CN103219467A - Flexible polymer solar battery with wrinkling structure and preparation method thereof - Google Patents
Flexible polymer solar battery with wrinkling structure and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a flexible polymer solar battery with a wrinkling structure, comprising a transparent electrode, a cavity transporting layer, photo-activation layer materials, an electron transporting layer and a metal electrode, wherein the photo-activation layer materials comprise a donor material and an acceptor material; the transparent electrode is made of graphene/PEDOT(poly(3,4-ethylenedioxythiophene):PSS(polystyrene sulfonate)/PET(polyethylene terephthalate) composite film; the hole transporting layer is made of a PEDOT:PSS film; an electron donor is made of P3HT; an electron acceptor is made of graphene/PEDOT:PSS composite particles; the electron transporting layer is made of a zinc-oxide film; and the metal electrode is made is silver. The flexible polymer solar battery is prepared by the following steps of: adopting an ink-jet printer to print a graphene/PEDOT:PSS transparent conducting layer, the hole transporting layer, active-layer materials, the electron transporting layer and metal slurry on a pre-stretched PET film in sequence, carrying out drying treatment on the materials under the temperature being 50-100 DEG C, then removing pre-stretching force and obtaining the flexible polymer solar battery with the wrinkling structure. The flexible polymer solar battery has the advantages that the sunlight utilization rate is high, the photoelectric conversion efficiency is high, the preparation process is simple and convenient, the mechanical stability is good, large-scale industrial preparation can be realized and the application prospect is wide.
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, with the cleaning regenerative resource---conversion of solar energy is the great attention that the solar cell of electric energy has been subjected to countries in the world.In various solar cells, the inorganic semiconductor solar cell is because higher, the technology maturation of electricity conversion has been captured the solar cell market of the present overwhelming majority.But the inorganic semiconductor solar cell exists many shortcomings, and, complex manufacturing technology big as cost height, energy consumption, inflexibility, weight be big, be difficult to large-area preparation etc., thereby limited its large-scale application in a lot of fields.
Compare with traditional inorganic solar cell, the flexible polymer solar battery cost is low, making is simple, be easy to the large tracts of land manufacturing, and flexible good, and the sensitive paper coin is the same can be crooked arbitrarily, can be installed in almost Anywhere, comprise top, window or the face glass of house and vehicle, and have floatation characteristic, make it can cover swimming pool or dam, reduce evaporation, while is produce power also, therefore has application space more widely, is the research focus in present photovoltaic field.Flexible polymer solar battery is in the laboratory research stage at present, chemical constitution by design and control photoactive layers (electron donor and electron acceptor), obtained about 10.0% electricity conversion, near or surpass the electricity conversion of flexible inorganic solar cell.But the polymer solar battery mechanical stability of higher electricity conversion is relatively poor, because polymer solar battery is a laminate structures, and the modulus of elasticity of every layer material, rigidity, ductility and the coefficient of expansion are all different, there are stretching, bending or action of thermal difference in preparation and the use, cause the destructions such as unsticking between fracture, crackle generation and the expansion and the functional layer of functional layer easily.Thereby the contradiction of the electricity conversion of polymer solar battery and the performance optimization of mechanical stability multiple target becomes one of urgent problem that solves of polymer solar battery research field.2012, Yueh-Lin Loo research group is by applying strain in advance to polymer solar battery, make functional layer form the fold pattern at the flexible substrates surface wrinkling, thereby make incident light that scattering take place in photoactive layers, increase the efficiency of light absorption of photoactive layers, thereby the raising electricity conversion, traditional relatively open and flat pattern improves about 37%.In addition, 2012, Zhenan Bao research group is by applying spin coating functional layer again behind the prestressing force to the polymer solar battery flexible substrates, after prestressing force is removed, functional layer forms the fold pattern at the flexible substrates surface wrinkling equally, and result of study shows, this structure polymer solar cell is after repeatedly than macrobending or tensile deformation amount, the polymer solar battery photovoltaic performance is constant substantially, illustrates that the solar cell with fold pattern functional layer has mechanical stability preferably.By last analysis as can be known, by polymer solar battery is applied prestrain, make functional layer at polymer solar battery flexible substrates surface wrinkling, be expected to solve the problem of 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, the unreasonable structure that has its source in and design, and preparation process complexity, choosing asks a kind of simple method design to prepare a kind of flexible polymer solar battery of new construction, has very important significance to realize polymer solar battery electricity conversion and the performance optimization of mechanical stability multiple target.
Summary of the invention
The present invention is directed to the stable problem that is difficult to improve simultaneously of polymer solar battery electricity conversion and mechanics, flexible polymer solar battery of a kind of new construction and preparation method thereof is provided.
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 the flexible and 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 the PEDOT:PSS film, electron donor material is P3HT, electron acceptor material is Graphene/PEDOT:PSS compound particle, and electron transfer layer is a Zinc oxide film, and metal anode is a 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, adopt ink-jet printer on pre-stretching polymer transparent substrates, to print conductive, hole mobile material, photoactive layers material, electron transport material, metal electrode material successively successively, and, remove prestretching force and promptly obtain the corrugated structures flexible polymer solar battery successively through 50～100 ℃ of following dried.
