CN103897489A - Fluoridated polyimide-base ink-jet printer ink for solar cells and preparation method thereof - Google Patents
Fluoridated polyimide-base ink-jet printer ink for solar cells and preparation method thereof Download PDFInfo
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- CN103897489A CN103897489A CN201210588985.5A CN201210588985A CN103897489A CN 103897489 A CN103897489 A CN 103897489A CN 201210588985 A CN201210588985 A CN 201210588985A CN 103897489 A CN103897489 A CN 103897489A
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Abstract
The invention relates to a fluoridated polyimide-base ink-jet printer ink for solar cells and a preparation method thereof. The ink is prepared from the following components in percentage by weight: 0.5-5% of fluoridated polyamide resin solution (the solid content of resin is 1-10%), 0.0001-0.1% of nano aluminum powder, 0.1-1% of viscosity regulator and the balance of solvent. The product can directly enhance the generating efficiency of the flexible or thin-film solar cell when being printed to the upper surface of the flexible or thin-film solar cell by an ink-jet printing technique.
Description
Technical field
Fluorinated polyimide base ink for ink-jet printer and preparation method thereof for flexibility or thin-film solar cells, by using the surface of this ink printed at flexibility or thin-film solar cells incidence surface, directly improves the efficiency of flexibility or thin-film solar cells.
Background technology
Because High-tech Material aromatic series polypyromelliticimide (PI) resin has the thermotolerance, winter hardiness, oxidation-resistance, radiation resistance, chemical resistant properties of insoluble, infusibility, highest level, good machinery and electrical specification, be widely used in numerous areas.Particularly optically transparent PI film has special applications in some fields, as optics half-wave plate of the optical waveguide material in aligning film material, the communication field of flexible solar anti-radiation protection material, solar cell substrate material, flexible transparent conducting film baseplate material, liquid-crystal display and planar lightwave circuit etc.
Commercialization standard polyimide, due to the rigidity of its molecular backbone chain and strong intermolecular interaction, often makes their indissoluble infusibilities, and poor processability has limited their further application, is especially difficult to be processed into film and coating and uses.In addition, standard polyimide is due to aromatic conjugated property and strong charge-transfer interaction high in its molecular chain, makes its polymeric film have dark color (yellow or brown), optical transparence is poor; And light-coloured transparent polyimide has important using value in liquid-crystal display, optical waveguides.Therefore, design and modification for polyimide molecule structure, it is a very significant research work that preparation has the function such as good solubility and film-forming properties, high optical transparency polyimide. Recent study is found, fluorinated polyimide shows good solubility property conventionally, especially contains the polyetherimide that trifluoromethyl replaces structure.This quasi-polyimide is normally obtained by fluorine-containing bis ether diamine monomer and common dianhydride monomer polycondensation.Due to the physicochemical property of the large free volume of trifluoromethyl and fluorine atom uniqueness, as larger electronegativity, less atomic radius, lower mole polarizability etc., also make this quasi-polyimide show the better optical property of more traditional polyimide, dielectric properties and low rate of moisture absorption.But, owing to having introduced the flexible ehter bond (containing two in every structural unit) of larger proportion in such fluorochemical polyether imide molecular backbone chain, often make the resistance to elevated temperatures of this base polymer have a large reduction compared with standard polyimide, its second-order transition temperature is mostly at 200～300 DEG C.Along with deepening continuously to solubility and the investigation of materials of functional polyalkylene imide; be subject to gradually increasing attention containing fluorenyl Cardo type polyimide. because the huge free volume of fluorenyl and rigidity condensed ring structure give this quasi-polyimide good over-all properties; as solubility property good in organic solvent, part kind dissolves in hydrochloric ether and amide solvent; Excellent heat-resisting and thermo-oxidative stability energy; Good mechanical property and low-k etc. provide technical support for obtaining functional polyimide film novel materials such as thering is high solvable and high optical transparency.
