CN100541822C - DSSC of a kind of nano-crystal film and preparation method thereof - Google Patents
DSSC of a kind of nano-crystal film and preparation method thereof Download PDFInfo
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- CN100541822C CN100541822C CNB2007100370687A CN200710037068A CN100541822C CN 100541822 C CN100541822 C CN 100541822C CN B2007100370687 A CNB2007100370687 A CN B2007100370687A CN 200710037068 A CN200710037068 A CN 200710037068A CN 100541822 C CN100541822 C CN 100541822C
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/542—Dye sensitized solar cells
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
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Abstract
The invention belongs to technical field of solar batteries, be specially a kind of its in containing nano-crystal film dye sensitized nano crystal salar battery of texture channel and preparation method thereof.In this solar cell, at the broad stopband of absorption photosensitizer Nano semiconductor film surface covering one deck liquid state, accurate solid-state or solid electrolyte, electrolytical opposite side is the electro-conductive glass that is coated with platinum layer, forms sandwich shape.Wherein, the nano-crystal film that contains texture channel relies on the channel design that self exists, and makes electrolyte be easy to be diffused into the film depths, has improved the interface contact between electrolyte and the film effectively, has improved the photoelectric conversion efficiency of DSSC.
Description
Technical field
This invention belongs to technical field of solar batteries, is specifically related to dye sensitized nano crystal salar battery of a kind of nano-crystal film and preparation method thereof.
Background technology
The our times rapid economy development has benefited from fossil energy, as the input widely and the application of oil, natural gas, coal and nuclear fission energy.Yet fossil energy will be in the promptly approaching exhaustion of the 21 century first half.In addition, the consumption of fossil energy can produce a large amount of pollutions simultaneously, causes environment to go from bad to worse.Overcome the only way of energy crisis and solution problem of environmental pollution---greatly develop regenerative resource, mainly contain: the utilization of (1) solar energy, (2) small power station and tidal power generation, (3) wind power generation.Wherein solar energy is with the largest potentiality, is optimal new forms of energy.According to estimates, to offer the energy of the earth be 3.2 * 10 to the annual sun
24J is about as much as human annual catabiotic 10000 times at present.Exploitation and to use solar cell be one of important channel that utilizes solar energy if be that 10% solar cell covers 0.1% earth surface with photoelectric conversion efficiency, just is enough to satisfy the present whole mankind's energy needs.Although accounting for the solar cell of main flow at present mainly is monocrystalline silicon, polysilicon, non-crystal silicon solar cell, because complicated preparation technology and too high production cost have limited its extensive use in daily life.The exploitation high efficiency, solar cell has now become the emphasis of countries in the world government energy research cheaply.
Copy plant chlorophyll photosynthesis principle to prepare solar cell is human dream always, the Michael of Lausanne, SUI university in 1991
A kind of dye sensitized nano crystal salar battery that people such as professor propose just is based on the solar cell of this principle development, and this battery cost is low and efficient is also higher.Dye sensitized nano crystal salar battery is mainly formed by transparent conduction base sheet, porous nano crystallized semiconductor thin film, dye sensitizing agent, electrolyte solution (containing super sensitizer) with to electrode.Carry out photosynthetic place-chlorophyll structure with plant and compare, dye sensitized nano crystal salar battery has similar structure.Its nano crystal semiconductor network configuration is equivalent to the thylakoid in the chlorophyll, plays a part to support the sensitizer dye molecule, increases the area that absorbs sunlight and transmits electronics; Dye molecule is equivalent to the chlorophyll in the chlorophyllinite, plays a part to absorb the sunlight photon.Because the porous nano crystallized semiconductor thin film has very large specific area, can adsorb a large amount of sensitising agents, thereby can absorb sunlight effectively, causes photoelectric conversion efficiency to reach more than 10%.At present, the electrolyte of dye sensitized nano crystal salar battery mainly is to contain I
3 -/ I
2Organic solvents such as the acetonitrile of oxidation-reduction pair, but liquid organic electrolyte exists problems such as solvent evaporates, leakage, flammable and high temperature instability, has a strong impact on the long-time stability of battery.Therefore people attempt adopting some accurate solid-state or solid electrolytes to replace liquid organic electrolyte.Yet with respect to liquid organic electrolyte, accurate solid-state or solid electrolyte is not easy to enter traditional nanometer crystal semiconductor film depths, has caused relatively poor interface contact.And contact of the interface between dye sensitized nano crystal semiconductive thin film and the electrolyte and interfacial reaction are one of principal elements of decision cell photoelectric conversion efficiency.Because interface contact is relatively poor, the photoelectric conversion efficiency of accurate solid-state, solid-state dye sensitized nano crystal salar battery is well below the efficient of liquid battery.People mainly modify accurate solid-state, solid electrolyte by some inorganic (titanium dioxide, silicon dioxide) nano particles of adding, oligomer at present, thereby improve the interface contact and improve photoelectric conversion efficiency.But the interface contact is desirable not enough, needs further to improve.
