CN103700508A - Perovskite oxide counter electrode material for DSSCs (dye sensitized solar cells) - Google Patents
Perovskite oxide counter electrode material for DSSCs (dye sensitized solar cells) Download PDFInfo
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- CN103700508A CN103700508A CN201310627427.XA CN201310627427A CN103700508A CN 103700508 A CN103700508 A CN 103700508A CN 201310627427 A CN201310627427 A CN 201310627427A CN 103700508 A CN103700508 A CN 103700508A
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Abstract
The invention discloses a perovskite oxide thin film electrode, a preparation method thereof and application of the perovskite oxide thin film electrode in the field of DSSCs (dye sensitized solar cells), and belongs to the field of DSSCs. The preparation method comprises the following steps: synthesizing perovskite oxide powder by using a sol-gel method, mixing the powder, a solvent, an additive and the like to obtain slurry, depositing the slurry on a conductive thin film substrate by using the silk screen printing method, and performing sintering to prepare a porous perovskite oxide counter electrode for DSSCs. The perovskite oxide thin film electrode, the preparation method and the application have the benefits that the perovskite oxide counter electrode is higher in catalytic performance, stable in chemical performance, and low in cost, the sources are extensive, the cost is greatly lowered and the large-scale industrialization of the DSSCs is facilitated.
Description
Technical field
The invention belongs to dye-sensitized solar cells technical field, be specifically related to dye-sensitized solar cells and use perofskite type oxide film to electrode.
Background technology
Dye-sensitized solar cells (dye sensitized solar cells, DSSCs) because it is with low cost, make simple, stable performance, environmental friendliness, demonstrate powerful commercial application value.From Gr professor tzel in 1991, develop first conversion efficiency and reach 7.9% dye-sensitized solar cells, the liquid electrolytic cell photoelectric conversion efficiency in laboratory has surpassed 12%(Science, 2011,334,6056 at present).And this novel solar battery based on nano-crystalline semiconductor material has the potential advantages of further raising the efficiency and reducing costs, very likely replace conventional solid-state photovoltaic device as silicon solar cell, cadmium antimonide hull cell and copper indium gallium selenide film battery, and become the leading of following solar cell.
DSSCs is mainly by the nanocrystalline TiO of porous semi-conductor of dye sensitization
2thin film work electrode, contain I
-/ I
3 -the electrolyte of oxidation-reduction pair and catalysis I
3 -electrode is formed.To electrode Main Function: collect and transport electronics (electronics that receives battery external loop also passes to the redox reaction duplet in electrolyte it); Absorption catalysis I
3 -; Reflection sees through light; The photoelectric properties and the photoelectric conversion efficiency that electrode pair are improved to DSSCs play an important role.Therefore, to electrode, need there is low resistance and high catalytic activity, to reduce the energy loss to electron transfer process on electrode.Typically to electrode, platinum (platinum, the Pt) Catalytic Layer by transparent conducting glass (FTO glass) and FTO conductive glass surface forms.But, noble metal platinum is not only disagreed with the original intention cheaply of dye-sensitized solar cells, large-scale production and application have obvious limitation, and the Pt Catalytic Layer existence that some technique makes is easily by the phenomenon of electrolyte corrosion, causes device stability to decline.Therefore, exploring the non-platinum of novel cheapness is one, DSSCs field study hotspot in recent years to electrode.
In recent years, perovskite composite oxide (ABO
3) there is higher electricity and lead, doping vario-property is carried out in B position is more of value to raising electrode performance.Wherein, the LaNi of better performances
0.8fe
0.2o
3in secondary metals hydride-air cell, realized Preliminary Applications.Meanwhile, lanthanum manganate base film has the performances such as electric heating, catalyst is temperature sensitive, causes researcher's extensive concern.Perofskite type oxide method for manufacturing thin film is numerous, and silk-screen printing technique is simple, is easy to scale.Perovskite composite oxide film prepared by silk screen print method has aboundresources to electrode, cheap, and environmental friendliness and applicable large-scale production characteristic are to replace the ideal material of platinum to electrode.
Summary of the invention
Limited to electrode reserves for traditional platinum, expensive, be not easy to the defects such as industrialization production, the object of the present invention is to provide that a kind of cost is low, catalytic activity is high and be suitable for perofskite type oxide that industrialization produces to electrode.
