CN103897489B - Fluorinated polyimide base ink for ink-jet printer used for solar batteries and preparation method - Google Patents
Fluorinated polyimide base ink for ink-jet printer used for solar batteries and preparation method Download PDFInfo
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Abstract
A kind of fluorinated polyimide base ink for ink-jet printer used for solar batteries and preparation method thereof, including the following component of following weight parts: the 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.Product out made by the present invention, uses inkjet technology, spray printing to flexible or thin-film solar cells upper surface, directly raising flexibility or the generating efficiency of thin-film solar cells.
Description
Technical field
Flexibility or thin-film solar cells fluorinated polyimide base ink for ink-jet printer and preparation method thereof, by using this ink printed on flexible or the surface of thin-film solar cells incidence surface, directly improve the flexible or efficiency of thin-film solar cells.
Background technology
Owing to High-tech Material aromatic series polypyromelliticimide (PI) resin has insoluble, the thermostability of infusibility, highest level, tolerance to cold, non-oxidizability, radiation resistance, chemical resistance, good mechanically and electrically characteristic, it is widely used in numerous areas.The most optically transparent PI film has special applications in some fields, such as the optical waveguide material in flexible solar anti-radiation protection material, solar cell substrate material, flexible transparent conducting film baseplate material, the aligning film material of liquid crystal display, communication field and the optics half-wave plate etc. of planar lightwave circuit.
Commercialization standard polyimide, due to the rigidity of its molecular backbone and strong intermolecular interaction, often makes they indissoluble infusibilities, poor processability, limits their further application, is especially difficult to into thin film and coating uses.In addition, standard polyimide is due to aromatic conjugated property high in its strand and strong charge-transfer interaction so that it is it is poor that thin polymer film has deep color (yellow or brown), optical transparence;And light-coloured transparent polyimides has important using value in liquid crystal display, fiber waveguide.Therefore, it is designed for polyimide molecule structure and modified, preparation has good solubility and the function polyimides such as film property, high optical transparency is a research work the most significant. and Recent study finds, fluorinated polyimide typically exhibits preferable solubility property, especially contains trifluoromethyl and replaces the Polyetherimide of structure.This quasi-polyimide is typically to be obtained by fluorine-containing bis ether diamine monomer and common dianhydride monomer polycondensation.The free volume big due to trifluoromethyl and the physicochemical properties of fluorine atom uniqueness, such as bigger electronegativity, less atomic radius, relatively low mole polarizability etc., this quasi-polyimide is also made to show the more preferable optical property of more traditional polyimides, dielectric properties and low hydroscopicity.But, owing to such fluorochemical polyether acid imide molecular backbone introducing the flexible ether linkage (containing two in every construction unit) of larger proportion, the resistance to elevated temperatures often making this base polymer has a big reduction compared with standard polyimide, and its vitrification point is mostly at 200～300 DEG C.Along with solubility and functional polyalkylene acid imide investigation of materials are deepened continuously, containing fluorenyl
Cardo type polyimides is the most more and more paid attention to.
The free volume huge due to fluorenyl and rigidity condensed cyclic structure give the combination property that this quasi-polyimide is excellent, and such as the most excellent solubility property, part kind dissolves in chlorohydrocarbon and amide solvent;Excellent heat-resisting and thermo oxidative stability energy；Good mechanical performance and low-k etc. having the functional polyimide film new materials such as high solvable and high optical transparency for acquisition provides technical support.
Effectively utilize in the middle of project at solar energy: solar photovoltaic utilization is the most with fastest developing speed, most active research field.The making of general solaode is mainly based on semi-conducting material, utilizes photoelectric material that opto-electronic conversion reaction generating occurs after absorbing luminous energy.According to the difference of material therefor, solaode can be divided into: 1, silicon solar cell；2, with multi-element compounds solaodes as material such as inorganic salt such as GaAs III-V compound, cadmium sulfide, CISs；3, the solaode prepared with functional high molecule material；4, nano-crystalline solar battery etc..