Summary of the invention
The object of the present invention is to provide a kind of electricity conversion height, can be applicable to nano-crystal film DSSC of liquid state, accurate solid-state or solid electrolyte and preparation method thereof.
Nano-crystal film DSSC provided by the invention, by liquid or the accurate solid-state or solid electrolyte of the broad stopband nanometer crystal semiconductor film surface coverage one deck that contains texture channel that has adsorbed photosensitizer, electrolytical opposite side is the electro-conductive glass that is coated with platinum layer, forms sandwich shape; Wherein, the described nanometer crystal semiconductor film that has adsorbed photosensitizer is a work electrode, and the electro-conductive glass of platinum plating layer is to electrode.Its structure as shown in Figure 1.
Among the present invention, the described broad stopband nanometer crystal semiconductor film thickness that contains texture channel is the 1-50 micron.
Among the present invention, described nanometer crystal semiconductor film can be titanium deoxid film, zinc-oxide film or SnO 2 thin film.
Among the present invention, described photosensitizer (dyestuff) can adopt cis-two thiocyanate radical-two (4,4 '-dicarboxylic acids-2,2 ' bipyridine) closes ruthenium cis-dithiocyanato bis (4,4 '-dicarboxy-2,2 '-bipyridine) ruthenium (being called for short the N3 dyestuff) and cis-two thiocyanate radical-4,4 '-dicarboxylic acids-2,2 ' bipyridine-4,4 '-dinonyl-2,2 ' bipyridine closes ruthenium cis-dithiocyanato4,4 '-dicarboxy-2,2 '-bipyridine-4,4 '-dinonyl-2,2 '-bipyridine ruthenium (being called for short the Z907 dyestuff).
Among the present invention, described liquid electrolyte is a 0.5M iodine, the 1-methyl of 0.45M N-tolimidazole-3-propyl imidazole iodized salt solution; Described quasi-solid electrolyte is mixed with nano SiO 2 particle by aforementioned liquid electrolyte and forms, and nano SiO 2 particle accounts for the 4-8% of electrolyte total weight.Described solid electrolyte can be the solid electrolyte of common solar cell.
Among the present invention, there is channel design in the nanometer crystal semiconductor film self that contains texture channel, the depths that is diffused into film for liquid, accurate solid-state or solid electrolyte provides transmission channel, has improved interface contact and interfacial reaction effectively, has greatly improved electricity conversion.
The preparation method of the DSSC of the nano-crystal film that the present invention proposes is as follows: will contain the nanometer crystal semiconductor film dye sensitization of texture channel, on film surface, cover liquid or the accurate solid-state or solid electrolyte of one deck again, the electro-conductive glass that is coated with platinum layer places electrolytical opposite side, entire cell is formed sandwich shape, and its structure as shown in Figure 1.Wherein, the titanium dioxide nanocrystalline film of dye sensitization is a work electrode, and the electro-conductive glass of platinum plating layer is to electrode, and carries out simplified package.