Above-mentioned purpose realizes by following scheme:
The perofskite type oxide that dye-sensitized solar cells is used is to an electrode,
It is characterized in that: preparation method comprises the following steps:
(1) slaine is joined in deionized water solvent, stir, again by EDTA n(EDTA proportionally): n(metal ion)=(0.1-100): 1 joins in the aqueous solution of slaine, add again adhesion agent ethylene glycol, ethylene glycol is n(ethylene glycol proportionally): n(EDTA)=(0.1-100): 1 adds, constantly stir, by dripping ammoniacal liquor or nitre acid for adjusting pH value stabilization at 4-12, water-bath evaporation water is got gel again, gel vacuumize at 60-200 ℃ is obtained to xerogel, then 100-500 ℃ of generation spontaneous combustion in air, after being ground, combustion product in air, carries out further heat treatment, heat-treatment temperature range is 60-1100 ℃, be prepared into perofskite type oxide powder,
(2) perofskite type oxide powder is mixed with solvent, additive and obtain screen printing sizing agent, the screen printing sizing agent configuring is ground to 0.5-12h, then adopt silk screen print method to be deposited in conductive film substrate, film drying after printing and 300-520 ℃ of sintering 0.5-12h, finally become dye-sensitized solar cells and use porous Ca-Ti ore type sull to electrode.
The perofskite type oxide that described a kind of dye-sensitized solar cells is used is to electrode, it is characterized in that: the mol ratio that described slaine is metal ion is La:Ni:Fe=1:(0.1-1): the nitrate of lanthanum (0.9-0), nickel and ferrous metal, prepared perofskite type oxide powder is LaNi
1-xfe
xo
3(x=0-0.9), or the mol ratio that described slaine is metal ion is La:Sr:Mn=(0.1-1): the nitrate of lanthanum (0.9-0), strontium and manganese metal, prepared perofskite type oxide powder is La
1-xsr
xmnO
3(x=0-0.9).
The perofskite type oxide that described a kind of dye-sensitized solar cells is used, to electrode, is characterized in that: described conductive film substrate is electro-conductive glass or other conductive substrates materials.
The perofskite type oxide that described a kind of dye-sensitized solar cells is used, to electrode, is characterized in that: described solvent is terpinol, and described additive is ethyl cellulose.
The perofskite type oxide that described a kind of dye-sensitized solar cells is used, to electrode, is characterized in that: each raw material weight proportioning of described screen printing sizing agent is: W
perovskite powder: W
terpinol: W
ethyl cellulose=1:(0.1-10): (0.3-30).
Described Ca-Ti ore type LaNi
1-xfe
xo
3to electrode, preparation comprises the steps: film
(1) according to La:Ni:Fe=1:(0.1-1): mol ratio (0.9-0) takes lanthanum nitrate, nickel nitrate and ferric nitrate, take deionized water as solvent, after fully stirring, according to n(EDTA): n(metal ion)=(0.1-100): 1 adds the ammonia spirit of EDTA, add again adhesion agent ethylene glycol, ethylene glycol is n(ethylene glycol proportionally): n(EDTA)=(0.1-100): 1 adds, constantly stir, regulate pH value stabilization at 4-12, water-bath 40-70 ℃ of heating slow evaporation moisture, finally obtain thick clear gel, by gel vacuumize 5-24h at 60-100 ℃, obtain xerogel, 300-500 ℃ of generation spontaneous combustion in air again, after being ground, combustion product in air, carries out further heat treatment, heat-treatment temperature range is 60-900 ℃, heating rate is 10 ℃ of min
-1.Obtain required Ca-Ti ore type LaNi
1-xfe
xo
3powder.
(2) by certain mass ratio, add terpinol and ethyl cellulose, itself and LaNi
1-xfe
xo
3the mass ratio of powder is W
laNi1-xFexO3: W
terpinol: W
ethyl cellulose=1:1:3; The slurry configuring grinds the slurry that forms the applicable silk screen printing of thickness for 30 minutes.Adopt silk screen print method by the slurry silk-screen configuring in conductive film substrate, at 300-520 ℃ of sintering 0.5-12h, naturally cooling with stove, formation porous LaNi
1-xfe
xo
3film is to electrode.