The preparation method of described flexible polymer solar battery comprises the steps:
The preparation of one .PEDOT:PSS/ Graphene compound particle comprises:
1.1) under condition of ice bath, 0.5～5.0g graphite is joined in the concentrated sulfuric acid of 60ml, strong agitation 30min is further with 12～30g KMnO
4Join in the above-mentioned mixed liquor, strong agitation 30min transfers to above-mentioned mixed liquor in 30 ℃ of water-baths, slowly adds 18～40gNaNO
3, stir 60min; Under stirring state, the 140ml deionized water is joined in the above-mentioned mixed liquor continuously, then it is transferred in the oil bath with 90 ℃ 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 stirring condition, in above-mentioned graphene oxide solution, add graphene oxide amount 5～25wt%PEDOT:PSS and disperse reagent, the dissolving back drips the hydrazine hydrate solution of 20ml～60ml, under 80 ℃ of temperature, react 1h, further in above-mentioned solution, drip 20ml～60ml acetic acid aqueous solution or hydriodic acid aqueous solution, continue reaction 60min, obtain stable graphene aqueous solution;
1.3) can directly centrifugal above-mentioned graphene aqueous solution obtain black precipitate, water cleans again, repeats twice after, centrifugal again, with the ethanol cleaning once, can obtain PEDOT:PSS/ Graphene compound particle;
Two. the ink preparation that flexible and transparent electrode PEDOT:PSS/ Graphene composite membrane is used:
PEDOT:PSS/ Graphene compound particle 2～10wt%, PEDOT:PSS10～17wt%, only son's ethers 0.10～0.4wt%, defoamer 901 or 020.02～0.08wt% are scattered in the water, and stirring gets final product;
Three. the hole transmission layer preparation of ink:
PEDOT:PSS5～10wt%, defoamer 901 or 020.05～0.12wt% are scattered in the water, and stirring gets final product;
Four. the photoactive layers preparation of ink:
P3HT0.25wt%～2.0wt%, PEDOT:PSS/ Graphene compound particle 0.25wt%～1.5wt%, only son's ethers 0.10～0.4wt%, defoamer 901 or 020.02～0.08wt% are scattered in the water, and stirring gets final product;
Five. the Zinc oxide film preparation of ink:
5.1) with 2～10gZn (Ac)
22H
2O and 0.5～2.0gPVP are dissolved in the 120ml methyl alcohol, react 6h under 70 ℃ of conditions, can obtain the burnett's solution of good stability;
5.2) can obtain white precipitate by centrifugal above-mentioned burnett's solution, water cleans again, repeats twice after, centrifugal again, with the ethanol cleaning once, can obtain PVP/ zinc oxide compound particle;
5.3) Zinc oxide film prepares the ink configuration of usefulness: above-mentioned 1～5wt% zinc oxide compound particle, 0.10～0.4wt% only son ethers, 0.02～0.08wt% defoamer 901 or 02 are distributed in the aqueous solution, and stirring under the normal temperature gets final product;
Six. the silverskin preparation of ink:
6.1) 0.5～2.0g silver nitrate and 0.5～3.0g PEDOT:PSS are dissolved in the 120ml distilled water, under 40 ℃ of conditions, drip 0.5～2.0ml hydrazine hydrate, react 4h, can obtain the Nano Silver hydrosol of good stability;
6.2) with the above-mentioned Nano Silver hydrosol, can be directly obtain black precipitate by centrifugal, water cleans again, repeats twice after, centrifugal again, clean once with ethanol, can obtain the silver-colored compound particle of PEDOT:PSS/;
6.3) silverskin prepares the ink configuration of usefulness: will the silver-colored compound particle of above-mentioned 1～5wt%PEDOT:PSS/, 0.10～0.4wt% only son ethers, 0.02～0.08wt% defoamer 901 or 02 be distributed in the aqueous solution, stirring under the normal temperature gets final product;
Seven. with the above-mentioned ink for preparing, adopt ink-jet printer on 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, remove prestretching force and promptly obtain the corrugated structures flexible polymer solar battery successively through 50～100 ℃ of following dried.
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, the base reservoir temperature of the described PET transparent substrates of step 7 is 20～40 ℃.
The preparation method of described flexible polymer solar battery, the solar cell of its preparation, its functional layer is orderly waveguiding structure, the wave amplitude height size is that 50nm～10 μ m, wave amplitude width size are 200nm～40 μ m, the type flexible polymer solar battery electricity conversion is 6.7% to the maximum, and under 90 ° of the bendings or (deflection is less than the 10%) condition of stretching, repeat 20 times, the photoelectricity transfer efficient is constant substantially.
Beneficial effect of the present invention:
Functional layer among the present invention is orderly corrugated structures, and photoactive layers has higher sunlight utilance, can increase substantially the electricity conversion of polymer battery, has also increased the mechanical stability of polymer solar battery simultaneously greatly.