Among the present invention, the preparation process that the nanometer that contains texture channel is partly led epitaxial not is as follows: 10-500 milligram metallic compound nano particle or monodimension nanometer material are mixed with 50-200 grams per liter Nano semiconductor (as titanium dioxide, zinc oxide, the tin oxide) colloid of 5-20 milliliter.Wherein, metallic compound is oxide, sulfide, hydroxide, phosphate, the carbonate of zinc, aluminium, iron, copper, magnesium, calcium, chromium, nickel.Their monodimension nanometer material can be nano wire, nanometer rods, nanotube or nano wire.Then colloid is covered on the substrate by coating or silk screen printing or other thin film-forming method, 200-600 ℃ of following roasting 15 minutes to 12 hours, cooling, repetitive operation is until the broad stopband nanometer crystal semiconductor film that obtains the 1-50 micron.Wherein substrate adopts transparent conductive substrate, mixes the tin ash electro-conductive glass of fluorine as employing.Utilize acid or alkali that the nano particle or the monodimension nanometer material of metallic compound are etched away subsequently, nano material is removed the back fully and produce corresponding nano-pore in film, forms the passage that contains texture, and this Kong Kedao is as electrolyte channels.
Among the present invention, the dye sensitization step is as follows: Nano semiconductor (as the titanium dioxide) epitaxial (putting into baking oven) of above-mentioned preparation was heated 10-120 minute down in 100-250 ℃, then cooling; Being immersed in concentration when being cooled to 25-100 ℃ is 10
-5-10
-3Sensitization in 2-48 hour among the N3 of mol or the Z907.
In the said method, etching metallic compound nano material (nanometer fruit grain or monodimension nanometer material) means can be by acid, alkali or Microwave Treatment, perhaps soaked in solvent.
Description of drawings
Fig. 1 is based on the structural representation of the DSSC of the nano-crystal film that contains texture channel.
Number in the figure, the 101-electro-conductive glass, the semiconductive thin film of 102-densification, the 103-sunlight, the 104-load, the nano crystal semiconductor epitaxial that contains texture channel that the 105-dyestuff covers, 106-electrolyte, 107-are coated with the electro-conductive glass of platinum layer.
Embodiment
Below in conjunction with specific embodiment technical scheme of the present invention is further described.
Embodiment 1
120 grams per liter nano titanium oxide colloidal dispersions of 165 milligrams of zinc oxide nanowires and 10 milliliters are mixed.Subsequently colloid is coated on the fine and close titanium deoxid film, 450 ℃ of following roastings 30 minutes, repetitive coatings and roasting process again were 10 microns nano titanium oxide epitaxial until obtaining thickness.This membrane electrode is immersed 0.5 of heat (75 ℃) rub/rise and soaked 48 hours in the hydrochloric acid solution, be removed fully up to zinc oxide nanowire.This electrode is put into titanium tetrachloride solution soak,, afterwards electrode is soaked sensitization in 12 hours in the acetonitrile of 3 * 10-4 mol Z907 dyestuff and butanol solution subsequently again 450 ℃ of following roastings 15 minutes.
Dye sensitization titanium dioxide nanocrystalline film with above-mentioned preparation is a negative electrode respectively, and the electro-conductive glass that is coated with platinum layer adopts a kind of quasi-solid electrolyte to come assembled battery for to electrode.Electrolyte is ion liquid based gel, by nano SiO 2 particle (5wt%) and ionic liquid (0.5M iodine, the 1-methyl of 0.45M N-tolimidazole-3-propyl imidazole iodized salt solution) is mixed.
Optical Electro-Chemistry is measured according to two traditional electrode systems and is measured, radiation source be 1000W solar simulator (1.5AM) (Oriel, USA).Photoelectric current and photovoltage output are measured by Keithley2400 digital source table (U.S. Keithley company).
The cell photoelectric conversion efficiency that is assembled into traditional titanium dioxide nanocrystalline film is 5.0%, and is 6.1% with the battery efficiency that the titanium dioxide nanocrystalline film that contains texture channel is assembled into, and has improved 22%.
Thereby, use the titanium dioxide nanocrystalline film that contains texture channel can greatly improve the performance of accurate solid-state or solid-state dye sensitized nano crystal salar battery.
