CN105304338B - It is a kind of for quantum dot sensitized solar battery to electrode and preparation method thereof - Google Patents
It is a kind of for quantum dot sensitized solar battery to electrode and preparation method thereof Download PDFInfo
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Abstract
It is a kind of for quantum dot sensitized solar battery to electrode and preparation method thereof, count protocol main points of the invention are: the structure to electrode is to grow one layer of Catalytic Layer being made of PbS and CuS in FTO electro-conductive glass substrate surface, which is prepared using cryochemistry bath sedimentation.Problem to be solved by this invention be it is at high cost to electrode existing Pt, catalytic performance is low and metal sulfide is poor to electrode stability, aiming at the problem that be not easy to encapsulate, provide it is a kind of it is low in cost, catalytic activity is higher, preparation process is simple.
Description
Technical field:
The invention belongs to field of solar energy utilization, also belong to field of nanometer material technology, and in particular to one kind is quick for quantum dot
Change the Pb of solar batteryxCu1-xS is to electrode and preparation method thereof
Background technique:
The bring Heavy environmental pollution in the increasingly exhausted and its use process of fossil energy, it is inexhaustible with it not
The solar energy exhausted is at important countermeasure to solve this problem.In all kinds of novel solar batteries, preparation process is simple, cost
Cheap quantum dot sensitized solar battery (QDSSC) causes the extensive concern of researcher.Compared with dye sensitizing agent, amount
Son point has adjustable band structure, and higher extinction coefficient, biggish natural dipole moment and exciton multiplier effect etc. are unique
Advantage (A. Kongkanand, et al., J. Am. Chem. Soc., 2008,130,4007).Therefore, it studies
QDSSC has very important significance to developing low-cost, efficient solar battery.
QDSSC is mainly formed by the light anode of absorption quantum dot, electrolyte and to electrode three parts, wherein to the work of electrode
With being that the electron transmission of external circuit is made its reducing/regenerating to electrolyte.In addition, oxidation in electrolyte can also be accelerated to go back electrode
Original plays catalytic action to the electron exchange rate between cathode.I-/I3 -It is common electricity in dye-sensitized solar cells
Liquid is solved, precious metals pt is to I-/I3 -With high catalytic activity and chemical stability, the charge at electrode/electrolyte interface is turned
Move impedance (Rct) very low, thus Pt is most common to electrode in dye-sensitized cell.But most of quanta point material is in I-/
I3 -Can be unstable due to chemical attack in electrolyte, thus more sulphur electrolyte (S are commonly used in the research of QDSSC2-/Sn 2-) generation
For I-/I3 -Hole-conductive layer as battery.But in S2-/Sn 2-In system, the catalytic activity of the noble metal electrodes such as Pt is very low,
Cause the Charge-transfer resistance to electrode/electrolyte interface very big, this is the fill factor and photoelectric conversion efficiency for leading to QDSSC
A relatively low major reason.In addition, the S in more sulphur electrolyte2-It is easily absorbing the surface Pt, generation poisons effect, influences
To the stability of electrode (J. G. Radich, et al., J. Phys. Chem. Lett., 2011,2,2453), institute
With Pt is not suitable for the optimal to electrode material of QDSSC.In order to reduce the electric charge transfer resistance to electrode/electrolyte interface
It is anti-, multiple material be attempted as to application of electrode in QDSSC, such as Cu2S(Pan. Z, et al., ACS Nano,
2013,7 (6): 5215), PbS(Tachan. Z, et al., J. Phys. Chem. C, 2011,115 (13):
6162), CoS(Yuan. H, et al., J. Electrochem. Soc., 2013,160 (9): H624) etc., these types
Metal sulfide has higher catalytic activity to electrode material compared with Pt, and cost is relatively low, but these types is to electricity at present
The preparation method of pole usually first uses HCl or H2SO4 corrodes metal (Cu, Pb etc.) paillon, and then more sulphur electrolysis drop exists
Foil surfaces, to form one layer of metal sulfide (Tachan. Z, et al., J. Phys. in metal foil surface
Chem. C, 2011, 115(13): 6162, G. Hodes, et al., J. Electrochem. Soc., 127(3):
544), although this preparation method comparison is easy, since electrolyte can constantly corrode metal foil after being packaged into battery
Piece, it is very poor to the stability of electrode；And since these types of metal sulfide is all to corrode on metal foil to electrode,
Adhesiveness is very poor between metal sulfide and foil substrate, along with metal foil surface is relatively rough, exists and is difficult to encapsulate
Problem, therefore be difficult to meet practical needs.