Transparency electrode among the present invention, photoactive layers material are all used high conductivity water good stability grapheme material, can effectively improve the electricity conversion and stability of polymer battery, and technology are simple, helps large-scale production.
Polymer solar battery manufacture craft among the present invention all adopts inkjet technology, has simplified production process, has reduced production cost, has improved production efficiency, can continuity operate, and has industrial value.
Description of drawings
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
The present invention is further illustrated below in conjunction with specific embodiment.
Embodiment 1
1. the preparation of functional layer ink jet ink for printing
(1) preparation of PEDOT:PSS/ Graphene compound particle
Under condition of ice bath, 1.5g graphite is joined in the concentrated sulfuric acid of 60ml, strong agitation 30min is further with 18gKMnO
4Join in the above-mentioned mixed liquor strong agitation 30min.Above-mentioned mixed liquor is transferred in 30 ℃ of water-baths, slowly added 20gNaNO
3, stir 60min; Under stirring state, the 140ml deionized water is joined in the above-mentioned mixed liquor continuously, then it is transferred in the oil bath with 90 ℃ 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 stirring condition, in above-mentioned glassy yellow graphene oxide solution, add graphene oxide amount 10wt%PEDOT:PSS and disperse reagent, the dissolving back drips the hydrazine hydrate solution of 30ml, under 80 ℃ of temperature, react 1h, further in above-mentioned solution, drip 20ml acetic acid aqueous solution (concentration is 20wt%), continue reaction 60min, obtain stable graphene aqueous solution; With above-mentioned graphene aqueous solution, can be directly obtain black precipitate by centrifugal, water cleans again, repeats twice after, centrifugal again, with the ethanol cleaning once, can obtain PEDOT:PSS/ Graphene compound particle.
(2) preparation of the compound ink of PEDOT:PSS/ Graphene
2wt%PEDOT:PSS/ Graphene compound particle, 10wt%PEDOT:PSS, 0.10% only son's ethers, 0.02wt% defoamer 901 are scattered in the water, and stirring gets final product.
(3) preparation of PEDOT:PSS ink
5wt%PEDOT:PSS, 0.05wt% defoamer 901 are scattered in the water, and stirring gets final product.
(4) preparation of photoactive layers material ink
Photoactive layers 1
P3HT0.28wt%, PEDOT:PSS/ Graphene compound particle 0.25wt%, 0.10% only son's ethers, 0.02% defoamer 901 are scattered in the water, and stirring gets final product.
Photoactive layers 2
P3HT0.25wt%, PEDOT:PSS/ Graphene compound particle 0.3wt%, 0.10% only son's ethers, 0.02% defoamer 901 are scattered in the water, and stirring gets final product.
(5) preparation of zinc oxide ink
With 2gZn (Ac)
22H
2O and 0.5PVP are dissolved in the 120ml methyl alcohol, react 6h under 70 ℃ of conditions, can obtain the burnett's solution of good stability.With above-mentioned burnett's solution, can be directly by the centrifugal white precipitate that obtains, water cleans again, repeats twice after, centrifugal again, with the ethanol cleaning once, can obtain PVP/ zinc oxide compound particle.Above-mentioned 1wt% zinc oxide compound particle, 0.10wt% only son ethers, 0.02wt% defoamer 901 are distributed in the aqueous solution, and stirring under the normal temperature to obtain ink-jet printing ink.
(6) preparation of silver-colored ink
0.5g silver nitrate and 0.5g PEDOT:PSS are dissolved in the 120ml distilled water, under 40 ℃ of conditions, drip the 0.5ml hydrazine hydrate, react 4h, can obtain the Nano Silver hydrosol of good stability.With the above-mentioned Nano Silver hydrosol, can be directly obtain black precipitate by centrifugal, water cleans again, repeats twice after, centrifugal again, clean once with ethanol, can obtain the silver-colored compound particle of PEDOT:PSS/.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, and stirring under the normal temperature to obtain ink-jet printing ink.
2. inkjet printing flexible polymer solar battery
With the above-mentioned stable, aqueous solution for preparing is ink-jet printing ink, adopt ink-jet printer on pre-stretching 5% polymer P ET transparent substrates (base reservoir temperature is 30 ℃), to print conductive, hole mobile material, photoactive layers material, electron transport material, metal electrode material successively successively, and, remove prestretching force and promptly obtain the corrugated structures flexible polymer solar battery successively through 50 ℃ of following dried.