Described Ca-Ti ore type La
1-xsr
xmnO
3to electrode, preparation comprises the steps: film
(1) according to La:Sr:Mn=1:(0.1-1): mol ratio (0.9-0) takes lanthanum nitrate, strontium nitrate and manganese nitrate, take deionized water as solvent, after fully stirring, according to n(EDTA): n(metal ion)=(0.1-100): 1 adds the ammonia spirit of EDTA, add again adhesion agent ethylene glycol, ethylene glycol is n(ethylene glycol proportionally): n(EDTA)=(0.1-100): 1 adds, constantly stir, regulate pH value stabilization at 4-12, water-bath 40-70 ℃ of heating slow evaporation moisture, finally obtain thick clear gel, by gel vacuumize 5-24h at 60-100 ℃, obtain xerogel, 300-500 ℃ of generation spontaneous combustion in air again, after being ground, combustion product in air, carries out further heat treatment, heat-treatment temperature range is 60-900 ℃, heating rate is 10 ℃ of min
-1.Obtain required Ca-Ti ore type La
1-xsr
xmnO
3powder.
(2) by certain mass ratio, add terpinol and ethyl cellulose, itself and La
1-xsr
xmnO
3the mass ratio of powder is W
la1-xSrxMnO3: W
terpinol: W
ethyl cellulose=1:1:3; The slurry configuring grinds the slurry that forms the applicable silk screen printing of thickness for 30 minutes.Adopt silk screen print method by the slurry silk-screen configuring in conductive film substrate, at 300-520 ℃ of sintering 0.5-12h, naturally cooling with stove, formation porous La
1-xsr
xmnO
3film is to electrode.
The perofskite type oxide of preparing according to the present invention is to electrode, and electricity conversion is different, wherein iron doping nickel acid lanthanum (LaNi
0.8fe
0.2o
3) film to electrode DSC photoelectric conversion efficiency higher than strontium lanthanum manganese oxide (La
0.6sr
0.4mnO
3and La
0.8sr
0.2mnO
3) film is to electrode.Meanwhile, perovskite composite oxide film has aboundresources, cheap, and environmental friendliness and applicable large-scale production characteristic are to replace the ideal material of noble metal platinum to electrode.
Accompanying drawing explanation
Accompanying drawing 1 LaNi
1-xfe
xo
3the XRD collection of illustrative plates of (x=0.2,0.4).
Accompanying drawing 2 Ca-Ti ore type LaNi
0.8fe
0.2o
3to electrode stereoscan photograph.Fig. 2 shows, is deposited on the LaNi of conductive film substrate surface
0.8fe
0.2o
3there is agglomeration in particle, presentation layer sheet.
Accompanying drawing 3 Ca-Ti ore type LaNi
0.8fe
0.2o
3, La
0.6sr
0.4mnO
3with pyrolysis platinum to the DSSCs current-voltage curve figure of electrode assembling (
j-
vcurve chart).
Embodiment
Below in conjunction with specific embodiment and coordinate accompanying drawing to be described in further detail the present invention, so that those skilled in the art understand the present invention better, but the present invention is not limited to following examples.
Embodiment 1: Ca-Ti ore type LaNi
0.8fe
0.2o
3preparation to electrode:
(1) weigh 0.005mol lanthanum nitrate (La(NiO
3)
3) 6H
2o), 0.004mol nickel nitrate (Ni(NiO
3)
2) 6H
2o), 0.001mol ferric nitrate (Fe(NiO
3)
3) 9H
2o), successively respectively each cationic nitrate is dissolved in deionized water, EDTA fully mixes with 0.011mol complexing agent, and to add the ethylene glycol of 0.033mol be adhesion agent.In the situation that constantly stirring, regulate pH value stabilization approximately 7, until obtain homogeneous transparent solution, and be placed on slow evaporation moisture at 40-70 ℃, until obtain transparent gel.By gel vacuumize 12h at 100 ℃, obtain cellular xerogel, in air, approximately 300 ℃ there is spontaneous combustion, after combustion product is ground, carry out further heat treatment in air, and heat-treatment temperature range is 60-900 ℃, and heating rate is 10 ℃ of min
-1.Obtain required Ca-Ti ore type LaNi
0.8fe
0.2o
3powder.