Summary of the invention:
Problem to be solved by this invention is for existing Pt is at high cost to electrode, catalytic performance is low and metal sulfide
It is poor to electrode stability, be not easy the problem of encapsulating, provide it is a kind of it is low in cost, catalytic activity is higher, preparation process is simple, can be big
The Pb for QDSSC of area preparationxCu1-xS is to electrode and preparation method thereof.It is this that low temperature solution polycondensation is passed through in FTO to electrode
Electro-conductive glass substrate surface deposits, and formation is combined closely between electrode material and substrate, and PbxCu1-xS thickness
Controllably, it is easy to encapsulate, the photoelectric conversion efficiency of QDSSC can be significantly improved.
To achieve the above object, the technical solution adopted by the present invention is that:
It is a kind of for quantum dot sensitized solar battery to electrode and preparation method thereof, it is characterised in that: to electrode
Structure is to grow one layer of Catalytic Layer being made of PbS and CuS in FTO electro-conductive glass substrate surface, which uses low temperature
Bath sedimentation is learned to be prepared.
Method includes the following steps:
1) substrate is cleaned
FTO electro-conductive glass substrate is sequentially placed into ethyl alcohol, acetone and deionized water added with detergent and is respectively cleaned by ultrasonic
It to remove the dust and grease of substrate surface, places into deionized water and is cleaned by ultrasonic 15 minutes, wash away containing dirt within 15 minutes
Then detergent and some inorganic pollutions are rinsed with deionized water ultrasound for 15 minutes again, finally spare with being dried with nitrogen.
2) preparation of chemical bath deposition solution
By 4.74 g(12.5 mmol) lead acetate, 2 g(50 mmol) sodium hydroxide, 1.52 g(20 mmol) thiocarbamide and
1.49 g(10 mmol) triethanolamine is dissolved in 400 ml deionized waters, it is mixing uniformly to form solution A.By 0.64 g(3.75
Mmol) copper chloride and 1.19 g(8 mmol) triethanolamine is dissolved in 100 ml deionized waters, it is mixing uniformly to form solution B.
Then solution A is slowly added in solution B under agitation, continues stirring and forms chemical bath deposition solution after ten minutes.
3) Pb is deposited in FTO glass basic surfacexCu1-xS is to electrode
The FTO electro-conductive glass substrate cleaned up is fixed on fixture, then substrate is dipped vertically into deposition solution,
With aluminium foil after the beaker sealing for filling solution, it is placed on magnetic stirring apparatus and carries out deposition reaction at room temperature, when depositing one section
Between after in FTO glass basic surface form one layer of khaki or pewter PbxCu1-xS film, the longer color of sedimentation time is more
It is deep.Electrode is taken out after reaction, is rinsed well with deionized water, and is dried for standby with baking oven.
Further, Pb in deposition solution described in step (2)2+Source can be lead acetate or plumbi nitras, Cu2+Source can be
Copper chloride or copper acetate, wherein Pb2+, Cu2+And S2-Molar ratio be 10:3:16.
Further, deposition solution described in step (2) is in strong basicity, and pH value is 13 or so.
Further, sedimentation time described in step (3) is 2 ~ 15 hours, the Pb of formationxCu1-xS Catalytic Layer with a thickness of
150~700 nm。
Compared with prior art, the present invention provides a kind of for replacing tradition Pt to the efficient Pb of electrodexCu1-xS is to electricity
Pole material and conveniently preparation method, present invention has an advantage that
1) compared with Pt is to electrode, PbxCu1-xS has higher catalytic activity to more sulphur electrolyte to electrode, can promote
Into the electron-transport to electrode/electrolyte interface, to significantly improve the photoelectric conversion efficiency of battery, while can be greatly reduced
The production cost of battery.