Obtain polymer solar battery by above technology, its functional layer is orderly waveguiding structure, the wave amplitude size is 180nm for 60nm, wave amplitude cycle, and wherein silver conductive film thickness is that 150nm, Zinc oxide film thickness are that 10nm, photoactive layers 2 film thicknesses are that 10nm, photoactive layers 1 film thickness are that 150nm, PEDOT:PSS film thickness are that 10nm, Graphene/PEDOT:PSS composite membrane thickness are 5nm.The type flexible polymer solar battery electricity conversion is 5.7% to the maximum, and repeats 20 times under 90 ° of the bendings or (deflection is less than the 10%) condition of stretching, and the 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 compound particle
Under condition of ice bath, 3.5g graphite is joined in the concentrated sulfuric acid of 60ml, strong agitation 30min is further with 20gKMnO
4Join in the above-mentioned mixed liquor strong agitation 30min.Above-mentioned mixed liquor is transferred in 30 ℃ of water-baths, slowly added 23gNaNO
3, stir 60min; Under stirring state, the 140ml deionized water is joined in the above-mentioned mixed liquor continuously, then it is transferred in the oil bath with 90 ℃ 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 stirring condition, in above-mentioned glassy yellow graphene oxide solution, add graphene oxide amount 15wt%PEDOT:PSS and disperse reagent, the dissolving back drips the hydrazine hydrate solution of 30ml, under 80 ℃ of temperature, react 1h, further in above-mentioned solution, drip 30ml acetic acid aqueous solution (concentration is 30wt%), continue reaction 60min, obtain stable graphene aqueous solution; With above-mentioned graphene aqueous solution, can be directly obtain black precipitate by centrifugal, water cleans again, repeats twice after, centrifugal again, with the ethanol cleaning once, can obtain PEDOT:PSS/ Graphene compound particle.
(2) preparation of the compound ink of PEDOT:PSS/ Graphene
3wt%PEDOT:PSS/ Graphene compound particle, 12wt%PEDOT:PSS, 0.11% only son's ethers, 0.03wt% defoamer 901 are scattered in the water, and stirring gets final product.
(3) preparation of PEDOT:PSS ink
8wt%PEDOT:PSS, 0.06wt% defoamer 901 are scattered in the water, and stirring gets final product.
(4) preparation of photoactive layers material ink
Photoactive layers 1
0.30wt%P3HT, 0.25wt%PEDOT:PSS/ Graphene compound particle, 0.10% only son's ethers, 0.02% defoamer 901 are scattered in the water, and stirring gets final product.
Photoactive layers 2
P3HT0.50wt%, PEDOT:PSS/ Graphene compound particle 0.7wt%, 0.13% only son's ethers, 0.04% defoamer 901 are scattered in the water, and stirring gets final product.
(5) preparation of zinc oxide ink
With 2gZn (Ac)
22H
2O and 0.5PVP are dissolved in the 120ml methyl alcohol, react 6h under 70 ℃ of conditions, can obtain the burnett's solution of good stability.With above-mentioned burnett's solution, can be directly by the centrifugal white precipitate that obtains, water cleans again, repeats twice after, centrifugal again, with the ethanol cleaning once, can obtain PVP/ zinc oxide compound particle.Above-mentioned 2wt% zinc oxide compound particle, 0.12wt% only son ethers, 0.03wt% defoamer 901 are distributed in the aqueous solution, and stirring under the normal temperature to obtain ink-jet printing ink.
(6) preparation of silver-colored ink
1.0g silver nitrate and 1.2g PEDOT:PSS are dissolved in the 120ml distilled water, under 40 ℃ of conditions, drip the 1.5ml hydrazine hydrate, react 4h, can obtain the Nano Silver hydrosol of good stability.With the above-mentioned Nano Silver hydrosol, can be directly obtain black precipitate by centrifugal, water cleans again, repeats twice after, centrifugal again, clean once with ethanol, can obtain the silver-colored compound particle of PEDOT:PSS/.Above-mentioned 2wt%PEDOT:PSS/ silver compound particle, 0.2% only son's ethers, 0.03wt% defoamer 901 are distributed in the aqueous solution, and stirring under the normal temperature to obtain ink-jet printing ink.
2. inkjet printing flexible polymer solar battery
With the above-mentioned stable, aqueous solution for preparing is ink-jet printing ink, adopt ink-jet printer on pre-stretching 5% polymer P ET transparent substrates (base reservoir temperature is 30 ℃), to print conductive, hole mobile material, photoactive layers material, electron transport material, metal electrode material successively successively, and, remove prestretching force and promptly obtain the corrugated structures flexible polymer solar battery successively through 50 ℃ of following dried.