Effectively utilizing in the middle of project of sun power: solar photovoltaic utilization is research field with fastest developing speed in the last few years, most active.The making of general solar cell is mainly taking semiconductor material as basis, opto-electronic conversion reaction generating occurs after utilizing photoelectric material to absorb luminous energy.According to the difference of material therefor, solar cell can be divided into: 1, silicon solar cell; 2, taking inorganic salt if the multi-element compounds such as gallium arsenide III-V compound, Cadmium Sulfide, copper indium diselenide are as the solar cell of material; 3, the solar cell of preparing with functional high molecule material; 4, nano-crystalline solar battery etc.
What prior art working efficiency was the highest is taking III-V family semiconductor inorganic materials as raw-material product.For example: the quantum well of the single junction type of gallium arsenide/germanium falls into crystal structure, and its photoelectric transformation efficiency can reach >18 %; For example, and multiple junction quantum well falls into the solar cell of crystal structure: InGaP/gallium arsenide/germanium, its photoelectric transformation efficiency can be up to >30 %.Most widely used at present, taking silicon as main: comprise non-crystalline silicon, photoelectric transformation efficiency approximately 9 %; Polysilicon, photoelectric transformation efficiency approximately 14 %; Silicon single crystal, photoelectric transformation efficiency approximately 17 %.Although in price, VI family elements Si is more cheap than III-V family semiconductor GaAs, the price of its manufacture, compared with polymer organic solar batteries, or expensive many; And in application, the light weight again overall plasticization organic solar batteries of the anxiety of crack-free can be realized via the processing of printing, except price reduces, be more suitable for the demand of portable electronic product, and indoor or cloudyly all can normally use (this is that siliceous solar cell is beyond one's reach), its practicality and market application range are promoted more.
Solar cell is a gordian technique, can advance more clean Energy production.But the Cost Problems of solar cell, has reduced the economic competitiveness of heliotechnics.For overcoming this problem, thin-film solar cells is the technology of current widespread use, can reduce in a large number the usage quantity of expensive semiconductor material, but the absorbing amount of thin-film solar cells is lower, and Performance Ratio is not gone up traditional solar cell.
Thin-film solar module is to be made up of glass substrate, metal level, transparency conducting layer, electrical function box, glueing material, semiconductor layer etc.Organic and inorganic composite solar battery is the solar cell based on organic conjugate polymer-inorganic nano-crystal composite system, because of while tool organic polymer material good film-forming property, level structure and band gap are easy to regulate, can prepare low cost, big area, flexible solar battery device and inorganic nano-crystal material high stability by wet method, high mobility, can construct the advantages such as ordered nano-structure, and become the study hotspot of area of solar cell in recent years.Metal nanoparticle can direct light enter solar cell better, prevents light escape.In traditional " thick film " solar cell, nanoparticle does not have any effect, is all by this film because all light absorbs, and this just relies on its thickness.But for film, nanoparticle just can be brought into play great role.Their scattering has increased light and has rested on the time in film, makes the light of overall absorption reach a kind of level, and traditional solar cell can match in excellence or beauty.
Aluminium and Nano silver grain are in the frequency spectrum of visible part, and focused ray enters solar cell well.But optical resonance also can cause nanoparticle absorb light, this efficiency that just means solar cell can be lower.Nano grain of silver sub-resonance is just in time in the crucial absorption spectrum part of solar cell, so the absorption of light is appreciable.Aluminum nanoparticles resonance has exceeded the crucial spectra part of solar cell.Loss to energy is less, and in addition, aluminum particulate is easy to passivation, although can change shape and size, after passivation, nanoparticle attribute change is very little.Nanoparticle has rough surface, and scattered beam can enter wide spectrum wavelength region more.This can bring larger absorption, thereby improves the whole efficiency of battery.
Ink-jet printing technology can form thin film layer by the uniform deposition of liquid organic materials, and therefore, this technology can solve large photoactivation thing dimensional problem in theory better.Drop on demand ink jet technique, can be accurately by deposition of material in position in the desired amount.Because ink-jet system is very high to the utilization ratio of material, can reduce manufacture production cost.
For adapting to above industrial requirement, we have invented fluorinated polyimide type nanometer aluminium powder ink.This ink passes through ink jet printing device, both can be used in the backlight place of thin-film solar cells, also can be used in the light inlet film surface of thin-film solar cells, also can be used in the middle layer of thin-film solar cells simultaneously, improve the efficiency of light absorption of solar cell.Improve the generating efficiency of solar cell.