2) compared with the PbS or CuS prepared on metal foil is to electrode, Pb prepared by the present inventionxCu1-xS is to electrode and base
Bottom adhesiveness is good, enhances the stability to electrode, and be convenient for the encapsulation of battery.
3) PbxCu1-xElectrode is prepared in S by solwution method at room temperature, simple process, low in cost, and this method is suitable
For large scale preparation based on flexible conducting substrate to electrode.
Detailed description of the invention:
Technical solution in order to enable those skilled in the art to better understand the present invention, below in conjunction with attached drawing and specific implementation
The invention will be described in further detail for example.These embodiments are merely to illustrate the purpose of the present invention, do not limit in any way
The scope of the present invention processed.
Fig. 1 (a) ~ (d) is respectively that method of the present invention was prepared with FTO substrate, deposition 2 hours, 7 hours and 15 hours
PbxCu1-xS electrode SEM figure,
Fig. 2 is Pb of the method for the present invention in deposition preparation in 7 hoursxCu1-xS electrode section SEM figure,
Fig. 3 is method of the present invention with the Pb of FTO substrate and deposition preparation in 7 hoursxCu1-xS electrode XRD diagram,
Fig. 4 is the Pb that method of the present invention is prepared with different sedimentation timesxCu1-xQDSSC electricity of the S to electrode assembling
Stream-voltage curve,
Fig. 5 is for method of the present invention with Pt to the QDSSC current -voltage curve figure of electrode assembling.
Embodiment 1
(1) Pb is preparedxCu1-xS is to electrode
1) substrate is cleaned
FTO electro-conductive glass substrate is sequentially placed into ethyl alcohol, acetone and deionized water added with detergent and is respectively cleaned by ultrasonic
It to remove the dust and grease of substrate surface, places into deionized water and is cleaned by ultrasonic 15 minutes, wash away containing dirt within 15 minutes
Then detergent and some inorganic pollutions are rinsed for 15 minutes with deionized water ultrasound, finally spare with being dried with nitrogen.
2) preparation of chemical bath deposition solution
By 4.74 g(12.5 mmol) lead acetate, 2 g(50 mmol) sodium hydroxide, 1.52 g(20 mmol) thiocarbamide and
1.49 g(10 mmol) triethanolamine is dissolved in 400 ml deionized waters, it is mixing uniformly to form solution A.By 0.64 g(3.75
Mmol) copper chloride and 1.19 g(8 mmol) triethanolamine is dissolved in 100 ml deionized waters, it is mixing uniformly to form solution B.
Then solution A is slowly added in solution B under agitation, continues stirring and forms chemical bath deposition solution after ten minutes,
Pb2+, Cu2+And S2-Molar ratio be 10:3:16.
3) Pb is deposited in electro-conductive glass substrate surfacexCu1-xS is to electrode
The FTO electro-conductive glass substrate cleaned up is fixed on fixture, then substrate is dipped vertically into deposition solution,
With aluminium foil after the beaker sealing for filling solution, it is placed on magnetic stirring apparatus and carries out deposition reaction at room temperature, deposition is after 2 hours
FTO substrate is taken out, is rinsed well with deionized water, and be dried for standby with baking oven, uses its thickness of scanning electron microscope test
For 173 nm, this electrode is named as PbxCu1-xS-2。
(2) the porous TiO of preparation CdSe quantum dot sensitization2Light anode (TiO2/ CdSe)
By silk screen print method by Dyesol-18NRT TiO2Slurry is coated on FTO electro-conductive glass, then at 500 DEG C
Muffle furnace in anneal 30 minutes, be cooled to room temperature to be formed with a thickness of 10 μm, area is 5 × 5 mm2Porous TiO2Electrode.With
Afterwards using electrochemical deposition method (X. Song, et al., Electrochimica Acta, 2013,108,449) more
Hole TiO2Surface deposits CdSe quantum dot, forms TiO2/ CdSe electrode.
