CN103219467B - Flexible polymer solar battery of corrugated structures and preparation method thereof - Google Patents
Flexible polymer solar battery of corrugated structures and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of flexible polymer solar battery of corrugated structures, comprise transparency electrode, hole transmission layer, photoactive layers material, electron transfer layer and metal electrode.Wherein, photoactive layers material comprises donor material and acceptor material.Transparency electrode is Graphene/PEDOT:PSS/PET composite membrane, hole transmission layer is PEDOT:PSS film, electron donor is P3HT, electron acceptor is Graphene/PEDOT:PSS compound particle, electron transfer layer is Zinc oxide film, metal electrode is silver.Adopt ink-jet printer in the PET film of pre-stretching, print the slurry of Graphene/PEDOT:PSS transparency conducting layer, hole transmission layer, active layer material, electron transfer layer and metal successively, and successively after process dry at 50 ~ 100 DEG C, removing prestretching force, namely obtains the flexible polymer solar battery of corrugated structures.The utilance of this battery to sunlight is high, photoelectric conversion efficiency is high, preparation technology is easy, and mechanical stability is good, can realize heavy industrialization preparation, be with a wide range of applications.
Description
Technical field
The present invention relates to a kind of polymer solar battery and preparation method thereof.
Background technology
Along with the aggravation of global energy crisis and environmental pollution, by clean regenerative resource---the solar cell that solar energy is converted into electric energy receives the great attention of countries in the world.In various solar cell, inorganic semiconductor solar cell, because electricity conversion is higher, technology maturation, has captured the solar cell market of the current overwhelming majority.But inorganic semiconductor solar cell also exists shortcomings, as high in cost, energy consumption is large, complex manufacturing technology, inflexibility, weight are large, be difficult to large area prepares, thus limits its large-scale application in a lot of fields.
Compared with conventional inorganic solar cell, flexible polymer solar battery cost is low, making is simple, be easy to large area manufacture, and flexible, and sensitive paper coin is the same can be bent arbitrarily, can be installed in almost Anywhere, comprise the top of house and vehicle, window or face glass, and there is floatation characteristic, make it can cover swimming pool or dam, reduce evaporation, simultaneously also produce power, therefore having application space more widely, is the study hotspot of current photovoltaic art.Current flexible polymer solar battery is in the laboratory research stage, by designing and control the chemical constitution of photoactive layers (electron donor and electron acceptor), obtained the electricity conversion of about 10.0%, close to or exceed the electricity conversion of flexible inorganic solar cell.But the polymer solar battery mechanical stability of high light electricity transformation efficiency is poor, because polymer solar battery is laminate structures, and the modulus of elasticity of every layer material, rigidity, ductility and the coefficient of expansion are all different, there is stretching, bending or action of thermal difference in preparation and use procedure, easily cause the destructions such as the unsticking between the fracture of functional layer, crackle generation and expansion and functional layer.Thus, the electricity conversion of polymer solar battery and the contradiction of mechanical stability multiple target performance optimization become one of problem that polymer solar battery research field urgently solves.2012, Yueh-LinLoo research group is by applying to strain in advance to polymer solar battery, functional layer is made to form fold pattern at flexible substrates surface wrinkling, thus make incident light, in photoactive layers, scattering occur, increase the efficiency of light absorption of photoactive layers, thus raising electricity conversion, relatively traditional open and flat pattern, improves about 37%.In addition, 2012, ZhenanBao research group passes through spin coating functional layer again after polymer solar battery flexible substrates Shi Hanzhang, after prestressing force removing, functional layer forms fold pattern at flexible substrates surface wrinkling equally, and result of study shows, this structure polymer solar cell is repeatedly comparatively after macrobending or tensile deformation amount, polymer solar battery photovoltaic performance is substantially constant, illustrates that the solar cell with fold pattern functional layer has good mechanical stability.From upper analysis, by applying prestrain to polymer solar battery, make functional layer at polymer solar battery flexible substrates surface wrinkling, be expected to the problem solving polymer solar battery electricity conversion and mechanical stability multiple target performance optimization contradiction.But the polymer solar battery electricity conversion of this structure relatively low (<2.0%) at present, have its source in the unreasonable structure designed, and preparation process is complicated, choosing asks a kind of simple method design to prepare a kind of flexible polymer solar battery of new construction, to realize polymer solar battery electricity conversion and the performance optimization of mechanical stability multiple target has very important significance.
Summary of the invention
The present invention is directed to polymer solar battery electricity conversion and mechanics stablizes the problem being difficult to simultaneously improve, provide flexible polymer solar battery of a kind of new construction and preparation method thereof.
Technical scheme provided by the invention is as follows:
A kind of flexible polymer solar battery of corrugated structures, it is characterized in that, described solar cell has corrugated structures, and its functional layer is the waveguiding structure (as shown in Figure 1) of long-range order, comprises successively: negative electrode, hole transmission layer, two-layer photoactive layers, electron transfer layer and metal anode; Wherein, described negative electrode is flexible transparent electrode, and photoactive layers comprises electron donor material and electron acceptor material.