(2) by certain mass ratio, add terpinol and ethyl cellulose, itself and LaNi
0.8fe
0.2o
3the mass ratio of powder is W
laNi0.8Fe0.2O3: W
terpinol: W
ethyl cellulose=1:1:3; The slurry configuring grinds the slurry that forms the applicable blade coating of thickness for 30 minutes.450 ℃ of sintering 30 minutes, naturally cooling with stove, form porous membrane.
Refer to Fig. 1, Figure 1 shows that Ca-Ti ore type LaNi prepared by the present invention
0.8fe
0.2o
3xRD collection of illustrative plates.All diffraction maximums and the comparison of standard spectrogram, confirm that gained crystal is Ca-Ti ore type pure phase LaNi
0.8fe
0.2o
3.
According to conventional methods by prepared Ca-Ti ore type LaNi
0.8fe
0.2o
3electrode assembling is become to DSSCs, and cell area is 0.25cm
2.The DSSCs assembling is recorded under AM1.5 simulated solar irradiation to the current-voltage curve (shown in Fig. 3 curve 1) of dye-sensitized solar cells.Adopt Ca-Ti ore type LaNi
0.8fe
0.2o
3dSSC to electrode assembling, its open circuit voltage (
v oc) be 556mV, short circuit current (
j sc) be 7.35mAcm
-2, fill factor, curve factor (FF) is 0.30, electricity conversion (
η) be 1.24%.
Embodiment 2: Ca-Ti ore type LaNi
0.6fe
0.4o
3preparation to electrode:
(1) weigh 0.005mol lanthanum nitrate (La(NiO
3)
3) 6H
2o), 0.003mol nickel nitrate (Ni(NiO
3)
2) 6H
2o), 0.002mol ferric nitrate (Fe(NiO
3)
3) 9H
2o), successively respectively each cationic nitrate is dissolved in deionized water, EDTA fully mixes with 0.011mol complexing agent, and to add the ethylene glycol of 0.033mol be adhesion agent.In the situation that constantly stirring, regulate pH value stabilization approximately 7, until obtain homogeneous transparent solution, and be placed on slow evaporation moisture at 40-70 ℃, until obtain transparent gel.By gel vacuumize 12h at 100 ℃, obtain cellular xerogel, in air, approximately 300 ℃ there is spontaneous combustion, after combustion product is ground, carry out further heat treatment in air, and heat-treatment temperature range is 60-900 ℃, and heating rate is 10 ℃ of min
-1.Obtain required Ca-Ti ore type LaNi
0.6fe
0.4o
3powder.
(2) by certain mass ratio, add terpinol and ethyl cellulose, itself and LaNi
0.6fe
0.4o
3the mass ratio of powder is W
laNi0.6Fe0.4O3: W
terpinol: W
ethyl cellulose=1:1:3; The slurry configuring grinds the slurry that forms the applicable blade coating of thickness for 30 minutes.450 ℃ of sintering 30 minutes, naturally cooling with stove, form porous membrane.
Refer to Fig. 1, Figure 1 shows that Ca-Ti ore type LaNi prepared by the present invention
0.6fe
0.4o
3xRD collection of illustrative plates.All diffraction maximums and the comparison of standard spectrogram, confirm that gained crystal is Ca-Ti ore type LaNi
0.6fe
0.4o
3, wherein contain a small amount of La
2o
3impurity phase.
According to conventional methods by prepared Ca-Ti ore type LaNi
0.6fe
0.4o
3electrode assembling is become to DSSCs, and cell area is 0.25cm
2.The DSSCs assembling is recorded under AM1.5 simulated solar irradiation its open circuit voltage (
v oc) be 509mV, short circuit current (
j sc) be 5.87mAcm
-2, fill factor, curve factor (FF) is 0.30, electricity conversion (
η) be 0.89%.