Summary of the invention
The object of the present invention is to provide a kind of flexibility or thin-film solar cells fluorinated polyimide base ink for ink-jet printer and preparation method thereof, by using the surface of this ink printed at flexibility or thin-film solar cells incidence surface, directly improve the efficiency of flexibility or thin-film solar cells.And flexibility or thin-film solar cells that tool was processed through this ink have self-cleaning effect.
For achieving the above object, the technical solution used in the present invention is as follows:
Fluorinated polyimide base ink for ink-jet printer used for solar batteries of the present invention, is characterized in that, comprises the following component of following weight parts:
Solution (resin solid content 1-10%) 0.5-5% of fluorinated polyimide resin;
Nanometer aluminium powder 0.0001-0.1%;
Viscosity-controlling agent 0.1 ~ 1%;
Surplus is solvent.
Described fluorinated polyimide resin is group or the hydroxyl of, silicon fluorine-containing through introducing, phosphorus or introduces the substituting group that volume is larger (as cast structural and other large side groups or at 2 of biphenyl, substituting group is introduced to produce non-coplanar structure in 2 '-position) destroy conjugation in a big way or make macromolecular chain bending, introduce fat, especially alicyclic structure unit or employing can make the monomer of main chain bending (as 3,4 '-and 3,3 '-dianhydride, the diamines that position replaces) etc. the fluorinated polyimide resin of modification.
Such as Chinese patent CN102504255A, CN1970603A, CN102558556A, the disclosed polyimide resin of CN1018183B; Or document: 1. face is apt to silver etc., the novel synthetic and sign containing pyridine ring diamines and solvable transparent fluorinated polyimide thereof, synthetic technology and application the 03rd phase 5-12 in 2010,2. He Man etc., containing the preparation of benzothiazole fluorinated polyimide and nonlinear optical property, Acta PhySico-Chimica Sinica, 2010, the disclosed polyimide resin of 26,3073-3079.
Described solvent is one or more in alcohol, ester, ether, amine, acid amides, ketone or hydrocarbon.Be preferably and in ink, at least contain that to account for ink mass percent be 20% ketone, 20% ester, 10% ether.
Described alcohol is methyl alcohol, ethanol, propyl alcohol, Virahol, butanols, amylalcohol, hexanol, or one or more in the fluorinated alohol of above-mentioned alcohol.
Described ketone is acetone, cyclohexanone, one or more in methylethylketone, first isopropyl acetone, methyl ethyl ketone, diisobutyl ketone, diacetone alcohol, N-Methyl pyrrolidone.
Described ester is one or more in alcohol ether-ether, methyl acetate, ethyl acetate, acetic acid 1-methoxyl group-2-propyl ester, propyl acetate, butylacetate, methyl propionate or ethyl propionate, glycol ethers acetic ester, butyl glycol acetate.
Described ether is one or more in diethyl ether, dipropyl ether, tetrahydrofuran (THF), dioxan, ethylene glycol ethyl ether or ethylene glycol monomethyl ether.
Described viscosity-controlling agent is METHYLPYRROLIDONE or poly-3 methyl thiophene.
The preparation method of fluorinated polyimide base ink for ink-jet printer used for solar batteries of the present invention, comprises the steps:
(1) by solution, viscosity-controlling agent and the solvent of the fluorinated polyimide resin of formula ratio, in emulsify at a high speed device, process 10-60 minute, rotating speed 10000-100000 rpm, is processed into even mix emulsion fluid;
(2) after above mix emulsion fluid machines with under same processing rotating speed environment, in 10-20 minute by nanometer aluminium powder in batches trace add continuously;
(3) above emulsion is after nanometer aluminium powder adds completely, more fully emulsified 10-30 minute; The flexibility that both must need after strainer filterings more than 300 orders or thin-film solar cells fluorinated polyimide base ink for ink-jet printer for above emulsion.