Obtain polymer solar battery by above technology, its functional layer is orderly waveguiding structure, the wave amplitude size is 190nm for 65nm, wave amplitude cycle, and wherein silver conductive film thickness is that 350nm, Zinc oxide film thickness are that 20nm, photoactive layers 2 film thicknesses are that 30nm, photoactive layers 1 film thickness are that 180nm, PEDOT:PSS film thickness are that 15nm, Graphene/PEDOT:PSS composite membrane thickness are 10nm.The type flexible polymer solar battery electricity conversion is 6.1% to the maximum, and repeats 20 times under 90 ° of the bendings or (deflection is less than the 10%) condition of stretching, and the 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 compound particle
Under condition of ice bath, 3.5g graphite is joined in the concentrated sulfuric acid of 60ml, strong agitation 30min is further with 20gKMnO
4Join in the above-mentioned mixed liquor strong agitation 30min.Above-mentioned mixed liquor is transferred in 30 ℃ of water-baths, slowly added 23gNaNO
3, stir 60min; Under stirring state, the 140ml deionized water is joined in the above-mentioned mixed liquor continuously, then it is transferred in the oil bath with 90 ℃ 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 stirring condition, in above-mentioned glassy yellow graphene oxide solution, add graphene oxide amount 15wt%PEDOT:PSS and disperse reagent, the dissolving back drips the hydrazine hydrate solution of 30ml, under 80 ℃ of temperature, react 1h, further in above-mentioned solution, drip 30ml acetic acid aqueous solution (concentration is 30wt%), continue reaction 60min, obtain stable graphene aqueous solution; With above-mentioned graphene aqueous solution, can be directly obtain black precipitate by centrifugal, water cleans again, repeats twice after, centrifugal again, with the ethanol cleaning once, can obtain PEDOT:PSS/ Graphene compound particle.
(2) preparation of the compound ink of PEDOT:PSS/ Graphene
3wt%PEDOT:PSS/ Graphene compound particle, 12wt%PEDOT:PSS, 0.11% only son's ethers, 0.03wt% defoamer 901 are scattered in the water, and stirring gets final product.
(3) preparation of PEDOT:PSS ink
8wt%PEDOT:PSS, 0.06wt% defoamer 901 are scattered in the water, and stirring gets final product.
(4) preparation of photoactive layers material ink
Photoactive layers 1
0.30wt%P3HT, 0.25wt%PEDOT:PSS/ Graphene compound particle, 0.10% only son's ethers, 0.02% defoamer 901 are scattered in the water, and stirring gets final product.
Photoactive layers 2
P3HT0.50wt%, PEDOT:PSS/ Graphene compound particle 0.7wt%, 0.13% only son's ethers, 0.04% defoamer 901 are scattered in the water, and stirring gets final product.
(5) preparation of zinc oxide ink
With 2gZn (Ac)
22H
2O and 0.5PVP are dissolved in the 120ml methyl alcohol, react 6h under 70 ℃ of conditions, can obtain the burnett's solution of good stability.With above-mentioned burnett's solution, can be directly by the centrifugal white precipitate that obtains, water cleans again, repeats twice after, centrifugal again, with the ethanol cleaning once, can obtain PVP/ zinc oxide compound particle.Above-mentioned 2wt% zinc oxide compound particle, 0.12wt% only son ethers, 0.03wt% defoamer 901 are distributed in the aqueous solution, and stirring under the normal temperature to obtain ink-jet printing ink.
(6) preparation of silver-colored ink
1.0g silver nitrate and 1.2g PEDOT:PSS are dissolved in the 120ml distilled water, under 40 ℃ of conditions, drip the 1.5ml hydrazine hydrate, react 4h, can obtain the Nano Silver hydrosol of good stability.With the above-mentioned Nano Silver hydrosol, can be directly obtain black precipitate by centrifugal, water cleans again, repeats twice after, centrifugal again, clean once with ethanol, can obtain the silver-colored compound particle of PEDOT:PSS/.Above-mentioned 2wt%PEDOT:PSS/ silver compound particle, 0.2% only son's ethers, 0.03wt% defoamer 901 are distributed in the aqueous solution, and stirring under the normal temperature to obtain ink-jet printing ink.
2. inkjet printing flexible polymer solar battery
With the above-mentioned stable, aqueous solution for preparing is ink-jet printing ink, adopt ink-jet printer on pre-stretching 10% polymer P ET transparent substrates (base reservoir temperature is 30 ℃), to print conductive, hole mobile material, photoactive layers material, electron transport material, metal electrode material successively successively, and, remove prestretching force and promptly obtain the corrugated structures flexible polymer solar battery successively through 50 ℃ of following dried.
Obtain polymer solar battery by above technology, its functional layer is orderly waveguiding structure, the wave amplitude size is 400nm for 105nm, wave amplitude cycle, and wherein silver conductive film thickness is that 350nm, Zinc oxide film thickness are that 20nm, photoactive layers 2 film thicknesses are that 30nm, photoactive layers 1 film thickness are that 180nm, PEDOT:PSS film thickness are that 15nm, Graphene/PEDOT:PSS composite membrane thickness are 10nm.The type flexible polymer solar battery electricity conversion is 5.4% to the maximum, and repeats 20 times under 90 ° of the bendings or (deflection is less than the 10%) condition of stretching, and the 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 compound particle
Under condition of ice bath, 3.5g graphite is joined in the concentrated sulfuric acid of 60ml, strong agitation 30min is further with 20gKMnO
4Join in the above-mentioned mixed liquor strong agitation 30min.Above-mentioned mixed liquor is transferred in 30 ℃ of water-baths, slowly added 23gNaNO
3, stir 60min; Under stirring state, the 140ml deionized water is joined in the above-mentioned mixed liquor continuously, then it is transferred in the oil bath with 90 ℃ 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 stirring condition, in above-mentioned glassy yellow graphene oxide solution, add graphene oxide amount 15wt%PEDOT:PSS and disperse reagent, the dissolving back drips the hydrazine hydrate solution of 30ml, under 80 ℃ of temperature, react 1h, further in above-mentioned solution, drip 30ml acetic acid aqueous solution (concentration is 30wt%), continue reaction 60min, obtain stable graphene aqueous solution; With above-mentioned graphene aqueous solution, can be directly obtain black precipitate by centrifugal, water cleans again, repeats twice after, centrifugal again, with the ethanol cleaning once, can obtain PEDOT:PSS/ Graphene compound particle.