Described flexible polymer solar battery, is characterized in that, described anode is metal A l, Ca, Mg, Li, Ag or In conducting film; Electron transfer layer is LiF, TiO
2, ZnO, CrO
x, CuO
x, Cs
2cO
3, CdSe, MoO
3or In
2s
3film; Photoactive layers 2 is phthalocyanine ketone or polythiophene class material and PEDOT:PSS/ Graphene or fullerene particle composite membrane; Photoactive layers 1 is phthalocyanine ketone or polythiophene class material and PEDOT:PSS/ Graphene or fullerene particle composite membrane; Hole transmission layer is PEDOT:PSS, MoO
3, NiO, CrO
x, CrN
xor WO
3-V
2o
5film; Negative electrode is Graphene/PEDOT:PSS composite membrane.
Described flexible polymer solar battery, is characterized in that, the thickness of described anode is 50nm ~ 500nm; The thickness of electron transfer layer is 10nm ~ 50nm; The thickness of photoactive layers 2 is 10nm ~ 50nm, and electron donor and electron acceptor mass ratio are 1:1.01 ~ 1.5; The thickness of photoactive layers 1 is 150nm ~ 250nm, and electron donor and electron acceptor mass ratio are 1.0:1.1 ~ 1.5; The thickness of hole transmission layer is 10nm ~ 30nm; The thickness of negative electrode is 5nm ~ 20nm.
Preferably, described negative electrode is Graphene/PEDOT:PSS/PET composite membrane, and hole transmission layer is PEDOT:PSS film, electron donor material is P3HT, electron acceptor material is Graphene/PEDOT:PSS compound particle, and electron transfer layer is Zinc oxide film, and metal anode is silver.
The present invention provides a kind of preparation method of flexible polymer solar battery of described corrugated structures simultaneously, it is characterized in that, ink-jet printer is adopted in the substrate of pre-stretching polymeric transparent, to print conductive, hole mobile material, photoactive layers material, electron transport material, metal electrode material successively successively, and dry process at 50 ~ 100 DEG C successively, namely removing prestretching force obtains corrugated structures flexible polymer solar battery.
The preparation method of described flexible polymer solar battery, comprises the steps:
The preparation of one .PEDOT:PSS/ graphene composite particle, comprising:
1.1) under condition of ice bath, 0.5 ~ 5.0g graphite is joined in the concentrated sulfuric acid of 60ml, strong agitation 30min, further by 12 ~ 30gKMnO
4join in above-mentioned mixed liquor, strong agitation 30min, above-mentioned mixed liquor is transferred in 30 DEG C of water-baths, slowly add 18 ~ 40gNaNO
3, stir 60min; Under agitation, 140ml deionized water is joined continuously in above-mentioned mixed liquor, then transferred in the oil bath of 90 DEG C of temperature, stir the 30min time; Dropwise add 10 ~ 15mlH again
2o
2, continue reaction 60min and make solution become glassy yellow from dark-brown;
1.2) under agitation, graphene oxide amount 5 ~ 25wt%PEDOT:PSS dispersing agent is added in above-mentioned graphene oxide solution, the hydrazine hydrate solution of 20ml ~ 60ml is dripped after dissolving, 1h is reacted at 80 DEG C of temperature, 20ml ~ 60ml acetic acid aqueous solution or hydriodic acid aqueous solution is dripped further in above-mentioned solution, continue reaction 60min, obtain stable graphene aqueous solution;
1.3) direct centrifugal above-mentioned graphene aqueous solution can obtain black precipitate, then water cleaning, after repeating twice, more centrifugal, with ethanol purge once, PEDOT:PSS/ graphene composite particle can be obtained;
Two. the ink preparation of flexible transparent electrode PEDOT:PSS/ graphene composite film:
PEDOT:PSS/ graphene composite particle 2 ~ 10wt%, PEDOT:PSS10 ~ 17wt%, only son's ethers 0.10 ~ 0.4wt%, defoamer 901 or 020.02 ~ 0.08wt% are scattered in water, stir;
Three. the preparation of hole transmission layer ink:
PEDOT:PSS5 ~ 10wt%, defoamer 901 or 020.05 ~ 0.12wt% are scattered in water, stir;
Four. the preparation of photoactive layers ink:
P3HT0.25wt% ~ 2.0wt%, PEDOT:PSS/ graphene composite particle 0.25wt% ~ 1.5wt%, only son's ethers 0.10 ~ 0.4wt%, defoamer 901 or 020.02 ~ 0.08wt% are scattered in water, stir;
Five. the preparation of Zinc oxide film ink:
5.1) by 2 ~ 10gZn (Ac)
22H
2o and 0.5 ~ 2.0gPVP is dissolved in 120ml methyl alcohol, under 70 DEG C of conditions, react 6h, can obtain the burnett's solution of good stability;
5.2) obtain white precipitate by centrifugal above-mentioned burnett's solution, then water cleaning, after repeating twice, more centrifugal, with ethanol purge once, PVP/ zinc oxide compound particle can be obtained;
5.3) ink that prepared by Zinc oxide film configures: be distributed in the aqueous solution by above-mentioned 1 ~ 5wt% zinc oxide compound particle, 0.10 ~ 0.4wt% only son ethers, 0.02 ~ 0.08wt% defoamer 901 or 02, stir under normal temperature;
Six. the preparation of silverskin ink:
6.1) be dissolved in 120ml distilled water by 0.5 ~ 2.0g silver nitrate and 0.5 ~ 3.0gPEDOT:PSS, under 40 DEG C of conditions, drip 0.5 ~ 2.0ml hydrazine hydrate, reaction 4h, can obtain the nano-silver hydrosol of good stability;
6.2) by above-mentioned nano-silver hydrosol, directly can obtain black precipitate by centrifugal, then water cleaning, after repeating twice, more centrifugal, with ethanol purge once, the silver-colored compound particle of PEDOT:PSS/ can be obtained;
6.3) ink that prepared by silverskin configures: be distributed in the aqueous solution by above-mentioned 1 ~ 5wt%PEDOT:PSS/ silver compound particle, 0.10 ~ 0.4wt% only son ethers, 0.02 ~ 0.08wt% defoamer 901 or 02, stir under normal temperature;
Seven. with the above-mentioned ink prepared, ink-jet printer is adopted in pre-stretching 5% ~ 25% polymer P ET transparent substrates, to print conductive, hole mobile material, photoactive layers material, electron transport material, metal electrode material successively successively, and dry process at 50 ~ 100 DEG C successively, namely removing prestretching force obtains corrugated structures flexible polymer solar battery.
