CN103952795A - Lead core structure polyaniline/graphene composite nanometer fiber material preparation method - Google Patents
Lead core structure polyaniline/graphene composite nanometer fiber material preparation method Download PDFInfo
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Abstract
The invention relates to a lead core structure polyaniline/graphene composite nanometer fiber material preparation method. In organic polymer blue light materials, organic polyfluorene is adopted as a blue light material preparation device and has the maximum defect of the decreased material stability in the case of long term work of the device or long term heating on the device, and the approach for overcoming the problem is to improve performances of aging resistance, carrier transporting and heat transfer of the material so as to increase the color purity retention time of the device. The method comprises: adopting obtained soluble graphene as a core layer, adopting polyaniline as a shell layer, adopting a casing type device, adopting a high-voltage electrostatic spinning technology to prepare the lead core structure polyaniline/graphene composite nanometer fiber material, and making the lead core structure polyaniline/graphene composite nanometer fiber material into photoluminescent devices and electroluminescent devices. The preparation method is used for aniline monomer, polyaniline, graphene oxide and graphene oxide nanometer fiber materials, preparation methods and applications.
Description
technical field:
the present invention relates to a kind of lead for retractable pencil structure and there is the substituent three arylamine-fluorene copolymer of aryl oxide and Graphene composite nano-fiber material, preparation method and application.
background technology:
within 1969, first S.K. Deb uses amorphous WO
3
prepare electrochromic device, by gold electrode to WO
3
film applies voltage, WO
3
film starts to become blue from negative pole, changes polarity of voltage, WO
3
film fades from positive pole.This initiative work has caused the very big interest of people to electrochromism research.
electrochromism refers to that off-color material issues raw redox reaction ion doping and the reversible variation of visible color that presents at extra electric field.Electrochromic device has color adjustability and the characteristic such as operating voltage is low, at aspects such as electrochromic display, smart window and camouflages, has huge using value.The variable color development of recent research between from near-infrared to microwave region, exploitation is in the application in the fields such as the thermal control gain of heat of optical communication, data storage and building or reduction of heat.
although early stage electrochromic device mainly be take inorganic oxide as main, because organic material has better color adjustability, the high features such as variable color contrast, fast-response time and solution film forming processing and more and more comes into one's own.Graphene demonstrates certain application prospect with its unique two dimensional surface and electronic structure, excellent performance in fields such as opto-electronic device and electrode materials.Graphene and derivative thereof have the features such as great specific area and easy modification and are suitable for developing high performance composite.The present invention organically combines Graphene and three arylamine polymers by high-voltage electrostatic spinning technology, and the introducing of Graphene has further promoted electron collection and the transmission of three arylamine polymer electroluminescent materials.
summary of the invention:
the object of the invention is synthetic a kind ofly to there are the substituent three arylamine monomers of aryl oxide, and utilize this monomer and a kind of polyaniline of fluorenes copolymerization; Utilize high-voltage electrostatic spinning technology that a kind of lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material preparation method is provided.
the object of the present invention is achieved like this:
a kind of method for making of lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material, the solubility Graphene obtaining of take is sandwich layer, polyaniline is shell, by bushing type device, utilize high-voltage electrostatic spinning technology to prepare a kind of lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material, and this composite nano-fiber material is made to luminescence generated by light, electroluminescent device.
the method for making of described lead for retractable pencil structure polyaniline/Graphene composite nano fiber, the first step: described polyaniline is dissolved in solvent, to gather [2,7-(9,9-dioctyl fluorene)-alternately-N-phenyl-N-(4-Phenoxyphenyl) aniline] be dissolved in toluene or tetrahydrofuran solvent, content is 1.0～12.0% (wt.%); Second step: the described ethanol of solubility Graphene or the concentration of the aqueous solution are 0.5～6.0% (wt.%), by bushing type syringe needle, the flow velocity ratio of utilizing micro-injection pump to control two kinds of solution is 1:0.2～1:3.0, polyaniline: Graphene, wherein, polyaniline solutions is as shell, and graphene solution is as core or sandwich layer; The 3rd step: under 18～30 ℃ of conditions, utilize high-voltage electrostatic spinning technology, adjusting spinning voltage is 10～30kV, and the distance between emission electrode and collecting electrode is 8～23cm, can on collecting electrode, obtain lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material.
the method for making of described lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material, described polyaniline is the polyaniline containing phenoxy group fluorine-triphenylamine structure, its preparation method is that the triphenylamine monomer (Mon) containing phenoxy group that purify the to obtain one-step polymerization of going forward side by side obtains poly-[2,7-(9,9-dioctyl fluorene)-alternately-N-phenyl-N-(4-Phenoxyphenyl) aniline]; Concrete steps are: take refined toluene as solvent, 1mmol triphenylamine monomer adds the ratio of toluene 10～25mL, adopt 9,9-dioctyl fluorene-2,7-hypoboric acid, along (1,3-PD) ester with containing the triphenylamine of phenoxy group, is that 1:1.0～1:1.05 adds according to mol ratio; Adding part by weight is the palladium catalyst Pd (PPh of 1:25～1:30 3 ) 4 , described palladium catalyst Pd (PPh 3 ) 4 with 9,9-dioctyl fluorene-2,7-hypoboric acid is along (1; ammediol) ratio of ester is 1:25～1:30; add the sodium carbonate liquor with the isopyknic 2.5～3.0M of toluene, under high-purity argon gas or nitrogen protection, the polyaniline by the preparation of Suzuki coupling reaction containing phenoxy group fluorine-triphenylamine structure.