(2) preparation of the compound ink of PEDOT:PSS/ Graphene
3wt%PEDOT:PSS/ Graphene compound particle, 12wt%PEDOT:PSS, 0.11% only son's ethers, 0.03wt% defoamer 901 are scattered in the water, and stirring gets final product.
(3) preparation of PEDOT:PSS ink
8wt%PEDOT:PSS, 0.06wt% defoamer 901 are scattered in the water, and stirring gets final product.
(4) preparation of photoactive layers material ink
Photoactive layers 1
1.1wt%P3HT, 1.0wt%PEDOT:PSS/ Graphene compound particle, 0.10% only son's ethers, 0.02% defoamer 901 are scattered in the water, and stirring gets final product.
Photoactive layers 2
P3HT1.1wt%, PEDOT:PSS/ Graphene compound particle 1.4wt%, 0.13% only son's ethers, 0.04% defoamer 901 are scattered in the water, and stirring gets final product.
(5) preparation of zinc oxide ink
With 2gZn (Ac)
22H
2O and 0.5PVP are dissolved in the 120ml methyl alcohol, react 6h under 70 ℃ of conditions, can obtain the burnett's solution of good stability.With above-mentioned burnett's solution, can be directly by the centrifugal white precipitate that obtains, water cleans again, repeats twice after, centrifugal again, with the ethanol cleaning once, can obtain PVP/ zinc oxide compound particle.Above-mentioned 2wt% zinc oxide compound particle, 0.12wt% only son ethers, 0.03wt% defoamer 901 are distributed in the aqueous solution, and stirring under the normal temperature to obtain ink-jet printing ink.
(6) preparation of silver-colored ink
1.0g silver nitrate and 1.2g PEDOT:PSS are dissolved in the 120ml distilled water, under 40 ℃ of conditions, drip the 1.5ml hydrazine hydrate, react 4h, can obtain the Nano Silver hydrosol of good stability.With the above-mentioned Nano Silver hydrosol, can be directly obtain black precipitate by centrifugal, water cleans again, repeats twice after, centrifugal again, clean once with ethanol, can obtain the silver-colored compound particle of PEDOT:PSS/.Above-mentioned 2wt%PEDOT:PSS/ silver compound particle, 0.2% only son's ethers, 0.03wt% defoamer 901 are distributed in the aqueous solution, and stirring under the normal temperature to obtain ink-jet printing ink.
2. inkjet printing flexible polymer solar battery
With the above-mentioned stable, aqueous solution for preparing is ink-jet printing ink, adopt ink-jet printer on pre-stretching 10% polymer P ET transparent substrates (base reservoir temperature is 30 ℃), to print conductive, hole mobile material, photoactive layers material, electron transport material, metal electrode material successively successively, and, remove prestretching force and promptly obtain the corrugated structures flexible polymer solar battery successively through 50 ℃ of following dried.
Obtain polymer solar battery by above technology, its functional layer is orderly waveguiding structure, the wave amplitude size is 420nm for 115nm, wave amplitude cycle, and wherein silver conductive film thickness is that 350nm, Zinc oxide film thickness are that 40nm, photoactive layers 2 film thicknesses are that 30nm, photoactive layers 1 film thickness are that 210nm, PEDOT:PSS film thickness are that 15nm, Graphene/PEDOT:PSS composite membrane thickness are 10nm.The type flexible polymer solar battery electricity conversion is 6.7% to the maximum, and repeats 20 times under 90 ° of the bendings or (deflection is less than the 10%) condition of stretching, and the 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 compound particle
Under condition of ice bath, 3.5g graphite is joined in the concentrated sulfuric acid of 60ml, strong agitation 30min is further with 20gKMnO
4Join in the above-mentioned mixed liquor strong agitation 30min.Above-mentioned mixed liquor is transferred in 30 ℃ of water-baths, slowly added 23gNaNO
3, stir 60min; Under stirring state, the 140ml deionized water is joined in the above-mentioned mixed liquor continuously, then it is transferred in the oil bath with 90 ℃ 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 stirring condition, in above-mentioned glassy yellow graphene oxide solution, add graphene oxide amount 15wt%PEDOT:PSS and disperse reagent, the dissolving back drips the hydrazine hydrate solution of 30ml, under 80 ℃ of temperature, react 1h, further in above-mentioned solution, drip 30ml acetic acid aqueous solution (concentration is 30wt%), continue reaction 60min, obtain stable graphene aqueous solution; With above-mentioned graphene aqueous solution, can be directly obtain black precipitate by centrifugal, water cleans again, repeats twice after, centrifugal again, with the ethanol cleaning once, can obtain PEDOT:PSS/ Graphene compound particle.