Nano metal aluminum particulate is easy to passivation, although can change shape and size, after passivation, nanoparticle attribute change is very little.Nanoparticle has rough surface, and scattered beam can enter wide spectrum wavelength region more.This can bring larger absorption, thereby improves the whole efficiency of battery.The scattering of metallic aluminium nanoparticle has increased light and has rested on the time in film, makes the light of overall absorption reach a kind of level, and traditional solar cell can match in excellence or beauty.Through using the thin-film solar cells of ink processing of the present invention to improve 3-15% than the thin-film solar cells performance without the processing of this ink.Thin-film solar cells is used after this ink, and metallic aluminium nanoparticle can direct light enter solar cell preferably, prevents light escape.Solve in traditional " thick film " solar cell, nanoparticle does not have any effect and all essential problems that relies on thickness solution of light absorption.
Embodiment
Embodiment 1
(1) by 0.5Kg fluorinated polyimide resin, (resin solid content is 10%, Changchun applied chemistry institute), viscosity-controlling agent (METHYLPYRROLIDONE) 0.1Kg, 99.3995Kg N, dinethylformamide mixes, in emulsify at a high speed device, process 10-60 minute, rotating speed 10000-100000 rpm, is processed into even mix emulsion fluid;
(2) after above mix emulsion fluid machines with under same processing rotating speed environment, in 10-20 minute by 0.005Kg acetone nanometer aluminium powder in batches trace add continuously;
(3) above emulsion is after nanometer aluminium powder adds completely, more fully emulsified 10-30 minute; (5) above emulsion with after 500 object strainer filterings both flexible or thin-film solar cells fluorinated polyimide ink for ink-jet printer.
By the ink of the present embodiment, respectively according to national QB/T2730.1-2005, QB/T2603-2007, GB/T13217.2-2009, GB/T 18724-2008/ISO 2836:2004 standard detection.To the quality inspection index of ink, as proportion, pH value, surface tension, viscosity, specific conductivity etc. detect, detected result all meets national GB.Tested ink is poured in cold-resistant packing bottle, put into (20 ± 1) DEG C cryostat and take out to 24h, return to after room temperature, detect its print performance.Detected result: its reductibility is good, never degenerates, not spoiled.
Embodiment 2
(1) by 2Kg fluorinated polyimide resin, (resin solid content is 5%, Changchun applied chemistry institute), viscosity-controlling agent (METHYLPYRROLIDONE) 0.3Kg, be mixed with solution with 10Kg ethanol, 20Kg acetone, 67.6999Kg glycol ethers acetic ester, in emulsify at a high speed device, process 10-60 minute, rotating speed 10000-100000 rpm, is processed into even mix emulsion fluid;
(2) after above mix emulsion fluid machines with under same processing rotating speed environment, in 10-20 minute by 0.0001Kg acetone nanometer aluminium powder in batches trace add continuously;
(3) above emulsion is after nanometer aluminium powder adds completely, more fully emulsified 10-30 minute; Above emulsion with after 800 object strainer filterings both flexible or thin-film solar cells fluorinated polyimide ink for ink-jet printer.
By the ink of the present embodiment, respectively according to national QB/T2730.1-2005, QB/T2603-2007, GB/T13217.2-2009, GB/T 18724-2008/ISO 2836:2004 standard detection.To the quality inspection index of ink, as proportion, pH value, surface tension, viscosity, specific conductivity etc. detect, detected result all meets national GB.Tested ink is poured in cold-resistant packing bottle, put into (20 ± 1) DEG C cryostat and take out to 24h, return to after room temperature, detect its print performance.Detected result: its reductibility is good, never degenerates, not spoiled.
Embodiment 3
(1) by 3Kg fluorinated polyimide resin, (resin solid content is 3%, Changchun applied chemistry institute), viscosity-controlling agent (METHYLPYRROLIDONE) 0.8Kg, 25Kg methyl ethyl ketone, 31.15Kg ethylene glycol ethyl ether, 20Kg butylacetate mix, in emulsify at a high speed device, process 10-60 minute, rotating speed 10000-100000 rpm, is processed into even mix emulsion fluid;
(2) after above mix emulsion fluid machines with under same processing rotating speed environment, in 10-20 minute by 0.05Kg acetone nanometer aluminium powder in batches trace add continuously;
(3) above emulsion is after nanometer aluminium powder adds completely, more fully emulsified 10-30 minute; Above emulsion with after 1000 object strainer filterings both flexible or thin-film solar cells fluorinated polyimide ink for ink-jet printer.