What prior art work efficiency was the highest is with Group III-V semiconductor inorganic material is raw-material product.Such as: the quantum well of GaAs/germanium single junction type falls into crystal structure, its photoelectric transformation efficiency up to > 18 %；And multiple junction quantum well falls into the solar cell of crystal structure, such as: InGaP/GaAs/germanium, its photoelectric transformation efficiency may be up to > 30 %.The most most widely used, based on silicon: to include non-crystalline silicon, photoelectric transformation efficiency about 9 %；Polysilicon, photoelectric transformation efficiency about 14 %；Monocrystal silicon, photoelectric transformation efficiency about 17 %.Although in price, VI race elements Si is more cheap than Group III-V semiconductor GaAs, but its price manufactured, compared with macromolecule organic solar batteries, expensive many；And in application, the overall plasticization organic solar batteries of the anxiety of light weight crack-free again can realize via the processing of printing, in addition to price reduction, it is more suitable for the demand of portable electronic product, and all can normally use (this is that siliceous solaode is beyond one's reach) at indoor or cloudy day so that its practicality and market application range more promote.
Solaode is a key technology, can advance the production of energy more cleaned.But the Cost Problems of solaode, reduces the economic competitiveness of heliotechnics.For overcoming this problem, thin-film solar cells is the technology being widely used at present, and can reduce the usage amount of expensive semi-conducting material in a large number, but the absorbing amount of thin-film solar cells is relatively low, and performance is less than traditional solaode.
Thin-film solar module is made up of glass substrate, metal level, transparency conducting layer, electrical function box, glueing material, semiconductor layer etc..Organic-inorganic composite solaode is solaode based on organic conjugate polymer-inorganic nano-crystal composite system, because having high-molecular organic material good film-forming property simultaneously, level structure and band gap can easily be accommodated, low cost, large area, flexible solar battery device and inorganic nano-crystal material high stability can be prepared by wet method, high mobility, the advantages such as ordered nano-structure can be constructed, and become the study hotspot of area of solar cell in recent years.Metal nanoparticle can preferably enter solaode with direct light, prevents light from escaping.In traditional " thick film " solaode, nanoparticle does not has any effect, because all of light absorption is all by this film, this just relies on its thickness.But, for thin film, nanoparticle just can play great role.Their scattering adds light and stops the time in the film, makes the light of overall absorption reach a kind of level, and can match in excellence or beauty traditional solaode.
Aluminum and Nano silver grain, in the frequency spectrum of visible part, can focus light into solaode well.But optical resonance also results in nanoparticle absorbing light, this means that the efficiency of solaode can be relatively low.Nano grain of silver sub-resonance is just in solaode key absorption spectrum part, so the absorption of light is appreciable.Aluminum nanoparticles resonates beyond solaode key spectra part.Loss to energy is less, additionally, aluminum particulate is easy to passivation, although can change shapes and sizes, after passivation, nanoparticle attribute change is the least.Nanoparticle has rough surface, scattering light can enter wide spectrum wave-length coverage more.This can bring bigger absorption, thus improves the whole efficiency of battery.
Ink-jet printing technology can form thin layer by the uniform deposition of liquid organic material, and therefore, this technology can preferably solve big photoactivation thing dimensional problem in theory.Drop on demand ink jet technique, can be deposited on appropriate location by material the most in the desired amount.Owing to ink-jet system is the highest to the utilization rate of material, manufacture production cost can be reduced.
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 at the backlight of thin-film solar cells, can also be used in thin-film solar cells enters light film surface, can also be used in the intermediate layer of thin-film solar cells simultaneously, improves the efficiency of light absorption of solaode.Improve the generating efficiency of solaode.
Summary of the invention
It is an object of the invention 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 this ink printed on flexible or the surface of thin-film solar cells incidence surface, directly improve the flexible or efficiency of thin-film solar cells.And have, through the water-treated flexibility of this ink or thin-film solar cells, there is self-cleaning effect.
