance match equivalent-circuit diagram of embodiment 8 tests.
Embodiment
Embodiment 1: the preparation of spherical acetylene black
At room temperature, being 99.99% argon gas with purity feeds in the tubular reactor with the speed of 5ml/min, continues 30min, and is heated to 650 ℃.Be that 99.99% the acetylene gas flow with 5ml/min under 5MPa pressure imports in the tubular reactor with purity with the 10min time subsequently, reacted 2 hours.Reaction finishes after cool to room temperature takes out, and weighing is 52mg, and productive rate is 97%; With 25ml tensio-active agent ethylene glycol (EG)-(wherein the PVP quality is 0.5g to Polyvinylpyrolidone (PVP) (PVP) solution, account for the surfactant soln total mass 1.7%) stir 30min at normal temperatures, use absolute ethanol washing then 4 times, 60 ℃ of vacuum-dryings 4 hours, promptly obtain the dispersive spherical acetylene black.
Embodiment 2: the preparation of porous spherical acetylene black light cathode
At room temperature, ultrasonic (ultrasound condition: 40kHz, 300W 5min) are dispersed in the dehydrated alcohol of 20ml with the 20mg spherical acetylene black; Conductive glass is placed on the whirler, drip this solution to the central position of conductive glass with sample injector, under the rotating speed of 1000r/min, rotation 30s obtains one deck acetylene black film, then at 60 ℃ of dry 5min; Repeat above rotation-drying process repeatedly, can obtain thickness is the acetylene black film of 20 μ m.
Embodiment 3: the mensuration of porous spherical acetylene black
Fig. 1 a is the scanning electron microscope analysis of the porous spherical acetylene black light cathode of embodiment 2 described method preparations, (Fig. 1 a) shows: on the evengranular FTO of the being dispersed in conductive glass of acetylene black and form the film of thickness homogeneous, further the sem analysis that amplifies can observe film vesicular structure (Fig. 1 b, 1c).Tem analysis (Fig. 1 d) has confirmed that further product is a globosity, and its diameter is 50-100nm.Specific surface is measured and is shown that the specific surface area of porous spherical acetylene black is 280-300m
2/ g.
Embodiment 4:
The making of dye sensitization titanium dioxide film: the method that adopts silk screen printing is titania slurry (prescription: 16wt% titanium dioxide powder (P25 type, the production of Germany Degussa company), 4wt% ethyl cellulose, 80wt% Terpineol 350) be coated in equably on the FTO conductive glass, through 450 ℃ of high temperature sintering 30min, naturally cool to room temperature, with 50mM TiCl4 solution-treated 30min, with distilled water, alcohol flushing surface, nitrogen dries up, again through 450 ℃ of high temperature sintering 30min.Obtain the poriferous titanium dioxide film (Fig. 2) that thickness is about 10 μ m.Be 3 * 10 with the titanium dioxide film that obtains in concentration subsequently
-4Soaked 12 hours in the ethanolic soln of the N3 dyestuff of M, take out the back and clean with dehydrated alcohol, nitrogen dries up.
Embodiment 5:
DSSC battery assembling: add sealing membrane (for example " surlyn " thermoplastic polymer film) between porous acetylene black light cathode (the acetylene black thickness is 20 μ m) that will make according to embodiment 2 and the dye sensitization titanium dioxide photo anode that makes according to embodiment 4, under dull and stereotyped pressing machine, be heated to 100 ℃, heated sealant 20min, two electrodes are bonded together fully, utilize vacuum or manual method to inject electrolyte solution at the photocathode dorsal pore then, and sealing.The structure iron of this cell apparatus is seen Fig. 3.The number in the figure meaning is: 1, transparent conducting glass; 2, semiconductor nano epitaxial; 3, photosensitizer; 4, ionogen; 5, porous acetylene black film; 6, conductive glass; 7, barrier film.The effective illuminating area of this battery is: 0.16cm
2, at AM1.5-100mW/cm
2Light intensity under test, adopt U.S. Keithley 2400 digital source tables to gather photoelectric current, photovoltage, the short-circuit current of acquisition (Jsc), open circuit voltage (Voc), packing factor (FF) and photoelectric efficiency are respectively 13.92mAcm
-2, 724mV, 0.57,5.76%.