(2) the compound ink preparation of PEDOT:PSS/ Graphene
3wt%PEDOT:PSS/ Graphene compound particle, 12wt%PEDOT:PSS, 0.11% only son's ethers, 0.03wt% defoamer 901 are scattered in the water, and stirring gets final product.
(3) preparation of PEDOT:PSS ink
8wt%PEDOT:PSS, 0.06wt% defoamer 901 are scattered in the water, and stirring gets final product.
(4) preparation of photoactive layers material ink
Photoactive layers 1
1.1wt%P3HT, 1.0wt%PEDOT:PSS/ Graphene compound particle, 0.10% only son's ethers, 0.02% defoamer 901 are scattered in the water, and stirring gets final product.
Photoactive layers 2
P3HT1.1wt%, PEDOT:PSS/ Graphene compound particle 1.4wt%, 0.13% only son's ethers, 0.04% defoamer 901 are scattered in the water, and stirring gets final product.
(5) preparation of zinc oxide ink
With 2gZn (Ac)
22H
2O and 0.5PVP are dissolved in the 120ml methyl alcohol, react 6h under 70 ℃ of conditions, can obtain the burnett's solution of good stability.With above-mentioned burnett's solution, can be directly by the centrifugal white precipitate that obtains, water cleans again, repeats twice after, centrifugal again, with the ethanol cleaning once, can obtain PVP/ zinc oxide compound particle.Above-mentioned 2wt% zinc oxide compound particle, 0.12wt% only son ethers, 0.03wt% defoamer 901 are distributed in the aqueous solution, and stirring under the normal temperature to obtain ink-jet printing ink.
(6) preparation of silver-colored ink
1.0g silver nitrate and 1.2g PEDOT:PSS are dissolved in the 120ml distilled water, under 40 ℃ of conditions, drip the 1.5ml hydrazine hydrate, react 4h, can obtain the Nano Silver hydrosol of good stability.With the above-mentioned Nano Silver hydrosol, can be directly obtain black precipitate by centrifugal, water cleans again, repeats twice after, centrifugal again, clean once with ethanol, can obtain the silver-colored compound particle of PEDOT:PSS/.Above-mentioned 2wt%PEDOT:PSS/ silver compound particle, 0.2% only son's ethers, 0.03wt% defoamer 901 are distributed in the aqueous solution, and stirring under the normal temperature to obtain ink-jet printing ink.
2. inkjet printing flexible polymer solar battery
With the above-mentioned stable, aqueous solution for preparing is ink-jet printing ink, adopt ink-jet printer on pre-stretching 20% polymer P ET transparent substrates (base reservoir temperature is 40 ℃), to print conductive, hole mobile material, photoactive layers material, electron transport material, metal electrode material successively successively, and, remove prestretching force and promptly obtain the corrugated structures flexible polymer solar battery successively through 50 ℃ of following dried.
Obtain polymer solar battery by above technology, its functional layer is orderly waveguiding structure, the wave amplitude size is that distance is 38 μ m between 8 μ m, the wave amplitude, and wherein silver conductive film thickness is that 355nm, Zinc oxide film thickness are that 42nm, photoactive layers 2 film thicknesses are that 30nm, photoactive layers 1 film thickness are that 208nm, PEDOT:PSS film thickness are that 18nm, Graphene/PEDOT:PSS composite membrane thickness are 12nm.The type flexible polymer solar battery electricity conversion is 5.1% to the maximum, and repeats 20 times under 90 ° of the bendings or (deflection is less than the 10%) condition of stretching, and the photoelectricity transfer efficient is 4.7%.
Claims (9)
1. the flexible polymer solar battery of a corrugated structures, it is characterized in that, described solar cell has corrugated structures, and its functional layer is the waveguiding structure of long-range order, comprises successively: negative electrode, hole transmission layer, two photoactive layers, electron transfer layer and metal anodes; Wherein, described negative electrode is the flexible and transparent electrode, and photoactive layers comprises electron donor material and electron acceptor material.
2. flexible polymer solar battery as claimed in claim 1 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.
3. flexible polymer solar battery as claimed in claim 2 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.
4. flexible polymer solar battery as claimed in claim 1, it is characterized in that, described negative electrode is Graphene/PEDOT:PSS/PET composite membrane, hole transmission layer is the PEDOT:PSS film, electron donor material is P3HT, electron acceptor material is Graphene/PEDOT:PSS compound particle, and electron transfer layer is a Zinc oxide film, and metal anode is a silver.