(3) it assembling quantum dot sensitization solar battery and tests
The TiO that will be prepared2/ CdSe light anode is placed on table top, and by the heat-sealing film cut " back-shaped " frame (60 μ
M) above-mentioned electrode surrounding is overlayed, then electrode is made with heat sealing machine heating to electrode and light anode in heat-sealing film surface cover
It is packaged together, then by pouring into more sulphur electrolyte (1 mol/L Na to the aperture accomplished fluently in advance on electrode2S and 1 mol/L S
The aqueous solution of powder), the preparation of quantum dot sensitized solar battery then can be completed with heat-sealing film sealed aperture.Assembled electricity
Pond is in 100 mW/cm2 Current -voltage curve is tested under the simulated solar irradiation of (AM 1.5).
Embodiment 2
(1) Pb is preparedxCu1-xS is to electrode
1) substrate is cleaned
With embodiment 1.
2) preparation of chemical bath deposition solution
With embodiment 1.
3) Pb is deposited in electro-conductive glass substrate surfacexCu1-xS is to electrode
The FTO electro-conductive glass substrate cleaned up is fixed on special fixture, substrate is then dipped vertically into deposition
In solution, with aluminium foil after the beaker sealing for filling solution, it is placed on magnetic stirring apparatus and carries out deposition reaction at room temperature, deposit
FTO substrate is taken out after 4 hours, is rinsed well, and be dried for standby with baking oven with deionized water, is used scanning electron microscope test
It is named as Pb with a thickness of 324 nm, this electrodexCu1-xS-4。
(2) the porous TiO of preparation CdSe quantum dot sensitization2Light anode (TiO2/CdSe)
With embodiment 1.
(3) it assembling quantum dot sensitization solar battery and tests
With embodiment 1.
Embodiment 3
(1) Pb is preparedxCu1-xS is to electrode
1) substrate is cleaned
With embodiment 1.
2) preparation of chemical bath deposition solution
With embodiment 1.
3) Pb is deposited in electro-conductive glass substrate surfacexCu1-xS is to electrode
The FTO electro-conductive glass substrate cleaned up is fixed on special fixture, substrate is then dipped vertically into deposition
In solution, with aluminium foil after the beaker sealing for filling solution, it is placed on magnetic stirring apparatus and carries out deposition reaction at room temperature, deposit
FTO substrate is taken out after 7 hours, is rinsed well, and be dried for standby with baking oven with deionized water, is used scanning electron microscope test
It is named as Pb with a thickness of 582 nm, this electrodexCu1-xS-7。
(2) the porous TiO of preparation CdSe quantum dot sensitization2Light anode (TiO2/CdSe)
With embodiment 1.
(3) it assembling quantum dot sensitization solar battery and tests
With embodiment 1.
Embodiment 4
(1) Pb is preparedxCu1-xS is to electrode
1) substrate is cleaned
With embodiment 1.
2) preparation of chemical bath deposition solution
With embodiment 1.
3) Pb is deposited in electro-conductive glass substrate surfacexCu1-xS is to electrode
The FTO electro-conductive glass substrate cleaned up is fixed on special fixture, substrate is then dipped vertically into deposition
In solution, with aluminium foil after the beaker sealing for filling solution, it is placed on magnetic stirring apparatus and carries out deposition reaction at room temperature, deposit
FTO substrate is taken out after 10 hours, is rinsed well with deionized water, and be dried for standby with baking oven, is surveyed using scanning electron microscope
It is tried with a thickness of 638 nm, this electrode is named as PbxCu1-xS-10。
(2) the porous TiO of preparation CdSe quantum dot sensitization2Light anode (TiO2/CdSe)
With embodiment 1.
(3) it assembling quantum dot sensitization solar battery and tests
With embodiment 1.
Embodiment 5
(1) Pb is preparedxCu1-xS is to electrode
1) substrate is cleaned
With embodiment 1.
2) preparation of chemical bath deposition solution
With embodiment 1.
3) Pb is deposited in electro-conductive glass substrate surfacexCu1-xS is to electrode
The FTO electro-conductive glass substrate cleaned up is fixed on special fixture, substrate is then dipped vertically into deposition
In solution, with aluminium foil after the beaker sealing for filling solution, it is placed on magnetic stirring apparatus and carries out deposition reaction at room temperature, deposit
FTO substrate is taken out after 15 hours, is rinsed well with deionized water, and be dried for standby with baking oven, is surveyed using scanning electron microscope
It is tried with a thickness of 672 nm, this electrode is named as PbxCu1-xS-15。
(2) the porous TiO of preparation CdSe quantum dot sensitization2Light anode (TiO2/CdSe)
With embodiment 1.