The preparation method of described flexible polymer solar battery, step 1.2) in, the concentration of described acetic acid aqueous solution is 20 ~ 40wt%; The concentration of described hydriodic acid aqueous solution is 20 ~ 40wt%.
The preparation method of described flexible polymer solar battery, described in step 7, the base reservoir temperature of PET transparent substrates is 20 ~ 40 DEG C.
The preparation method of described flexible polymer solar battery, its solar cell prepared, its functional layer is orderly waveguiding structure, wave amplitude height size is 50nm ~ 10 μm, wave amplitude width size is 200nm ~ 40 μm, the type flexible polymer solar battery electricity conversion is 6.7% to the maximum, and repeat 20 times under 90-degree bent or stretching (deflection is less than 10%) condition, photoelectricity transfer efficient is substantially constant.
Beneficial effect of the present invention:
Functional layer in the present invention is orderly corrugated structures, and photoactive layers has higher sunlight utilance, can increase substantially the electricity conversion of polymer battery, also greatly increases the mechanical stability of polymer solar battery simultaneously.
The good grapheme material of high connductivity water stability all used by transparency electrode in the present invention, photoactive layers material, effectively can improve electricity conversion and the stability of polymer battery, and technique is simple, is conducive to large-scale production.
Polymer solar battery manufacture craft in the present invention all adopts inkjet technology, simplifies production process, reduces production cost, improve production efficiency, continuity can operate, has industrial value.
Accompanying drawing explanation
Fig. 1 solar battery structure figure of the present invention.
Wherein, 1-anode, 2-electron transfer layer, 3-photoactive layers 2,4-photoactive layers 1,5-hole transmission layer, 6-negative electrode.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment 1
1. the preparation of functional layer ink jet ink for printing
(1) preparation of PEDOT:PSS/ graphene composite particle
Under condition of ice bath, 1.5g graphite is joined in the concentrated sulfuric acid of 60ml, strong agitation 30min, further by 18gKMnO
4join in above-mentioned mixed liquor, strong agitation 30min.Above-mentioned mixed liquor is transferred in 30 DEG C of water-baths, slowly add 20gNaNO
3, stir 60min; Under agitation, 140ml deionized water is joined continuously in above-mentioned mixed liquor, then transferred in the oil bath of 90 DEG C of temperature, stir the 30min time; Dropwise add 12mlH again
2o
2, continue reaction 60min and make solution become glassy yellow from dark-brown; Under agitation, graphene oxide amount 10wt%PEDOT:PSS dispersing agent is added in above-mentioned glassy yellow graphene oxide solution, the hydrazine hydrate solution of 30ml is dripped after dissolving, 1h is reacted at 80 DEG C of temperature, 20ml acetic acid aqueous solution (concentration is 20wt%) is dripped further in above-mentioned solution, continue reaction 60min, obtain stable graphene aqueous solution; By above-mentioned graphene aqueous solution, directly can obtain black precipitate by centrifugal, then water cleaning, after repeating twice, more centrifugal, with ethanol purge once, PEDOT:PSS/ graphene composite particle can be obtained.
(2) preparation of PEDOT:PSS/ Graphene compound ink
2wt%PEDOT:PSS/ graphene composite particle, 10wt%PEDOT:PSS, 0.10% only son's ethers, 0.02wt% defoamer 901 are scattered in water, stir.
(3) preparation of PEDOT:PSS ink
5wt%PEDOT:PSS, 0.05wt% defoamer 901 is scattered in water, stirs.
(4) preparation of photoactive layers material ink
Photoactive layers 1
P3HT0.28wt%, PEDOT:PSS/ graphene composite particle 0.25wt%, 0.10% only son's ethers, 0.02% defoamer 901 are scattered in water, stir.
Photoactive layers 2
P3HT0.25wt%, PEDOT:PSS/ graphene composite particle 0.3wt%, 0.10% only son's ethers, 0.02% defoamer 901 are scattered in water, stir.
(5) preparation of zinc oxide ink
By 2gZn (Ac)
22H
2o and 0.5PVP is dissolved in 120ml methyl alcohol, under 70 DEG C of conditions, react 6h, can obtain the burnett's solution of good stability.By above-mentioned burnett's solution, directly can obtain white precipitate by centrifugal, then water cleaning, after repeating twice, more centrifugal, with ethanol purge once, PVP/ zinc oxide compound particle can be obtained.Above-mentioned 1wt% zinc oxide compound particle, 0.10wt% only son ethers, 0.02wt% defoamer 901 are distributed in the aqueous solution, stir under normal temperature and can obtain ink-jet printing ink.