Embodiment 3: Ca-Ti ore type La
0.6sr
0.4mnO
3the preparation of electrode
(1) weigh 0.009mol lanthanum nitrate (La(NiO
3)
36H
2o), 0.006mol strontium nitrate (Sr(NiO
3)
2), 0.015mol manganese nitrate (Mn(NiO
3)
2, 50%), successively respectively each cationic nitrate is dissolved in deionized water, EDTA fully mixes with 0.033mol complexing agent, and to add the ethylene glycol of 0.099mol be adhesion agent.Regulate pH value stabilization after approximately 7, and be placed on slow evaporation moisture at 40-70 ℃, until obtain the transparent gel of peony viscous.By gel vacuumize 12h at 100 ℃, obtain the cellular xerogel of brown, in air, approximately 300 ℃ there is spontaneous combustion, after combustion product is ground, carry out further heat treatment in air, and heat-treatment temperature range is 60-900 ℃, and heating rate is 10 ℃ of min
-1, obtain required Ca-Ti ore type La
0.6sr
0.4mnO
3powder.
(2) by certain mass ratio, add terpinol and ethyl cellulose, itself and La
0.6sr
0.4mnO
3the mass ratio of powder is W La
0.6sr
0.4mnO
3: W
terpinol: W
ethyl cellulose=1:1:3; The slurry configuring grinds the slurry that forms the applicable blade coating of thickness for 30 minutes.450 ℃ of sintering 30 minutes, naturally cooling with stove, form porous membrane.
According to conventional methods by prepared Ca-Ti ore type La
0.6sr
0.4mnO
3electrode assembling is become to DSSCs, and cell area is 0.25cm
2.The DSSCs assembling is recorded under AM1.5 simulated solar irradiation to the current-voltage curve (shown in Fig. 3 curve 2) of dye-sensitized solar cells.Adopt Ca-Ti ore type La
0.6sr
0.4mnO
3dSSC to electrode assembling, its open circuit voltage (
v oc) be 625mV, short circuit current (
j sc) be 2.73mAcm
-2, fill factor, curve factor (FF) is 0.14, electricity conversion (
η) be 0.24%.
Embodiment 4: Ca-Ti ore type La
0.8sr
0.2mnO
3the preparation of electrode
(1) weigh 0.012mol lanthanum nitrate (La(NiO
3)
36H
2o), 0.003mol strontium nitrate (Sr(NiO
3)
2), 0.015mol manganese nitrate (Mn(NiO
3)
2, 50%), successively respectively each cationic nitrate is dissolved in deionized water, EDTA fully mixes with 0.033mol complexing agent, and to add the ethylene glycol of 0.099mol be adhesion agent.Regulate pH value stabilization after approximately 7, and be placed on slow evaporation moisture at 40-70 ℃, until obtain the transparent gel of peony viscous.By gel vacuumize 12h at 100 ℃, obtain the cellular xerogel of brown, in air, approximately 300 ℃ there is spontaneous combustion, after combustion product is ground, carry out further heat treatment in air, and heat-treatment temperature range is 60-900 ℃, and heating rate is 10 ℃ of min
-1, obtain required Ca-Ti ore type La
0.8sr
0.2mnO
3powder.
(2) by certain mass ratio, add terpinol and ethyl cellulose, itself and La
0.8sr
0.2mnO
3the mass ratio of powder is W
la0.8Sr0.2MnO3: W
terpinol: W
ethyl cellulose=1:1:3; The slurry configuring grinds the slurry that forms the applicable blade coating of thickness for 30 minutes.450 ℃ of sintering 30 minutes, naturally cooling with stove, form porous membrane.
According to conventional methods by prepared Ca-Ti ore type La
0.8sr
-0.2mnO
3electrode assembling is become to DSSCs, and cell area is 0.25cm
2.The DSSCs assembling is recorded under AM1.5 simulated solar irradiation its open circuit voltage (
v oc) be 510mV, short circuit current (
j sc) be 5.37mAcm
-2, fill factor, curve factor (FF) is 0.13, electricity conversion (
η) be 0.37%.
Comparative example 1: as a comparison, we also adopt pyrolysismethod to prepare platinum to electrode.5mM platinum acid chloride solution is dripped and is coated in 1.5 * 1.5cm
2fTO conductive glass surface, and in Muffle furnace sintering 30 minutes at 400 ℃, naturally cooling with stove, make required platinum to electrode.The platinum of preparation, to electrode, is assembled into DSSCs under same case, and cell area is 0.25cm
2.The DSSCs assembling is recorded under AM1.5 simulated solar irradiation to the current-voltage curve (shown in Fig. 3 curve 3) of dye-sensitized solar cells.Adopt the DSSCs of pyrolysis platinum to electrode assembling, its open circuit voltage (
v oc) be 683mV, short circuit current (
j sc) be 8.13mAcm
-2, fill factor, curve factor (FF) is 0.63, electricity conversion (
η) be 3.48%.