For achieving the above object, the technical solution used in the present invention is as follows:
The fluorinated polyimide base ink for ink-jet printer used for solar batteries of the present invention, it is characterised in that include 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 through introducing fluorine-containing, the group of silicon, phosphorus or hydroxyl or introducing the bigger substituent group of volume (such as cast structural and other big side bases or at the 2 of biphenyl, 2 '-position introduces substituent group to produce non-co-planar structure) destroy large range of conjugation or make macromolecular chain bend, introduce fat, especially alicyclic structure unit or employing can make the monomer of backbone twist (such as 3,4 '-and 3,3 '-dianhydride, the substituted diamidogen of meta) etc. modified fluorinated polyimide resin.
Polyimide resin disclosed in such as Chinese patent CN102504255A, CN1970603A, CN102558556A, CN1018183B；Or document: the 1. kind silver of face etc., novel containing pyridine ring diamidogen and the synthesis of fluorinated polyimide of the solvable transparency and sign, synthetic technology and application the 03rd phase 5-12 in 2010,2. He Man etc., prepare and nonlinear optical property containing benzothiazole fluorinated polyimide, Acta PhySico-Chimica Sinica, 2010, polyimide resin disclosed in 26,3073-3079.
Described solvent is one or more in alcohol, ester, ether, amine, amide, ketone or hydrocarbon.It is preferably in ink at least to contain and accounts for ketone that drop mass percentage ratio is 20%, the ester of 20%, the ether of 10%.
Described alcohol is one or more in methanol, ethanol, propanol, isopropanol, butanol, amylalcohol, hexanol, or the fluorinated alohol of above-mentioned alcohol.
Described ketone is acetone, cyclohexanone, one or more in butanone, first isopropyl acetone, methyl ethyl ketone, diisobutyl ketone, DAA, 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, butyl acetate, methyl propionate or ethyl propionate, glycol ethers acetas, butyl glycol acetate.
Described ether is one or more in diethyl ether, dipropyl ether, oxolane, dioxanes, ethylene glycol or ethylene glycol monomethyl ether.
Described viscosity-controlling agent is METHYLPYRROLIDONE or poly-3 methyl thiophene.
The preparation method of the fluorinated polyimide base ink for ink-jet printer used for solar batteries of the present invention, comprises the steps:
(1) solution of the fluorinated polyimide resin of formula ratio, viscosity-controlling agent and solvent are mixed, process 10-60 minute in high speed emulsator, rotating speed 10000-100000 rpm, be processed into uniform mix emulsion fluid；
(2), under same processing rotating speed environment, nanometer aluminium powder trace in batches is continuously added in 10-20 minute after emulsion mixed above machines；
(3) above emulsion is after nanometer aluminium powder adds completely, more fully emulsified 10-30 minute；Above the emulsion flexibility that both must need after strainer filterings more than 300 mesh or thin-film solar cells fluorinated polyimide base ink for ink-jet printer.
Nano metal aluminum particulate is easy to passivation, although can change shapes and sizes, after passivation, nanoparticle attribute change is the least.Nanoparticle has rough surface, scattering light can enter wide spectrum wave-length coverage more.This can bring bigger absorption, thus improves the whole efficiency of battery.The scattering of metallic aluminium nanoparticle adds light and stops the time in the film, makes the light of overall absorption reach a kind of level, and can match in excellence or beauty traditional solaode.Thin-film solar cells through using ink of the present invention to process improves 3-15% than the thin-film solar cells performance processed without this ink.After thin-film solar cells uses this ink, metallic aluminium nanoparticle can preferably enter solaode with direct light, prevents light from escaping.Solving in traditional " thick film " solaode, nanoparticle does not has any effect and all of light absorption must rely on the problem that thickness solves.
Detailed description of the invention
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, high speed emulsator processes 10-60 minute, rotating speed 10000-100000 rpm, is processed into uniform mix emulsion fluid；
(2) with under same processing rotating speed environment after emulsion mixed above machines, in 10-20 minute, 0.005Kg acetone nanometer aluminium powder trace in batches is continuously added to；
(3) above emulsion is after nanometer aluminium powder adds completely, more fully emulsified 10-30 minute；(5) above emulsion with after the strainer filtering of 500 mesh both flexible or thin-film solar cells fluorinated polyimide ink for ink-jet printer.