(6) preparation of silver-colored ink
0.5g silver nitrate and 0.5gPEDOT:PSS are dissolved in 120ml distilled water, drip 0.5ml hydrazine hydrate under 40 DEG C of conditions, reaction 4h, can obtain the nano-silver hydrosol of good stability.By above-mentioned nano-silver hydrosol, directly can obtain black precipitate by centrifugal, then water cleaning, after repeating twice, more centrifugal, with ethanol purge once, the silver-colored compound particle of PEDOT:PSS/ can be obtained.Above-mentioned 1wt%PEDOT:PSS/ silver compound particle, 0.10 ~ 0.4wt% only son ethers, 0.02 ~ 0.08wt% defoamer 901 are distributed in the aqueous solution, stir under normal temperature and can obtain ink-jet printing ink.
2. inkjet printing flexible polymer solar battery
With the above-mentioned stable, aqueous solution prepared for ink-jet printing ink, ink-jet printer is adopted in pre-stretching 5% polymer P ET transparent substrates (base reservoir temperature is 30 DEG C), to print conductive, hole mobile material, photoactive layers material, electron transport material, metal electrode material successively successively, and dry process at 50 DEG C successively, namely removing prestretching force obtains corrugated structures flexible polymer solar battery.
Polymer solar battery is obtained by above technique, its functional layer is orderly waveguiding structure, wave amplitude size is 60nm, the wave amplitude cycle is 180nm, and wherein silver conductive film thickness is 150nm, Zinc oxide film thickness is 10nm, photoactive layers 2 film thickness is 10nm, photoactive layers 1 film thickness be 150nm, PEDOT:PSS film thickness is 10nm, Graphene/PEDOT:PSS composite film thickness is 5nm.The type flexible polymer solar battery electricity conversion is 5.7% to the maximum, and repeats 20 times under 90-degree bent or stretching (deflection is less than 10%) condition, and photoelectricity transfer efficient is 5.5%.
Embodiment 2
1. the preparation of functional layer ink jet ink for printing
(1) preparation of PEDOT:PSS/ graphene composite particle
Under condition of ice bath, 3.5g graphite is joined in the concentrated sulfuric acid of 60ml, strong agitation 30min, further by 20gKMnO
4join in above-mentioned mixed liquor, strong agitation 30min.Above-mentioned mixed liquor is transferred in 30 DEG C of water-baths, slowly add 23gNaNO
3, stir 60min; Under agitation, 140ml deionized water is joined continuously in above-mentioned mixed liquor, then transferred in the oil bath of 90 DEG C of temperature, stir the 30min time; Dropwise add 14mlH again
2o
2, continue reaction 60min and make solution become glassy yellow from dark-brown; Under agitation, graphene oxide amount 15wt%PEDOT:PSS dispersing agent is added in above-mentioned glassy yellow graphene oxide solution, the hydrazine hydrate solution of 30ml is dripped after dissolving, 1h is reacted at 80 DEG C of temperature, 30ml acetic acid aqueous solution (concentration is 30wt%) is dripped further in above-mentioned solution, continue reaction 60min, obtain stable graphene aqueous solution; By above-mentioned graphene aqueous solution, directly can obtain black precipitate by centrifugal, then water cleaning, after repeating twice, more centrifugal, with ethanol purge once, PEDOT:PSS/ graphene composite particle can be obtained.
(2) preparation of PEDOT:PSS/ Graphene compound ink
3wt%PEDOT:PSS/ graphene composite particle, 12wt%PEDOT:PSS, 0.11% only son's ethers, 0.03wt% defoamer 901 are scattered in water, stir.
(3) preparation of PEDOT:PSS ink
8wt%PEDOT:PSS, 0.06wt% defoamer 901 is scattered in water, stirs.
(4) preparation of photoactive layers material ink
Photoactive layers 1
0.30wt%P3HT, 0.25wt%PEDOT:PSS/ graphene composite particle, 0.10% only son's ethers, 0.02% defoamer 901 are scattered in water, stir.
Photoactive layers 2
P3HT0.50wt%, PEDOT:PSS/ graphene composite particle 0.7wt%, 0.13% only son's ethers, 0.04% defoamer 901 are scattered in water, stir.
(5) preparation of zinc oxide ink
By 2gZn (Ac)
22H
2o and 0.5PVP is dissolved in 120ml methyl alcohol, under 70 DEG C of conditions, react 6h, can obtain the burnett's solution of good stability.By above-mentioned burnett's solution, directly can obtain white precipitate by centrifugal, then water cleaning, after repeating twice, more centrifugal, with ethanol purge once, PVP/ zinc oxide compound particle can be obtained.Above-mentioned 2wt% zinc oxide compound particle, 0.12wt% only son ethers, 0.03wt% defoamer 901 are distributed in the aqueous solution, stir under normal temperature and can obtain ink-jet printing ink.
(6) preparation of silver-colored ink
1.0g silver nitrate and 1.2gPEDOT:PSS are dissolved in 120ml distilled water, drip 1.5ml hydrazine hydrate under 40 DEG C of conditions, reaction 4h, can obtain the nano-silver hydrosol of good stability.By above-mentioned nano-silver hydrosol, directly can obtain black precipitate by centrifugal, then water cleaning, after repeating twice, more centrifugal, with ethanol purge once, the silver-colored compound particle of PEDOT:PSS/ can be obtained.Above-mentioned 2wt%PEDOT:PSS/ silver compound particle, 0.2% only son's ethers, 0.03wt% defoamer 901 are distributed in the aqueous solution, stir under normal temperature and can obtain ink-jet printing ink.