Embodiment 6:
Embodiment 7:
Fig. 4 is for making photoelectric current (I)-photovoltage (V) graphic representation of DSSC photocathode respectively with acetylene black (AB)/FTO, platinum (Pt)/FTO and FTO according to embodiment 5.As can be seen from the figure: of the present inventionly make the DSSC of photocathode at AM1.5-100mW/cm with porous spherical acetylene black film
2Under the light intensity, obtained 5.76% photoelectric efficiency; Short-circuit current (Jsc), open circuit voltage (Voc) and packing factor (FF) are respectively 13.92mAcm
-2, 724mV, 0.57.
As a comparison: with 1.5 * 10
-2Mol/L H
2PtCl
6Aqueous isopropanol, be applied on the FTO conductive glass with spin-coating method, as in the retort furnace, 390 ℃ of sintering 30min make H after the drying at room temperature
2PtCl
6Thermolysis taking place generate platinum on the FTO surface, makes the Pt/FTO electrode.Adopt electrolytic solution and the test condition identical, obtained 7.18% photoelectric efficiency with embodiment 5.Obtained 0.25% photoelectric efficiency with FTO as counter electrode under the similarity condition.Data in the associative list 1 are as can be seen: the DSSC that makes photocathode with porous spherical acetylene black of the present invention has higher opto-electronic conversion performance.
The photoelectric properties of table 1 dye sensitization solar battery under different photocathodes
| Voc(mV) | Jsc(mA/cm 2) | FF | η(％) | |
| Pt/FTO AB/FTO FTO | 728 724 651 | 15.26 13.92 2.89 | 0.65 0.57 0.14 | 7.18 5.76 0.25 |
Embodiment 8:
Fig. 5 has provided the structure iron that is assembled into sheet cell according to embodiment 2 prepared different thickness porous spherical acetylene black electrodes, and the number in the figure meaning is: 1, conductive glass; 2, porous acetylene black film; 3, ionogen; 4, porous acetylene black film; 5, conductive glass; 6, barrier film.Two interelectrode distances are 60 μ m, are electrolytic solution with embodiment 6.Electro-chemical test carries out under 25 ℃ of room temperatures.Electro catalytic activity is measured and is adopted U.S. PARSTAT 2273 impedance test systems.The electrochemical AC impedance spectrum of different AB thickness as shown in Figure 6.Its equivalent circuit Fig. 7, fitting result sees Table 2.Wherein HFS is charge migration resistance (Rct), and low frequency part is by diffusion (Zw) control.Bibliographical information: DSSC will show excellent photoelectric performance, and the Rct of its photocathode should be less than 10 Ω cm
2[A.Hauch, A.Georg, Electrochim.Acta2001,46,3457].Data as can be seen from table: when acetylene black thickness was 20 μ m, its charge transfer resistance (Rct) was 7.9 Ω cm
2, show that acetylene black light cathode of the present invention has good catalytic action.
The electrochemical AC impedance fitting result of the different thickness photocathodes of table 2
| Thickness/μm | RCT/Ωcm 2 | Rs/Ωcm 2 |
| 0.7 5 10 20 25 | 20.0 14.3 12.6 7.9 9.1 | 5.39 5.46 6.08 6.78 7.46 |
By the porous acetylene black light cathode is carried out photoelectric properties and electrochemical property test, as can be seen: when porous acetylene black light cathode thickness of the present invention is 20 μ m, to I
-/ I
3 -Have higher electro catalytic activity, be applied among the DSSC, obtained 5.76% photoelectric transformation efficiency.This comes from the structural characteristics of spherical acetylene black electrode material: as the spherical acetylene black of photocathode catalytic active substance, because its high electroconductibility and bigger specific surface area can increase ionogen effectively and contact with interelectrode, reduce the internal resistance of cell, improve I
-/ I
3 -With the electron exchange performance of photocathode, thereby guarantee effectively carrying out of DSSC opto-electronic conversion.Simple, with low cost characteristics that porous acetylene black light cathode provided by the invention has preparation process demonstrate the application prospect that potential substitutes the Pt photocathode.
Claims (10)
1, a kind of acetylene black electrode material is characterized in that it is made up of spherical acetylene black, and its diameter is 50-100nm, and specific surface area is 280-300m
2/ g.