By the ink of the present embodiment, respectively according to country QB/T2730.1-2005, QB/T2603-2007, GB/T13217.2-2009, GB/T 18724-2008/ISO
2836:2004 standard detection.Quality inspection index to ink, detects such as proportion, pH value, surface tension, viscosity, electrical conductivity etc., and testing result all meets country's GB.Tested ink is poured in cold-resistant Packaging Bottle, puts in (-20 ± 1) DEG C cryostat and take out to 24h, after returning to room temperature, detect its print performance.Testing result: its reproducibility is good, never degenerates, the most 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 configured to solution with 10Kg ethanol, 20Kg acetone, 67.6999Kg glycol ethers acetas, high speed emulsator processes 10-60 minute, rotating speed 10000-100000 rpm, is processed into uniform mix emulsion fluid；
(2) with under same processing rotating speed environment after emulsion mixed above machines, in 10-20 minute, 0.0001Kg acetone nanometer aluminium powder trace in batches is continuously added to；
(3) above emulsion is after nanometer aluminium powder adds completely, more fully emulsified 10-30 minute；Above emulsion with after the strainer filtering of 800 mesh both flexible or thin-film solar cells fluorinated polyimide ink for ink-jet printer.
By the ink of the present embodiment, respectively according to country QB/T2730.1-2005, QB/T2603-2007, GB/T13217.2-2009, GB/T 18724-2008/ISO
2836:2004 standard detection.Quality inspection index to ink, detects such as proportion, pH value, surface tension, viscosity, electrical conductivity etc., and testing result all meets country's GB.Tested ink is poured in cold-resistant Packaging Bottle, puts in (-20 ± 1) DEG C cryostat and take out to 24h, after returning to room temperature, detect its print performance.Testing result: its reproducibility is good, never degenerates, the most 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, 20Kg butyl acetate mix, high speed emulsator processes 10-60 minute, rotating speed 10000-100000 rpm, is processed into uniform mix emulsion fluid；
(2) with under same processing rotating speed environment after emulsion mixed above machines, in 10-20 minute, 0.05Kg acetone nanometer aluminium powder trace in batches is continuously added to；
(3) above emulsion is after nanometer aluminium powder adds completely, more fully emulsified 10-30 minute；Above emulsion with after the strainer filtering of 1000 mesh both flexible or thin-film solar cells fluorinated polyimide ink for ink-jet printer.
By the ink of the present embodiment, respectively according to country QB/T2730.1-2005, QB/T2603-2007, GB/T13217.2-2009, GB/T 18724-2008/ISO
2836:2004 standard detection.Quality inspection index to ink, detects such as proportion, pH value, surface tension, viscosity, electrical conductivity etc., and testing result all meets country's GB.Tested ink is poured in cold-resistant Packaging Bottle, puts in (-20 ± 1) DEG C cryostat and take out to 24h, after returning to room temperature, detect its print performance.Testing result: its reproducibility is good, never degenerates, the most 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 configured to solution with 20Kg butyl glycol acetate, 10Kg butanol, 20Kg oxolane, 44.9 Kg ethyl propionate mixing, high speed emulsator processes 10-60 minute, rotating speed 10000-100000 rpm, is processed into uniform mix emulsion fluid；
(2) with under same processing rotating speed environment after emulsion mixed above machines, in 10-20 minute, 0.1Kg acetone nanometer aluminium powder trace in batches is continuously added to；
(3) above emulsion is after nanometer aluminium powder adds completely, more fully emulsified 10-30 minute；Above emulsion with after the strainer filtering of 600 mesh both flexible or thin-film solar cells fluorinated polyimide ink for ink-jet printer.
By the ink of the present embodiment, respectively according to country QB/T2730.1-2005, QB/T2603-2007, GB/T13217.2-2009, GB/T 18724-2008/ISO
2836:2004 standard detection.Quality inspection index to ink, detects such as proportion, pH value, surface tension, viscosity, electrical conductivity etc., and testing result all meets country's GB.Tested ink is poured in cold-resistant Packaging Bottle, puts in (-20 ± 1) DEG C cryostat and take out to 24h, after returning to room temperature, detect its print performance.Testing result: its reproducibility is good, never degenerates, the most 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 oxolane, 44.92Kg butyl acetate are configured to solution, high speed emulsator processes 10-60 minute, rotating speed 10000-100000 rpm, is processed into uniform mix emulsion fluid；
(2) with under same processing rotating speed environment after emulsion mixed above machines, in 10-20 minute, 0.08Kg acetone nanometer aluminium powder trace in batches is continuously added to；
(3) above emulsion is after nanometer aluminium powder adds completely, more fully emulsified 10-30 minute；Above emulsion with after the strainer filtering of 500 mesh both flexible or thin-film solar cells fluorinated polyimide ink for ink-jet printer.