2. inkjet printing flexible polymer solar battery
With the above-mentioned stable, aqueous solution prepared for ink-jet printing ink, ink-jet printer is adopted in pre-stretching 5% polymer P ET transparent substrates (base reservoir temperature is 30 DEG C), to print conductive, hole mobile material, photoactive layers material, electron transport material, metal electrode material successively successively, and dry process at 50 DEG C successively, namely removing prestretching force obtains corrugated structures flexible polymer solar battery.
Polymer solar battery is obtained by above technique, its functional layer is orderly waveguiding structure, wave amplitude size is 65nm, the wave amplitude cycle is 190nm, and wherein silver conductive film thickness is 350nm, Zinc oxide film thickness is 20nm, photoactive layers 2 film thickness is 30nm, photoactive layers 1 film thickness be 180nm, PEDOT:PSS film thickness is 15nm, Graphene/PEDOT:PSS composite film thickness is 10nm.The type flexible polymer solar battery electricity conversion is 6.1% to the maximum, and repeats 20 times under 90-degree bent or stretching (deflection is less than 10%) condition, and photoelectricity transfer efficient is 6.0%.
Embodiment 3
1. the preparation of functional layer ink jet ink for printing
(1) preparation of PEDOT:PSS/ graphene composite particle
Under condition of ice bath, 3.5g graphite is joined in the concentrated sulfuric acid of 60ml, strong agitation 30min, further by 20gKMnO
4join in above-mentioned mixed liquor, strong agitation 30min.Above-mentioned mixed liquor is transferred in 30 DEG C of water-baths, slowly add 23gNaNO
3, stir 60min; Under agitation, 140ml deionized water is joined continuously in above-mentioned mixed liquor, then transferred in the oil bath of 90 DEG C of temperature, stir the 30min time; Dropwise add 14mlH again
2o
2, continue reaction 60min and make solution become glassy yellow from dark-brown; Under agitation, graphene oxide amount 15wt%PEDOT:PSS dispersing agent is added in above-mentioned glassy yellow graphene oxide solution, the hydrazine hydrate solution of 30ml is dripped after dissolving, 1h is reacted at 80 DEG C of temperature, 30ml acetic acid aqueous solution (concentration is 30wt%) is dripped further in above-mentioned solution, continue reaction 60min, obtain stable graphene aqueous solution; By above-mentioned graphene aqueous solution, directly can obtain black precipitate by centrifugal, then water cleaning, after repeating twice, more centrifugal, with ethanol purge once, PEDOT:PSS/ graphene composite particle can be obtained.
(2) preparation of PEDOT:PSS/ Graphene compound ink
3wt%PEDOT:PSS/ graphene composite particle, 12wt%PEDOT:PSS, 0.11% only son's ethers, 0.03wt% defoamer 901 are scattered in water, stir.
(3) preparation of PEDOT:PSS ink
8wt%PEDOT:PSS, 0.06wt% defoamer 901 is scattered in water, stirs.
(4) preparation of photoactive layers material ink
Photoactive layers 1
0.30wt%P3HT, 0.25wt%PEDOT:PSS/ graphene composite particle, 0.10% only son's ethers, 0.02% defoamer 901 are scattered in water, stir.
Photoactive layers 2
P3HT0.50wt%, PEDOT:PSS/ graphene composite particle 0.7wt%, 0.13% only son's ethers, 0.04% defoamer 901 are scattered in water, stir.
(5) preparation of zinc oxide ink
By 2gZn (Ac)
22H
2o and 0.5PVP is dissolved in 120ml methyl alcohol, under 70 DEG C of conditions, react 6h, can obtain the burnett's solution of good stability.By above-mentioned burnett's solution, directly can obtain white precipitate by centrifugal, then water cleaning, after repeating twice, more centrifugal, with ethanol purge once, PVP/ zinc oxide compound particle can be obtained.Above-mentioned 2wt% zinc oxide compound particle, 0.12wt% only son ethers, 0.03wt% defoamer 901 are distributed in the aqueous solution, stir under normal temperature and can obtain ink-jet printing ink.
(6) preparation of silver-colored ink
1.0g silver nitrate and 1.2gPEDOT:PSS are dissolved in 120ml distilled water, drip 1.5ml hydrazine hydrate under 40 DEG C of conditions, reaction 4h, can obtain the nano-silver hydrosol of good stability.By above-mentioned nano-silver hydrosol, directly can obtain black precipitate by centrifugal, then water cleaning, after repeating twice, more centrifugal, with ethanol purge once, the silver-colored compound particle of PEDOT:PSS/ can be obtained.Above-mentioned 2wt%PEDOT:PSS/ silver compound particle, 0.2% only son's ethers, 0.03wt% defoamer 901 are distributed in the aqueous solution, stir under normal temperature and can obtain ink-jet printing ink.