By the ink of the present embodiment, respectively according to national QB/T2730.1-2005, QB/T2603-2007, GB/T13217.2-2009, GB/T 18724-2008/ISO 2836:2004 standard detection.To the quality inspection index of ink, as proportion, pH value, surface tension, viscosity, specific conductivity etc. detect, detected result all meets national GB.Tested ink is poured in cold-resistant packing bottle, put into (20 ± 1) DEG C cryostat and take out to 24h, return to after room temperature, detect its print performance.Detected result: its reductibility is good, never degenerates, not spoiled.
Embodiment 4
(1) by 4Kg fluorinated polyimide resin, (resin solid content is 8%, Ningbo Jinshan Electronic Materials Co., Ltd), viscosity-controlling agent (poly-3 methyl thiophene) 1Kg, be mixed with solution with 20Kg butyl glycol acetate, 10Kg butanols, 20Kg tetrahydrofuran (THF), 44.9 Kg ethyl propionates mix, in emulsify at a high speed device, process 10-60 minute, rotating speed 10000-100000 rpm, is processed into even mix emulsion fluid;
(2) after above mix emulsion fluid machines with under same processing rotating speed environment, in 10-20 minute by 0.1Kg acetone nanometer aluminium powder in batches trace add continuously;
(3) above emulsion is after nanometer aluminium powder adds completely, more fully emulsified 10-30 minute; Above emulsion with after 600 object strainer filterings both flexible or thin-film solar cells fluorinated polyimide ink for ink-jet printer.
By the ink of the present embodiment, respectively according to national QB/T2730.1-2005, QB/T2603-2007, GB/T13217.2-2009, GB/T 18724-2008/ISO 2836:2004 standard detection.To the quality inspection index of ink, as proportion, pH value, surface tension, viscosity, specific conductivity etc. detect, detected result all meets national GB.Tested ink is poured in cold-resistant packing bottle, put into (20 ± 1) DEG C cryostat and take out to 24h, return to after room temperature, detect its print performance.Detected result: its reductibility is good, never degenerates, not spoiled.
Embodiment 5
(1) by 5Kg fluorinated polyimide resin, (resin solid content is 1%, Ningbo Jinshan Electronic Materials Co., Ltd), viscosity-controlling agent (poly-3 methyl thiophene) 0.6Kg, use 10KgN, dinethylformamide, 20Kg acetone, 20Kg tetrahydrofuran (THF), 44.92Kg butylacetate are mixed with solution, in emulsify at a high speed device, process 10-60 minute, rotating speed 10000-100000 rpm, is processed into even mix emulsion fluid;
(2) after above mix emulsion fluid machines with under same processing rotating speed environment, in 10-20 minute by 0.08Kg acetone nanometer aluminium powder in batches trace add continuously;
(3) above emulsion is after nanometer aluminium powder adds completely, more fully emulsified 10-30 minute; Above emulsion with after 500 object strainer filterings both flexible or thin-film solar cells fluorinated polyimide ink for ink-jet printer.
By the ink of the present embodiment, respectively according to national QB/T2730.1-2005, QB/T2603-2007, GB/T13217.2-2009, GB/T 18724-2008/ISO 2836:2004 standard detection.To the quality inspection index of ink, as proportion, pH value, surface tension, viscosity, specific conductivity etc. detect, detected result all meets national GB.Tested ink is poured in cold-resistant packing bottle, put into (20 ± 1) DEG C cryostat and take out to 24h, return to after room temperature, detect its print performance.Detected result: its reductibility is good, never degenerates, not spoiled.
Claims (10)
1. a fluorinated polyimide base ink for ink-jet printer used for solar batteries, is characterized in that, comprises the following component of following weight parts:
Solution (resin solid content 1-10%) 0.5-5% of fluorinated polyimide resin;
Nanometer aluminium powder 0.0001-0.1%;
Viscosity-controlling agent 0.1 ~ 1%;
Surplus is solvent.
2. fluorinated polyimide base ink for ink-jet printer used for solar batteries according to claim 1, it is characterized in that: described polyimide resin is group or the hydroxyl of, silicon fluorine-containing through introducing, phosphorus or introduces the larger substituting group of volume and destroy conjugation in a big way or make macromolecular chain bending, introduce lipid structure unit or employing and can make the monomer modified polyimide resin of main chain bending.