2, the preparation method of the described acetylene black electrode material of claim 1, it be in tube furnace with high purity acetylene gas through Pintsch process, it is characterized in that through following step:
1) at room temperature, being 99.99% argon gas with purity feeds in the tubular reactor with the speed of 5ml/min, being heated to 650 ℃, is that acetylene gas flow with 5ml/min under 5MPa pressure of 99.99% imports in the tubular reactor subsequently with purity, reacts 2 hours;
2) reaction finishes after cool to room temperature takes out the back and under agitation handles with tensio-active agent, uses absolute ethanol washing 3-5 time then, at 60-80 ℃ of vacuum-drying 2-4 hour, obtains the dispersive spherical acetylene black.
3,, it is characterized in that described tensio-active agent is ethylene glycol-Polyvinylpyrolidone (PVP) solution according to the preparation method of the described acetylene black electrode material of claim 2.
4, according to the preparation method of the described acetylene black electrode material of claim 3, the mass ratio that it is characterized in that described tensio-active agent ethylene glycol and Polyvinylpyrolidone (PVP) is 55: 1.
5, a kind of preparation method who prepares the described acetylene black electrode material photocathode of claim 1, it is to adopt spin coating technique, it is characterized in that through following step:
At room temperature, the spherical acetylene black ultra-sonic dispersion in dehydrated alcohol, is placed conductive glass on the whirler, drip the central position of this solution to conductive glass, under the rotating speed of 1000-5000r/min, rotation 15-60s, obtain one deck acetylene black film, then at 60 ℃ of dry 5min; Repeat rotation-drying process repeatedly, can obtain thickness is the acetylene black film of 0.1-50 μ m.
6,, it is characterized in that the quality of described spherical acetylene black and dehydrated alcohol and volume ratio are 1: 1 according to the preparation method of the described acetylene black electrode material photocathode of claim 5.
7, a kind of dye sensitization solar battery, it comprises light anode, photocathode, thermoplastic barrier film and electrolytic solution, it is characterized in that:
Described smooth anode is the dye sensitization titanium dioxide photo anode, and it comprises base material FTO conductive glass, and nano titanium dioxide film, photosensitizer are the N3 dyestuff;
Described photocathode is an acetylene black light cathode, comprises spherical acetylene black electrode material and base material FTO conductive glass, and the diameter of described spherical acetylene black is 50-100nm, and specific surface area is 280-300m
2/ g;
The prescription of described electrolytic solution is: in the solvent of 1: 1 acetonitrile of volume ratio and methoxypropionitrile, add 1 of 0.6M, and 2-dimethyl-3-propyl imidazole iodine, the lithium iodide of 0.1M, the iodine of 0.05M and the tert .-butylpyridine of 0.5M are made supporting electrolyte.
8, according to the described dye sensitization solar battery of claim 7, the preparation method who it is characterized in that described dye sensitization titanium dioxide photo anode is through following step:
Method by silk screen printing is coated in titania slurry on the FTO conductive glass equably, through 450 ℃ of high temperature sintering 30min, naturally cools to room temperature, uses 50mMTiCl
4Solution-treated 30min, with distilled water, alcohol flushing surface, nitrogen dries up; Through 450 ℃ of high temperature sintering 30min, obtain the porous-film that thickness is about 10 μ m again; Subsequently with the titanium dioxide film that obtains 3 * 10
-4Soaked 12 hours in the ethanolic soln of the N3 dyestuff of M, take out the back and clean with dehydrated alcohol, nitrogen dries up.
9, according to the described dye sensitization solar battery of claim 8, it is characterized in that the mass percent of described titania slurry is formed: 16% titanium dioxide powder, 4% ethyl cellulose and 80% Terpineol 350.
10, the preparation method of the described dye sensitization solar battery of claim 7, it is characterized in that it being: between dye sensitization titanium dioxide photo anode and acetylene black light cathode, add sealing membrane through following step, by dull and stereotyped pressing machine heating and pressurization, two electrodes are bonded together fully, utilize vacuum or manual method to inject electrolyte solution at the photocathode dorsal pore then, and hermetic electrolyte matter is injected aperture.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102002724A (en) * | 2010-04-23 | 2011-04-06 | 盛义平 | Acetylene black cathode provided with waterproof membrane and used for producing hydrogen peroxide and manufacturing method thereof |
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|---|---|---|---|---|
| CN102002724A (en) * | 2010-04-23 | 2011-04-06 | 盛义平 | Acetylene black cathode provided with waterproof membrane and used for producing hydrogen peroxide and manufacturing method thereof |
| CN102002724B (en) * | 2010-04-23 | 2011-08-17 | 盛义平 | Acetylene black cathode provided with waterproof membrane and used for producing hydrogen peroxide and manufacturing method thereof |
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