2. inkjet printing flexible polymer solar battery
With the above-mentioned stable, aqueous solution prepared for ink-jet printing ink, ink-jet printer is adopted in pre-stretching 10% polymer P ET transparent substrates (base reservoir temperature is 30 DEG C), to print conductive, hole mobile material, photoactive layers material, electron transport material, metal electrode material successively successively, and dry process at 50 DEG C successively, namely removing prestretching force obtains corrugated structures flexible polymer solar battery.
Polymer solar battery is obtained by above technique, its functional layer is orderly waveguiding structure, wave amplitude size is 105nm, the wave amplitude cycle is 400nm, and wherein silver conductive film thickness is 350nm, Zinc oxide film thickness is 20nm, photoactive layers 2 film thickness is 30nm, photoactive layers 1 film thickness be 180nm, PEDOT:PSS film thickness is 15nm, Graphene/PEDOT:PSS composite film thickness is 10nm.The type flexible polymer solar battery electricity conversion is 5.4% to the maximum, and repeats 20 times under 90-degree bent or stretching (deflection is less than 10%) condition, and photoelectricity transfer efficient is 5.4%.
Embodiment 4
1. the preparation of functional layer ink jet ink for printing
(1) preparation of PEDOT:PSS/ graphene composite particle
Under condition of ice bath, 3.5g graphite is joined in the concentrated sulfuric acid of 60ml, strong agitation 30min, further by 20gKMnO
4join in above-mentioned mixed liquor, strong agitation 30min.Above-mentioned mixed liquor is transferred in 30 DEG C of water-baths, slowly add 23gNaNO
3, stir 60min; Under agitation, 140ml deionized water is joined continuously in above-mentioned mixed liquor, then transferred in the oil bath of 90 DEG C of temperature, stir the 30min time; Dropwise add 14mlH again
2o
2, continue reaction 60min and make solution become glassy yellow from dark-brown; Under agitation, graphene oxide amount 15wt%PEDOT:PSS dispersing agent is added in above-mentioned glassy yellow graphene oxide solution, the hydrazine hydrate solution of 30ml is dripped after dissolving, 1h is reacted at 80 DEG C of temperature, 30ml acetic acid aqueous solution (concentration is 30wt%) is dripped further in above-mentioned solution, continue reaction 60min, obtain stable graphene aqueous solution; By above-mentioned graphene aqueous solution, directly can obtain black precipitate by centrifugal, then water cleaning, after repeating twice, more centrifugal, with ethanol purge once, PEDOT:PSS/ graphene composite particle can be obtained.
(2) preparation of PEDOT:PSS/ Graphene compound ink
3wt%PEDOT:PSS/ graphene composite particle, 12wt%PEDOT:PSS, 0.11% only son's ethers, 0.03wt% defoamer 901 are scattered in water, stir.
(3) preparation of PEDOT:PSS ink
8wt%PEDOT:PSS, 0.06wt% defoamer 901 is scattered in water, stirs.
(4) preparation of photoactive layers material ink
Photoactive layers 1
1.1wt%P3HT, 1.0wt%PEDOT:PSS/ graphene composite particle, 0.10% only son's ethers, 0.02% defoamer 901 are scattered in water, stir.
Photoactive layers 2
P3HT1.1wt%, PEDOT:PSS/ graphene composite particle 1.4wt%, 0.13% only son's ethers, 0.04% defoamer 901 are scattered in water, stir.
(5) preparation of zinc oxide ink
By 2gZn (Ac)
22H
2o and 0.5PVP is dissolved in 120ml methyl alcohol, under 70 DEG C of conditions, react 6h, can obtain the burnett's solution of good stability.By above-mentioned burnett's solution, directly can obtain white precipitate by centrifugal, then water cleaning, after repeating twice, more centrifugal, with ethanol purge once, PVP/ zinc oxide compound particle can be obtained.Above-mentioned 2wt% zinc oxide compound particle, 0.12wt% only son ethers, 0.03wt% defoamer 901 are distributed in the aqueous solution, stir under normal temperature and can obtain ink-jet printing ink.
(6) preparation of silver-colored ink
1.0g silver nitrate and 1.2gPEDOT:PSS are dissolved in 120ml distilled water, drip 1.5ml hydrazine hydrate under 40 DEG C of conditions, reaction 4h, can obtain the nano-silver hydrosol of good stability.By above-mentioned nano-silver hydrosol, directly can obtain black precipitate by centrifugal, then water cleaning, after repeating twice, more centrifugal, with ethanol purge once, the silver-colored compound particle of PEDOT:PSS/ can be obtained.Above-mentioned 2wt%PEDOT:PSS/ silver compound particle, 0.2% only son's ethers, 0.03wt% defoamer 901 are distributed in the aqueous solution, stir under normal temperature and can obtain ink-jet printing ink.
2. inkjet printing flexible polymer solar battery
With the above-mentioned stable, aqueous solution prepared for ink-jet printing ink, ink-jet printer is adopted in pre-stretching 10% polymer P ET transparent substrates (base reservoir temperature is 30 DEG C), to print conductive, hole mobile material, photoactive layers material, electron transport material, metal electrode material successively successively, and dry process at 50 DEG C successively, namely removing prestretching force obtains corrugated structures flexible polymer solar battery.