3. fluorinated polyimide base ink for ink-jet printer used for solar batteries according to claim 1, is characterized in that: described solvent is one or more in alcohol, ester, ether, amine, acid amides, ketone or hydrocarbon.
4. fluorinated polyimide base ink for ink-jet printer used for solar batteries according to claim 3 is characterized in that: in described ink, contain ketone, ester and ether simultaneously.
5. fluorinated polyimide base ink for ink-jet printer used for solar batteries according to claim 3, is characterized in that: described alcohol is methyl alcohol, ethanol, propyl alcohol, Virahol, butanols, amylalcohol, hexanol, or one or more in the fluorinated alohol of above-mentioned alcohol.
6. according to the fluorinated polyimide base ink for ink-jet printer used for solar batteries described in claim 3 or 4, it is characterized in that: described ketone is acetone, cyclohexanone one or more in methylethylketone, first isopropyl acetone, methyl ethyl ketone, diisobutyl ketone, diacetone alcohol, N-Methyl pyrrolidone.
7. according to the fluorinated polyimide base ink for ink-jet printer used for solar batteries described in claim 3 or 4, it is characterized in that: described ester is one or more in alcohol ether-ether, methyl acetate, ethyl acetate, acetic acid 1-methoxyl group-2-propyl ester, propyl acetate, butylacetate, methyl propionate or ethyl propionate, glycol ethers acetic ester, butyl glycol acetate.
8. according to the fluorinated polyimide base ink for ink-jet printer used for solar batteries described in claim 3 or 4, it is characterized in that: described ether is one or more in diethyl ether, dipropyl ether, tetrahydrofuran (THF), dioxan, ethylene glycol ethyl ether or ethylene glycol monomethyl ether.
9. fluorinated polyimide base ink for ink-jet printer used for solar batteries according to claim 1, is characterized in that: described viscosity-controlling agent is METHYLPYRROLIDONE or poly-3 methyl thiophene.
10. the preparation method of fluorinated polyimide base ink for ink-jet printer used for solar batteries as claimed in claim 1, is characterized in that, comprises the steps:
(1) by solution, viscosity-controlling agent and the solvent of the fluorinated polyimide resin of formula ratio, in emulsify at a high speed device, process 10-60 minute, rotating speed 10000-100000 rpm, is processed into even mix emulsion fluid;
(2) after above mix emulsion fluid machines with under same processing rotating speed environment, in 10-20 minute by nanometer aluminium powder in batches trace add continuously;
(3) above emulsion is after nanometer aluminium powder adds completely, more fully emulsified 10-30 minute; The flexibility that both must need after strainer filterings more than 300 orders or thin-film solar cells fluorinated polyimide base ink for ink-jet printer for above emulsion.
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| CN109337437A (en) * | 2018-10-12 | 2019-02-15 | 楼乐超 | A kind of preparation process of solubility environment-friendly ink |
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| CN101010388A (en) * | 2005-03-04 | 2007-08-01 | 韩商英泰股份有限公司 | Conductive inks and manufacturing method thereof |
| CN102169739A (en) * | 2011-02-25 | 2011-08-31 | 乐山新天源太阳能电力有限公司 | Nanometer aluminum paste for solar battery and manufacturing method thereof |
| KR20110134800A (en) * | 2010-06-09 | 2011-12-15 | 한양대학교 산학협력단 | Thermochromic polymer containing aqueous solution for using as ink of ink-jet printer, preparation method thereof and printing method therewith |
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| CN101010388A (en) * | 2005-03-04 | 2007-08-01 | 韩商英泰股份有限公司 | Conductive inks and manufacturing method thereof |
| KR20110134800A (en) * | 2010-06-09 | 2011-12-15 | 한양대학교 산학협력단 | Thermochromic polymer containing aqueous solution for using as ink of ink-jet printer, preparation method thereof and printing method therewith |
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| CN109337437A (en) * | 2018-10-12 | 2019-02-15 | 楼乐超 | A kind of preparation process of solubility environment-friendly ink |
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