Embodiment 2
The 100 grams per liter nano titanium oxide colloidal dispersions of 100 milligrams of aluminium hydrate nano rods with 10 milliliters are mixed.Subsequently colloid is coated on the fine and close titanium deoxid film, 600 ℃ of following roastings 10 minutes, repetitive coatings and roasting process again were 15 microns nano titanium oxide epitaxial until obtaining thickness.This membrane electrode is immersed 0.5 of heat (75 ℃) rub/rise and soaked 40 hours in the sodium hydroxide solution, be removed fully up to the aluminium hydrate nano rod.This electrode is put into titanium tetrachloride solution soaks, subsequently again 300 ℃ of following roastings 40 minutes, afterwards with electrode 10
-5Soak sensitization in 20 hours in the acetonitrile of mol N3 dyestuff and the butanol solution.
Dye sensitization titanium dioxide nanocrystalline film with above-mentioned preparation is a negative electrode respectively, and the electro-conductive glass that is coated with platinum layer has adopted a kind of liquid electrolyte to come assembled battery for to electrode.Liquid electrolyte is a 0.5M iodine, the 1-methyl of 0.45M N-tolimidazole-3-propyl imidazole iodized salt solution.
Optical Electro-Chemistry is measured according to two traditional electrode systems and is measured, radiation source be 1000W solar simulator (1.5AM) (Oriel, USA).Photoelectric current and photovoltage output are measured by Keithley2400 digital source table (U.S. Keithley company).
The cell photoelectric conversion efficiency that is assembled into traditional titanium dioxide nanocrystalline film is 5.4%, and is 5.9% with the battery efficiency that the titanium dioxide nanocrystalline film that contains texture channel is assembled into, and has improved 9%.
Embodiment 3
120 grams per liter nano titanium oxide colloidal dispersions of 50 milligrams of iron oxide nano-wires and 10 milliliters are mixed.Subsequently colloid is coated on the fine and close titanium deoxid film, 350 ℃ of following roastings 30 minutes, repetitive coatings and roasting process again were 10 microns nano titanium oxide epitaxial until obtaining thickness.This membrane electrode is immersed 0.5 of heat (75 ℃) rub/rise and soaked 48 hours in the hydrochloric acid solution, be removed fully up to iron oxide nano-wire.This electrode is put into titanium tetrachloride solution soaks, subsequently again 400 ℃ of following roastings 30 minutes, afterwards with electrode 10
-5Soak sensitization in 8 hours in the acetonitrile of mol N3 dyestuff and the butanol solution.
Dye sensitization titanium dioxide nanocrystalline film with above-mentioned preparation is a negative electrode respectively, and the electro-conductive glass that is coated with platinum layer has adopted a kind of quasi-solid electrolyte to come assembled battery for to electrode.Electrolyte is ion liquid based gel, by nano SiO 2 particle (5wt%) and ionic liquid (0.5M iodine, the 1-methyl of 0.45M N-tolimidazole-3-propyl imidazole iodized salt solution) is mixed.
Optical Electro-Chemistry is measured according to two traditional electrode systems and is measured, radiation source be 1000W solar simulator (1.5AM) (Oriel, USA).Photoelectric current and photovoltage output are measured by Keithley2400 digital source table (U.S. Keithley company).
The cell photoelectric conversion efficiency that is assembled into traditional titanium dioxide nanocrystalline film is 5.0%, and is 5.7% with the battery efficiency that the titanium dioxide nanocrystalline film that contains texture channel is assembled into, and has improved 14%.
Embodiment 4
120 grams per liter nano titanium oxide colloidal dispersions of 165 milligrams of copper sulfide nano mitrons and 10 milliliters are mixed.Subsequently colloid is coated on the fine and close titanium deoxid film, 450 ℃ of following roastings 30 minutes, repetitive coatings and roasting process again were 10 microns nano titanium oxide epitaxial until obtaining thickness.This membrane electrode is immersed 0.5 of heat (75 ℃) rub/rise and soaked 48 hours in the hydrochloric acid solution, be removed fully up to the copper sulfide nano mitron.This electrode is put into titanium tetrachloride solution soaks, subsequently again 450 ℃ of following roastings 15 minutes, afterwards with electrode 10
-4Soak sensitization in 12 hours in the acetonitrile of mol N3 dyestuff and the butanol solution.