Polymer solar battery is obtained by above technique, its functional layer is orderly waveguiding structure, wave amplitude size is 115nm, the wave amplitude cycle is 420nm, and wherein silver conductive film thickness is 350nm, Zinc oxide film thickness is 40nm, photoactive layers 2 film thickness is 30nm, photoactive layers 1 film thickness be 210nm, PEDOT:PSS film thickness is 15nm, Graphene/PEDOT:PSS composite film thickness is 10nm.The type flexible polymer solar battery electricity conversion is 6.7% to the maximum, and repeats 20 times under 90-degree bent or stretching (deflection is less than 10%) condition, and photoelectricity transfer efficient is 6.4%.
Embodiment 5
1. the preparation of functional layer ink jet ink for printing
(1) preparation of PEDOT:PSS/ graphene composite particle
Under condition of ice bath, 3.5g graphite is joined in the concentrated sulfuric acid of 60ml, strong agitation 30min, further by 20gKMnO
4join in above-mentioned mixed liquor, strong agitation 30min.Above-mentioned mixed liquor is transferred in 30 DEG C of water-baths, slowly add 23gNaNO
3, stir 60min; Under agitation, 140ml deionized water is joined continuously in above-mentioned mixed liquor, then transferred in the oil bath of 90 DEG C of temperature, stir the 30min time; Dropwise add 14mlH again
2o
2, continue reaction 60min and make solution become glassy yellow from dark-brown; Under agitation, graphene oxide amount 15wt%PEDOT:PSS dispersing agent is added in above-mentioned glassy yellow graphene oxide solution, the hydrazine hydrate solution of 30ml is dripped after dissolving, 1h is reacted at 80 DEG C of temperature, 30ml acetic acid aqueous solution (concentration is 30wt%) is dripped further in above-mentioned solution, continue reaction 60min, obtain stable graphene aqueous solution; By above-mentioned graphene aqueous solution, directly can obtain black precipitate by centrifugal, then water cleaning, after repeating twice, more centrifugal, with ethanol purge once, PEDOT:PSS/ graphene composite particle can be obtained.
(2) the ink preparation of PEDOT:PSS/ Graphene compound
3wt%PEDOT:PSS/ graphene composite particle, 12wt%PEDOT:PSS, 0.11% only son's ethers, 0.03wt% defoamer 901 are scattered in water, stir.
(3) preparation of PEDOT:PSS ink
8wt%PEDOT:PSS, 0.06wt% defoamer 901 is scattered in water, stirs.
(4) preparation of photoactive layers material ink
Photoactive layers 1
1.1wt%P3HT, 1.0wt%PEDOT:PSS/ graphene composite particle, 0.10% only son's ethers, 0.02% defoamer 901 are scattered in water, stir.
Photoactive layers 2
P3HT1.1wt%, PEDOT:PSS/ graphene composite particle 1.4wt%, 0.13% only son's ethers, 0.04% defoamer 901 are scattered in water, stir.
(5) preparation of zinc oxide ink
By 2gZn (Ac)
22H
2o and 0.5PVP is dissolved in 120ml methyl alcohol, under 70 DEG C of conditions, react 6h, can obtain the burnett's solution of good stability.By above-mentioned burnett's solution, directly can obtain white precipitate by centrifugal, then water cleaning, after repeating twice, more centrifugal, with ethanol purge once, PVP/ zinc oxide compound particle can be obtained.Above-mentioned 2wt% zinc oxide compound particle, 0.12wt% only son ethers, 0.03wt% defoamer 901 are distributed in the aqueous solution, stir under normal temperature and can obtain ink-jet printing ink.
(6) preparation of silver-colored ink
1.0g silver nitrate and 1.2gPEDOT:PSS are dissolved in 120ml distilled water, drip 1.5ml hydrazine hydrate under 40 DEG C of conditions, reaction 4h, can obtain the nano-silver hydrosol of good stability.By above-mentioned nano-silver hydrosol, directly can obtain black precipitate by centrifugal, then water cleaning, after repeating twice, more centrifugal, with ethanol purge once, the silver-colored compound particle of PEDOT:PSS/ can be obtained.Above-mentioned 2wt%PEDOT:PSS/ silver compound particle, 0.2% only son's ethers, 0.03wt% defoamer 901 are distributed in the aqueous solution, stir under normal temperature and can obtain ink-jet printing ink.
2. inkjet printing flexible polymer solar battery
With the above-mentioned stable, aqueous solution prepared for ink-jet printing ink, ink-jet printer is adopted in pre-stretching 20% polymer P ET transparent substrates (base reservoir temperature is 40 DEG C), to print conductive, hole mobile material, photoactive layers material, electron transport material, metal electrode material successively successively, and dry process at 50 DEG C successively, namely removing prestretching force obtains corrugated structures flexible polymer solar battery.
Polymer solar battery is obtained by above technique, its functional layer is orderly waveguiding structure, wave amplitude size is 8 μm, the spacing of wave amplitude is 38 μm, and wherein silver conductive film thickness is 355nm, Zinc oxide film thickness is 42nm, photoactive layers 2 film thickness is 30nm, photoactive layers 1 film thickness be 208nm, PEDOT:PSS film thickness is 18nm, Graphene/PEDOT:PSS composite film thickness is 12nm.The type flexible polymer solar battery electricity conversion is 5.1% to the maximum, and repeats 20 times under 90-degree bent or stretching (deflection is less than 10%) condition, and photoelectricity transfer efficient is 4.7%.