(3) it assembling quantum dot sensitization solar battery and tests
With embodiment 1.
Fig. 1 (a) is the surface SEM figure of FTO electro-conductive glass substrate, it can be seen that FTO conductive glass surface is rough,
SnO2Particle size is uneven, and corner angle are clearly demarcated, is in irregular fish scale-shaped.Fig. 1 (b) ~ (d) is respectively deposition 2 hours, 7 hours and 15
The Pb of hour preparationxCu1-xS electrode surface SEM figure, as we can see from the figure when deposited between be 2 hours when, SnO2The rib of particle
Angle becomes more rounded, implies that its surface deposited some nano particles, but the surface appearance feature of FTO is still as it can be seen that say
The nano particle of bright deposition is lower to the coverage rate of FTO, these exposed FTO substrates do not have catalytic activity to more sulphur electrolyte,
Battery performance is adversely affected after being assembled into device.After extending to 7 hours between when deposited, it can be clearly seen that FTO table
Face deposited the nano particle of one layer of even compact, and the shape characteristic of FTO fades away, and illustrate nano particle to FTO's
Coverage rate improves.Continue to extend to 15 hours between when deposited, nanoparticle size becomes larger, and the film of deposition is more and more thicker.And
And it is smoothly fine and close from things sample to can see sample surfaces, occurs without crackle, shows that film obtained has preferable matter
Amount.
Fig. 2 is the Pb for depositing preparation in 7 hoursxCu1-xS electrode section SEM schemes, as we can see from the figure PbxCu1-xS film
Thickness is relatively uniform, about 582 nm.
Fig. 3 is the Pb for depositing preparation in 7 hoursxCu1-xS electrode XRD diagram, it can be seen from the figure that in addition to substrate SnO2Spread out
It penetrates outside peak, and several new diffraction maximums (with mark) occurs, compare and find with standard diagram (JCPDS No.05-0592),
Cubic phase rock salt structure is corresponded respectively to positioned at 2 θ=26.02 °, 30.16 °, 43.12 °, the diffraction maximums of 71.04 ° and 84.26 °
(111), (200), (220), (420) and (511) crystal face of PbS illustrates in film containing this component of PbS, and be located at 2 θ=
27.50 °, 31.34 ° and 47.46 ° of diffraction maximum (with mark), with hexagonal crystal system CuS(JCPDS No. 06-0464's)
(101), (103) are corresponding with (110) crystal face, illustrate containing this component of CuS in film, so that prove to be prepared is
PbxCu1-xS film.
Fig. 4 is the Pb prepared by different sedimentation timesxCu1-xElectric current-electricity of the S to the quantum dot sensitized battery of electrode assembling
It buckles line, table 1 is the photoelectric properties parameter obtained from figure.It can be seen that being based on Pb from tablexCu1-xBattery of the S-2 to electrode
Photoelectric conversion efficiency is very low, and only 0.95%, this is because the Pb of FTO substrate surface depositionxCu1-xS catalyst amounts are very little, greatly
Barish FTO does not have catalytic activity to more sulphur electrolyte, too big to electrode/electrolyte interface resistance, has seriously affected electricity
The performance in pond.Extended between when deposited 7 hours, the PbS catalyst of the surface FTO deposition increases, to the catalytic performance of electrode into
One step improves, and makes PbxCu1-xThe cell photoelectric transfer efficiency of S-7 construction reaches 2.39%.When being continued growing between when deposited,
PbxCu1-xThe thickness of S further increases, and the internal resistance for making paired electrode becomes larger, to make to reduce the catalytic performance of electrode, battery
Photovoltaic parameter decline.
QDSSC photoelectric properties parameter of each ZnO/PbS of table 1 to electrode assembling
Embodiment 6
(1) preparation Pt is to electrode (comparison electrode)
1) substrate is cleaned
With embodiment 1.