Dye sensitization titanium dioxide nanocrystalline film with above-mentioned preparation is a negative electrode respectively, and the electro-conductive glass that is coated with platinum layer has adopted a kind of quasi-solid electrolyte to come assembled battery for to electrode.Electrolyte is ion liquid based gel, by nano SiO 2 particle (5wt%) and ionic liquid (0.5M iodine, the 1-methyl of 0.45M N-tolimidazole-3-propyl imidazole iodized salt solution) is mixed.
Optical Electro-Chemistry is measured according to two traditional electrode systems and is measured, radiation source be 1000W solar simulator (1.5AM) (Oriel, USA).Photoelectric current and photovoltage output are measured by Keithley2400 digital source table (U.S. Keithley company).
The cell photoelectric conversion efficiency that is assembled into traditional titanium dioxide nanocrystalline film is 5.0%, and is 5.6% with the battery efficiency that the titanium dioxide nanocrystalline film that contains texture channel is assembled into, and has improved 12%.
Embodiment 5
120 grams per liter nano titanium oxide colloidal dispersions of 300 milligrams of magnesium carbonate and calcium carbonate nano granulate mixture and 10 milliliters are mixed.Subsequently colloid is coated on the fine and close titanium deoxid film, 450 ℃ of following roastings 30 minutes, repetitive coatings and roasting process again were 10 microns nano titanium oxide epitaxial until obtaining thickness.This membrane electrode is immersed 0.5 of heat (75 ℃) rub/rise and soaked 48 hours in the hydrochloric acid solution, be removed fully up to magnesium carbonate and calcium carbonate nano particle.This electrode is put into titanium tetrachloride solution soaks, subsequently again 450 ℃ of following roastings 15 minutes, afterwards with electrode 10
-5Soak sensitization in 12 hours in the acetonitrile of mol N3 dyestuff and the butanol solution.
Dye sensitization titanium dioxide nanocrystalline film with above-mentioned preparation is a negative electrode respectively, and the electro-conductive glass that is coated with platinum layer has adopted a kind of quasi-solid electrolyte to come assembled battery for to electrode.Electrolyte is ion liquid based gel, by nano SiO 2 particle (5wt%) and ionic liquid (0.5M iodine, the 1-methyl of 0.45M N-tolimidazole-3-propyl imidazole iodized salt solution) is mixed.
Optical Electro-Chemistry is measured according to two traditional electrode systems and is measured, radiation source be 1000W solar simulator (1.5AM) (Oriel, USA).Photoelectric current and photovoltage output are measured by Keithley2400 digital source table (U.S. Keithley company).
The cell photoelectric conversion efficiency that is assembled into traditional titanium dioxide nanocrystalline film is 5.0%, and is 5.8% with the battery efficiency that the titanium dioxide nanocrystalline film that contains texture channel is assembled into, and has improved 16%.
Embodiment 6
120 grams per liter nano titanium oxide colloidal dispersions of 20 milligrams of chromium phosphate nano wires and nickel hydroxide nano line mixture and 10 milliliters are mixed.Subsequently colloid is coated on the fine and close titanium deoxid film, 450 ℃ of following roastings 30 minutes, repetitive coatings and roasting process again were 10 microns nano titanium oxide epitaxial until obtaining thickness.This membrane electrode is immersed 0.5 of heat (75 ℃) rub/rise and soaked 48 hours in the hydrochloric acid solution, be removed fully up to chromium phosphate and nickel hydroxide nano line.This electrode is put into titanium tetrachloride solution soaks, subsequently again 450 ℃ of following roastings 15 minutes, afterwards with electrode 10
-3Soak sensitization in 12 hours in the acetonitrile of mol N3 dyestuff and the butanol solution.
Dye sensitization titanium dioxide nanocrystalline film with above-mentioned preparation is a negative electrode respectively, and the electro-conductive glass that is coated with platinum layer has adopted a kind of quasi-solid electrolyte to come assembled battery for to electrode.Electrolyte is ion liquid based gel, by nano SiO 2 particle (5wt%) and ionic liquid (0.5M iodine, the 1-methyl of 0.45M N-tolimidazole-3-propyl imidazole iodized salt solution) is mixed.