Claims (4)
1. the preparation method of the flexible polymer solar battery of a corrugated structures, it is characterized in that, ink-jet printer is adopted in the substrate of pre-stretching polymeric transparent, to print conductive, hole mobile material, photoactive layers material, electron transport material, metal electrode material successively successively, and dry process at 50 ~ 100 DEG C successively, namely removing prestretching force obtains corrugated structures flexible polymer solar battery, comprises the steps:
The preparation of one .PEDOT:PSS/ graphene composite particle, comprising:
1.1) under condition of ice bath, 0.5 ~ 5.0g graphite is joined in the concentrated sulfuric acid of 60ml, strong agitation 30min, further by 12 ~ 30gKMnO
4join in above-mentioned solution, strong agitation 30min, above-mentioned mixed liquor is transferred in 30 DEG C of water-baths, slowly add 18 ~ 40gNaNO
3, stir 60min; Under agitation, 140ml deionized water is joined continuously in above-mentioned mixed liquor, then transferred in the oil bath of 90 DEG C of temperature, stir the 30min time; Dropwise add 10 ~ 15mlH again
2o
2, continue reaction 60min and make solution become glassy yellow from dark-brown;
1.2) under agitation, the PEDOT:PSS dispersing agent of graphene oxide amount 5 ~ 25wt% is added in above-mentioned solution, the hydrazine hydrate solution of 20ml ~ 60ml is dripped after dissolving, 1h is reacted at 80 DEG C of temperature, 20ml ~ 60ml acetic acid aqueous solution or hydriodic acid aqueous solution is dripped further in above-mentioned solution, continue reaction 60min, obtain stable graphene aqueous solution;
1.3) direct centrifugal above-mentioned graphene aqueous solution can obtain black precipitate, then water cleaning, after repeating twice, more centrifugal, with ethanol purge once, PEDOT:PSS/ graphene composite particle can be obtained;
Two. the ink preparation of flexible transparent electrode PEDOT:PSS/ graphene composite film:
PEDOT:PSS/ graphene composite particle 2 ~ 10wt%, PEDOT:PSS10 ~ 17wt%, only son's ethers 0.10 ~ 0.4wt%, defoamer 901 or 020.02 ~ 0.08wt% are scattered in water, stir;
Three. the preparation of hole transmission layer ink:
PEDOT:PSS5 ~ 10wt%, defoamer 901 or 020.05 ~ 0.12wt% are scattered in water, stir;
Four. the preparation of photoactive layers ink:
P3HT0.25wt% ~ 2.0wt%, PEDOT:PSS/ graphene composite particle 0.25wt% ~ 1.5wt%, only son's ethers 0.10 ~ 0.4wt%, defoamer 901 or 020.02 ~ 0.08wt% are scattered in water, stir;
Five. the preparation of Zinc oxide film ink:
5.1) by 2 ~ 10gZn (Ac)
22H
2o and 0.5 ~ 2.0gPVP is dissolved in 120ml methyl alcohol, under 70 DEG C of conditions, react 6h, can obtain the burnett's solution of good stability;
5.2) obtain white precipitate by centrifugal above-mentioned burnett's solution, then water cleaning, after repeating twice, more centrifugal, with ethanol purge once, PVP/ zinc oxide compound particle can be obtained;
5.3) ink that prepared by Zinc oxide film configures: be distributed in the aqueous solution by 1 ~ 5wt%PVP/ zinc oxide compound particle, 0.10 ~ 0.4wt% only son ethers, 0.02 ~ 0.08wt% defoamer 901 or 02, stir under normal temperature;
Six. the preparation of silverskin ink:
6.1) be dissolved in 120ml distilled water by 0.5 ~ 2.0g silver nitrate and 0.5 ~ 3.0gPEDOT:PSS, under 40 DEG C of conditions, drip 0.5 ~ 2.0ml hydrazine hydrate, reaction 4h, can obtain the nano-silver hydrosol of good stability;
6.2) by above-mentioned nano-silver hydrosol, directly can obtain black precipitate by centrifugal, then water cleaning, after repeating twice, more centrifugal, with ethanol purge once, the silver-colored compound particle of PEDOT:PSS/ can be obtained;
6.3) ink that prepared by silverskin configures: be distributed in the aqueous solution by 1 ~ 5wt%PEDOT:PSS/ silver compound particle, 0.10 ~ 0.4wt% only son ethers, 0.02 ~ 0.08wt% defoamer 901 or 02, stir under normal temperature;
Seven. with the above-mentioned ink prepared, ink-jet printer is adopted in pre-stretching 5% ~ 25% polymer P ET transparent substrates, to print conductive, hole mobile material, photoactive layers material, electron transport material, metal electrode material successively successively, and dry process at 50 ~ 100 DEG C successively, namely removing prestretching force obtains corrugated structures flexible polymer solar battery.
2. the preparation method of flexible polymer solar battery as claimed in claim 1, is characterized in that, step 1.2) in, the concentration of described acetic acid aqueous solution is 20 ~ 40wt%; The concentration of described hydriodic acid aqueous solution is 20 ~ 40wt%.
3. the preparation method of flexible polymer solar battery as claimed in claim 1, it is characterized in that, described in step 7, the base reservoir temperature of PET transparent substrates is 20 ~ 40 DEG C.
4. the preparation method of flexible polymer solar battery as claimed in claim 1, it is characterized in that, its solar cell prepared, its functional layer is orderly waveguiding structure, and wave amplitude height size is 50nm ~ 10 μm, wave amplitude width size is 200nm ~ 40 μm.
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