2) the Pt Catalytic Layer for using magnetron sputtering method to deposit a layer thickness in FTO substrate surface as 100 nm or so.
(2) the porous TiO of preparation CdSe quantum dot sensitization2Light anode (TiO2/CdSe)
With embodiment 1.
(3) it assembling quantum dot sensitization solar battery and tests
With embodiment 1.
Fig. 5 is current -voltage curve of the Pt to the QDSSC of electrode assembling, as we can see from the figure the cell light of Pt assembling
Photoelectric transformation efficiency is 1.22%, is lower than PbxCu1-xThe photoelectric conversion efficiency of S-7 electrode 2.39%, this is because Pt is electrolysed more sulphur
Caused by the catalytic activity of liquid is weaker.
Claims (3)
1. a kind of preparation method to electrode for quantum dot sensitized solar battery, it is characterised in that: to the structure of electrode
To grow one layer of Catalytic Layer being made of PbS and CuS in FTO electro-conductive glass substrate surface, which is bathed using cryochemistry
Sedimentation is prepared, comprising the following steps:
1) substrate is cleaned
FTO electro-conductive glass substrate is sequentially placed into ethyl alcohol, acetone and deionized water added with detergent and is respectively cleaned by ultrasonic 15 points
Clock places into deionized water and is cleaned by ultrasonic 15 minutes, wash away the washing containing dirt to remove the dust and grease of substrate surface
Then agent and some inorganic pollutions are rinsed with deionized water ultrasound for 15 minutes again, finally spare with being dried with nitrogen；
2) preparation of chemical bath deposition solution
12.5mmol lead acetate, 50mmol sodium hydroxide, 20mmol thiocarbamide and 10mmol triethanolamine are dissolved in 400ml deionization
In water, it is mixing uniformly to form solution A；3.75mmol copper chloride and 8mmol triethanolamine are dissolved in 100ml deionized water,
It is mixing uniformly to form solution B；Then solution A is slowly added in solution B under agitation, continues stirring after ten minutes
Form chemical bath deposition solution；
3) Pb is deposited in FTO glass basic surfacexCu1-xS is to electrode
The FTO electro-conductive glass substrate cleaned up is fixed on fixture, then substrate is dipped vertically into deposition solution, uses aluminium
Foil is placed on magnetic stirring apparatus after the beaker sealing for filling solution and carries out deposition reaction at room temperature, after depositing a period of time
One layer of khaki or pewter Pb are formed in FTO glass basic surfacexCu1-xS film, sedimentation time is longer, and color is deeper；Instead
Electrode is taken out after answering, is rinsed well with deionized water, and is dried for standby with baking oven.
2. a kind of preparation method to electrode for quantum dot sensitized solar battery according to claim 1, feature
Be: deposition solution described in step (2) is in strong basicity, and pH value is 13 or so.
3. a kind of preparation method to electrode for quantum dot sensitized solar battery according to claim 1, feature
Be: sedimentation time described in step (3) is 2 ~ 15 hours, the Pb of formationxCu1-xS Catalytic Layer with a thickness of 150 ~ 700nm.
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| CN102208288A (en) * | 2011-03-08 | 2011-10-05 | 武汉大学 | Double-surface light-incident dye sensitized solar cell and preparation method thereof |
| CN102881457A (en) * | 2012-09-18 | 2013-01-16 | 中国科学院合肥物质科学研究院 | Universal method for preparing sulfide counter electrode by adopting soft chemical process |
| CN103560013A (en) * | 2013-11-07 | 2014-02-05 | 武汉大学 | Dye-sensitized solar cell with sulfide counter electrode and preparation method thereof |
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| CN102208288A (en) * | 2011-03-08 | 2011-10-05 | 武汉大学 | Double-surface light-incident dye sensitized solar cell and preparation method thereof |
| CN102881457A (en) * | 2012-09-18 | 2013-01-16 | 中国科学院合肥物质科学研究院 | Universal method for preparing sulfide counter electrode by adopting soft chemical process |
| CN103560013A (en) * | 2013-11-07 | 2014-02-05 | 武汉大学 | Dye-sensitized solar cell with sulfide counter electrode and preparation method thereof |
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