5. the preparation method of the flexible polymer solar battery of a corrugated structures, it is characterized in that, adopt ink-jet printer on pre-stretching polymer transparent substrates, to print conductive, hole mobile material, photoactive layers material, electron transport material, metal electrode material successively successively, and, remove prestretching force and promptly obtain the corrugated structures flexible polymer solar battery successively through 50～100 ℃ of following dried.
6. the preparation method of flexible polymer solar battery as claimed in claim 5 is characterized in that, comprises the steps:
The preparation of one .PEDOT:PSS/ Graphene compound particle comprises:
1.1) under condition of ice bath, 0.5～5.0g graphite is joined in the concentrated sulfuric acid of 60ml, strong agitation 30min is further with 12～30g KMnO
4Join in the above-mentioned mixed liquor, strong agitation 30min transfers to above-mentioned mixed liquor in 30 ℃ of water-baths, slowly adds 18～40gNaNO
3, stir 60min; Under stirring state, the 140ml deionized water is joined in the above-mentioned mixed liquor continuously, then it is transferred in the oil bath with 90 ℃ 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 stirring condition, in above-mentioned graphene oxide solution, add graphene oxide amount 5～25wt%PEDOT:PSS and disperse reagent, the dissolving back drips the hydrazine hydrate solution of 20ml～60ml, under 80 ℃ of temperature, react 1h, further in above-mentioned solution, drip 20ml～60ml acetic acid aqueous solution or hydriodic acid aqueous solution, continue reaction 60min, obtain stable graphene aqueous solution;
1.3) can directly centrifugal above-mentioned graphene aqueous solution obtain black precipitate, water cleans again, repeats twice after, centrifugal again, with the ethanol cleaning once, can obtain PEDOT:PSS/ Graphene compound particle;
Two. the ink preparation that flexible and transparent electrode PEDOT:PSS/ Graphene composite membrane is used:
PEDOT:PSS/ Graphene compound particle 2～10wt%, PEDOT:PSS10～17wt%, only son's ethers 0.10～0.4wt%, defoamer 901 or 020.02～0.08wt% are scattered in the water, and stirring gets final product;
Three. the hole transmission layer preparation of ink:
PEDOT:PSS5～10wt%, defoamer 901 or 020.05～0.12wt% are scattered in the water, and stirring gets final product;
Four. the photoactive layers preparation of ink:
P3HT0.25wt%～2.0wt%, PEDOT:PSS/ Graphene compound particle 0.25wt%～1.5wt%, only son's ethers 0.10～0.4wt%, defoamer 901 or 020.02～0.08wt% are scattered in the water, and stirring gets final product;
Five. the Zinc oxide film preparation of ink:
5.1) with 2～10gZn (Ac)
22H
2O and 0.5～2.0gPVP are dissolved in the 120ml methyl alcohol, react 6h under 70 ℃ of conditions, can obtain the burnett's solution of good stability;
5.2) can obtain white precipitate by centrifugal above-mentioned burnett's solution, water cleans again, repeats twice after, centrifugal again, with the ethanol cleaning once, can obtain PVP/ zinc oxide compound particle;
5.3) Zinc oxide film prepares the ink configuration of usefulness: above-mentioned 1～5wt% zinc oxide compound particle, 0.10～0.4wt% only son ethers, 0.02～0.08wt% defoamer 901 or 02 are distributed in the aqueous solution, and stirring under the normal temperature gets final product;
Six. the silverskin preparation of ink:
6.1) 0.5～2.0g silver nitrate and 0.5～3.0g PEDOT:PSS are dissolved in the 120ml distilled water, under 40 ℃ of conditions, drip 0.5～2.0ml hydrazine hydrate, react 4h, can obtain the Nano Silver hydrosol of good stability;
6.2) with the above-mentioned Nano Silver hydrosol, can be directly obtain black precipitate by centrifugal, water cleans again, repeats twice after, centrifugal again, clean once with ethanol, can obtain the silver-colored compound particle of PEDOT:PSS/;
6.3) silverskin prepares the ink configuration of usefulness: will the silver-colored compound particle of above-mentioned 1～5wt%PEDOT:PSS/, 0.10～0.4wt% only son ethers, 0.02～0.08wt% defoamer 901 or 02 be distributed in the aqueous solution, stirring under the normal temperature gets final product;
Seven. with the above-mentioned ink for preparing, adopt ink-jet printer on 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, remove prestretching force and promptly obtain the corrugated structures flexible polymer solar battery successively through 50～100 ℃ of following dried.
7. the preparation method of flexible polymer solar battery as claimed in claim 6 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%.
8. the preparation method of flexible polymer solar battery as claimed in claim 6 is characterized in that, the base reservoir temperature of the described PET transparent substrates of step 7 is 20～40 ℃.
9. the preparation method of flexible polymer solar battery as claimed in claim 6 is characterized in that, the solar cell of its preparation, and its functional layer is orderly waveguiding structure, the wave amplitude height size is that 50nm～10 μ m, wave amplitude width size are 200nm～40 μ m.
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