Optical Electro-Chemistry is measured according to two traditional electrode systems and is measured, radiation source be 1000W solar simulator (1.5AM) (Oriel, USA).Photoelectric current and photovoltage output are measured by Keithley2400 digital source table (U.S. Keithley company).
The cell photoelectric conversion efficiency that is assembled into traditional titanium dioxide nanocrystalline film is 5.0%, and is 5.7% with the battery efficiency that the titanium dioxide nanocrystalline film that contains texture channel is assembled into, and has improved 14%.
Claims (5)
1, a kind of preparation method of DSSC of nano-crystal film, it is characterized in that concrete steps are as follows: will contain the nanometer crystal semiconductor film dye sensitization of texture channel, on film surface, cover liquid or the accurate solid-state or solid electrolyte of one deck again, the electro-conductive glass that is coated with platinum layer places electrolytical opposite side, and entire cell is formed sandwich shape; The nanometer crystal semiconductor film of dye sensitization is a work electrode, and the electro-conductive glass of platinum plating layer is to electrode, and encapsulates; Wherein:
The used photosensitizer of described dye sensitization is N
3Dyestuff or Z907 dyestuff;
It is as follows that the described nanometer that contains texture channel is partly led the preparation process of stopping epitaxial: step 1, at first 10-500 milligram metallic compound nano particle or monodimension nanometer material are mixed with the 50-200 grams per liter Nano semiconductor colloid of 5-20 milliliter; Wherein, metallic compound is oxide, sulfide, hydroxide, phosphate or the carbonate of zinc, aluminium, iron, copper, magnesium, calcium, chromium, nickel; Step 2 covers colloid on the substrate by coating or silk screen printing thin film-forming method then, 200-600 ℃ of following roasting 15 minutes to 12 hours, and cooling, the repetitive operation step 2 is until the broad stopband nanometer crystal semiconductor film that obtains the 1-50 micron; Step 3 utilizes acid or alkali that the nano particle or the monodimension nanometer material of metallic compound are etched away at last, and nano material is removed the back fully and produce corresponding nano-pore in film, forms the passage that contains texture; Described monodimension nanometer material is nano wire, nanometer rods, nanotube or nano wire.
2, preparation method according to claim 1 pond is characterized in that described nanometer crystal semiconductor film can be titanium deoxid film, zinc-oxide film or SnO 2 thin film.
3, preparation method according to claim 1 is characterized in that described nanometer crystal semiconductor film thickness is the 1-50 micron.
4, preparation method according to claim 1 is characterized in that described liquid electrolyte is a 0.5M iodine, the 1-methyl of 0.45MN-tolimidazole-3-propyl imidazole iodized salt solution; Described quasi-solid electrolyte is mixed with nano SiO 2 particle by aforementioned liquid electrolyte and forms, and nano SiO 2 particle accounts for the 4-8% of electrolyte total weight.
5, preparation method according to claim 1, the method that it is characterized in that described etching nano particle or monodimension nanometer material is formic acid, alkali or Microwave Treatment, perhaps soaked in solvent.
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| US8048814B2 (en) * | 2009-05-19 | 2011-11-01 | Innovalight, Inc. | Methods and apparatus for aligning a set of patterns on a silicon substrate |
| CN102260046B (en) * | 2010-05-28 | 2013-04-17 | 中国科学院大连化学物理研究所 | Microwave synthesis method of zinc oxide film with oriented nanorod structure |
| CN102683032B (en) * | 2011-06-27 | 2014-05-14 | 河南理工大学 | Preparation of foliated titanium dioxide nano array thin film electrode and application of foliated titanium dioxide nano array thin film electrode in dye sensitized solar cell |
| CN104538191B (en) * | 2014-12-16 | 2017-11-07 | 中南大学 | The preparation method and dye-sensitized solar cell anode and DSSC of dye-sensitized solar cell anode |
| CN105552235B (en) * | 2015-12-24 | 2017-11-03 | 上海博暄能源科技有限公司 | A kind of method for improving perovskite solar battery efficiency |
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