Claims (5)
1. the perofskite type oxide that dye-sensitized solar cells is used is to an electrode,
It is characterized in that: preparation method comprises the following steps:
(1) slaine is joined in deionized water solvent, stir, again by EDTA n(EDTA proportionally): n(metal ion)=(0.1-100): 1 joins in the aqueous solution of slaine, add again adhesion agent ethylene glycol, ethylene glycol is n(ethylene glycol proportionally): n(EDTA)=(0.1-100): 1 adds, constantly stir, by dripping ammoniacal liquor or nitre acid for adjusting pH value stabilization at 4-12, water-bath evaporation water is got gel again, gel vacuumize at 60-200 ℃ is obtained to xerogel, then 100-500 ℃ of generation spontaneous combustion in air, after being ground, combustion product in air, carries out further heat treatment, heat-treatment temperature range is 60-1100 ℃, be prepared into perofskite type oxide powder,
(2) perofskite type oxide powder is mixed with solvent, additive and obtain screen printing sizing agent, the screen printing sizing agent configuring is ground to 0.5-12h, then adopt silk screen print method to be deposited in conductive film substrate, film drying after printing and 300-520 ℃ of sintering 0.5-12h, finally become dye-sensitized solar cells and use porous Ca-Ti ore type sull to electrode.
2. the perofskite type oxide that a kind of dye-sensitized solar cells according to claim 1 is used is to electrode, it is characterized in that: the mol ratio that described slaine is metal ion is La:Ni:Fe=1:(0.1-1): the nitrate of lanthanum (0.9-0), nickel and ferrous metal, prepared perofskite type oxide powder is LaNi
1-xfe
xo
3(x=0-0.9), or the mol ratio that described slaine is metal ion is La:Sr:Mn=(0.1-1): the nitrate of lanthanum (0.9-0), strontium and manganese metal, prepared perofskite type oxide powder is La
1-xsr
xmnO
3(x=0-0.9).
3. the perofskite type oxide that a kind of dye-sensitized solar cells according to claim 1 is used, to electrode, is characterized in that: described conductive film substrate is electro-conductive glass or other conductive substrates materials.
4. the perofskite type oxide that a kind of dye-sensitized solar cells according to claim 1 is used, to electrode, is characterized in that: described solvent is terpinol, and described additive is ethyl cellulose.
5. the perofskite type oxide that a kind of dye-sensitized solar cells according to claim 4 is used, to electrode, is characterized in that: each raw material weight proportioning of described screen printing sizing agent is: W
perovskite powder: W
terpinol: W
ethyl cellulose=1:(0.1-10): (0.3-30).
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Cited By (6)
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|---|---|---|---|---|
| CN104091692A (en) * | 2014-05-30 | 2014-10-08 | 上海北京大学微电子研究院 | Solar cell with high conversion efficiency and preparation method thereof |
| CN106024396A (en) * | 2016-07-13 | 2016-10-12 | 中国科学院武汉物理与数学研究所 | Counter electrode for dye-sensitized solar cell and preparation method thereof |
| CN112058272A (en) * | 2020-08-20 | 2020-12-11 | 天津大学 | Perovskite type catalyst prepared by sol-gel weak oxidation calcination method and method |
| CN114100604A (en) * | 2020-08-27 | 2022-03-01 | 清华大学 | LaMnO3Catalyst, preparation method and application thereof |
| CN114813880A (en) * | 2022-04-28 | 2022-07-29 | 安徽大学 | Integrated electrochemical gas sensor and preparation process thereof |
| CN115084318A (en) * | 2022-07-18 | 2022-09-20 | 西南科技大学 | Inorganic perovskite type LaNiO 3 Preparation and application of visible photoconductive film |
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| 刘珩等: "中温固体氧化物燃料电池LaNi0.6Fe0.4O3-δ阴极材料的制备及性能表征", 《电化学》, 30 November 2011 (2011-11-30) * |
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| CN115084318B (en) * | 2022-07-18 | 2023-06-09 | 西南科技大学 | Inorganic perovskite type LaNiO 3 Preparation and application of visible photoconductive film |
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