By the ink of the present embodiment, respectively according to country's QB/T2730.1-2005, QB/T2603-2007, GB/T13217.2-2009, GB/T 18724-2008/ISO 2836:2004 standard detection.Quality inspection index to ink, detects such as proportion, pH value, surface tension, viscosity, electrical conductivity etc., and testing result all meets country's GB.Tested ink is poured in cold-resistant Packaging Bottle, puts in (-20 ± 1) DEG C cryostat and take out to 24h, after returning to room temperature, detect its print performance.Testing result: its reproducibility is good, never degenerates, the most spoiled.
Claims (9)
1. a fluorinated polyimide base ink for ink-jet printer used for solar batteries, it is characterised in that include the following component of following weight parts:
Resin solid content is the solution 0.5-5% of the fluorinated polyimide resin of 1-10%；
Nanometer aluminium powder 0.0001-0.1%；
Viscosity-controlling agent 0.1 ~ 1%；
Surplus is solvent；
Described fluorinated polyimide resin is through introducing fluorine-containing, the group of silicon, phosphorus or hydroxyl or introduce the bigger substituent group large range of conjugation of destruction of volume or make macromolecular chain bend, introducing lipid structure unit or use the monomer modified polyimide resin that can make backbone twist.
Fluorinated polyimide base ink for ink-jet printer used for solar batteries the most according to claim 1, it is characterised in that: described solvent is one or more in alcohol, ester, ether, amine, amide, ketone or hydrocarbon.
Fluorinated polyimide base ink for ink-jet printer used for solar batteries the most according to claim 2, it is characterised in that: described ink contains ketone, ester and ether simultaneously.
Fluorinated polyimide base ink for ink-jet printer used for solar batteries the most according to claim 2, it is characterised in that: described alcohol is one or more in methanol, ethanol, propanol, isopropanol, butanol, amylalcohol, hexanol, or the fluorinated alohol of above-mentioned alcohol.
5. according to the fluorinated polyimide base ink for ink-jet printer used for solar batteries described in Claims 2 or 3, it is characterized in that: described ketone is acetone, cyclohexanone, one or more in butanone, first isopropyl acetone, methyl ethyl ketone, diisobutyl ketone, DAA, N-Methyl pyrrolidone.
6. according to the fluorinated polyimide base ink for ink-jet printer used for solar batteries described in Claims 2 or 3, it is characterised 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, butyl acetate, methyl propionate or ethyl propionate, glycol ethers acetas, butyl glycol acetate.
7. according to the fluorinated polyimide base ink for ink-jet printer used for solar batteries described in Claims 2 or 3, it is characterised in that: described ether is one or more in diethyl ether, dipropyl ether, oxolane, dioxanes, ethylene glycol or ethylene glycol monomethyl ether.
Fluorinated polyimide base ink for ink-jet printer used for solar batteries the most according to claim 1, it is characterised in that: 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 the most as claimed in claim 1, it is characterised in that comprise the steps:
(1) solution of the fluorinated polyimide resin of formula ratio, viscosity-controlling agent and solvent are mixed, process 10-60 minute in high speed emulsator, rotating speed 10000-100000 rpm, be processed into uniform mix emulsion fluid；
(2), under same processing rotating speed environment, nanometer aluminium powder trace in batches is continuously added in 10-20 minute after emulsion mixed above machines；
(3) above emulsion is after nanometer aluminium powder adds completely, more fully emulsified 10-30 minute；The above emulsion fluorinated polyimide base ink for ink-jet printer used for solar batteries i.e. obtaining needs after strainer filterings more than 300 mesh.
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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 |
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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 |
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