the preparation method of described lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material, the preparation process of described solubility Graphene: take the reagent such as crystalline flake graphite, the concentrated sulfuric acid, phosphoric acid, potassium permanganate and hydrogen peroxide and prepare graphene oxide; Utilize above-mentioned graphene oxide modulation to obtain the graphite oxide aqueous solution that concentration is 8mgmL-1; Get this graphite oxide aqueous solution of 26mL and join in three-necked bottle, under heating, stirring condition, add the TGA of 1mL to carry out redox, the time is 2～3h, obtains the aqueous solution of Graphene (T-RGO); 200 μ L ammoniacal liquor are added dropwise in above-mentioned graphene aqueous solution, more than ultrasonic 10min, under heating, stirring condition, add 0.4g hydroxylamine hydrochloride, reaction 2h, obtains Graphene, cleans standby; The ratio of the volume of the described concentrated sulfuric acid and the quality of crystalline flake graphite is 4mL:1g～6mL:1g, the described concentrated sulfuric acid and the volume ratio of phosphoric acid are 8:1～10:1, described potassium permanganate and the mass ratio of crystalline flake graphite are 7:1～8:1, described deionized water and the volume ratio of the concentrated sulfuric acid are 4:1～6:1, the described concentrated sulfuric acid and the volume ratio of hydrogen peroxide are 1:1～3:1, described hydrogen peroxide mass concentration is 25～35%, and described mixing speed is 200～300rpm; Described heating-up temperature is 80～85 ℃.
the preparation method of described lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material, the described chemical formula containing phenoxy group polyaniline polymer is poly-[2,7-(9,9-dioctyl fluorene)-alternately-N-phenyl-N-(4-Phenoxyphenyl) aniline], polymer number-average molecular weight is 13,302～31,235.
device prepared by lead for retractable pencil structure polyaniline/Graphene composite nano fiber prepared by the preparation method of described lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material, lead for retractable pencil structure polyaniline/Graphene composite nano fiber diameter is 100～600nm, wherein gather [2,7-(9,9-dioctyl fluorene)-alternately-N-phenyl-N-(4-Phenoxyphenyl) aniline] as the shell of composite nano-fiber material, thickness is 20～100nm; Graphene is as core or the stratum nucleare of lead for retractable pencil structure composite nano-fiber material, and diameter is 60～400nm; The thickness of described lead for retractable pencil structure poly-[2,7-(9,9-dioctyl fluorene)-alternately-N-phenyl-N-(4-Phenoxyphenyl) aniline]/Graphene composite nano-fiber material film is 100nm～75 μ m, and fibre length is 15 μ m～15cm.
device prepared by described lead for retractable pencil structure polyaniline/Graphene composite nano fiber, described composite nano-fiber material device light emitting layer thickness is 100nm～75 μ m, the excitation voltage adopting is 30mV～50V, room temperature condition, emission wavelength is adjustable, wave-length coverage is 340～450nm, and luminous efficiency is 5.5～25.0lm/W.
the application of above-mentioned lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material aspect luminescence generated by light, electroluminescent device.
beneficial effect:
1. the present invention utilizes that chemical method is synthetic has substituent three arylamine monomers containing phenoxy group of aryl oxide, utilizes this monomer synthetic poly-[2,7-(9,9-dioctyl fluorene)-alternately-N-phenyl-N-(4-Phenoxyphenyl) aniline].By high-voltage electrostatic spinning technology, prepared a kind of lead for retractable pencil structure poly-[2,7-(9,9-dioctyl fluorene)-alternately-N-phenyl-N-(4-Phenoxyphenyl) aniline]/graphene nano fiber electroluminescent material, the thickness of composite nano-fiber membrane is that 100nm～75 μ m is adjustable, the average diameter of fiber is 100～600nm, and the length of fiber is 15 μ m～15cm; Introducing by Graphene has improved the sub-transmission performance of polyaniline current-carrying, and then improves material thermal resistance and can and electroluminescent stability, improve three arylamine polymer interchains gatherings.
the present invention is synthetic has the substituent triphenylamine polymer of aryl oxide.This is based on what time following: 1. the N atom on triphenylamine demonstrates electropositivity when forming radical cation (hole), and the oxygen of aryl oxide has to electronics, therefore can improve the stability of N radical cation, and then improve electroluminescent stability.2. aryl oxide has heat resistance, can further improve the heat resistance of aniline polymer material and stop interchain to be assembled.3. Graphene has good charge transport properties, can further improve the charge transport properties of material.
accompanying drawing explanation:
accompanying drawing 1 is the chemical structural drawing of poly-in the present invention [2,7-(9,9-dioctyl fluorene)-alternately-N-phenyl-N-(4-Phenoxyphenyl) aniline].
accompanying drawing 2 is structural representations of lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material in the present invention.
accompanying drawing 3 is the structural representations that contain the electroluminescent device of the substituent lead for retractable pencil structure polyaniline/Graphene of aryl oxide composite nano-fiber material composition in the present invention.
accompanying drawing 4 is the infrared spectrograms of polyaniline P in the present invention.
accompanying drawing 5 is the proton nmr spectra 1H-NMR of polyaniline P in the present invention, wherein, and solvent: deuterochloroform (CDCl3).
accompanying drawing 6 is the carbon-13 nmr spectra 13C-NMR of polyaniline P in the present invention.
the specific embodiment:
embodiment 1:
a kind of method for making of lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material, the solubility Graphene obtaining of take is sandwich layer, polyaniline is shell, by bushing type device, utilize high-voltage electrostatic spinning technology to prepare lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material, and this lead for retractable pencil structure nano fibrous material is made to luminescence generated by light, electroluminescent device.
embodiment 2:
according to the preparation method of the lead for retractable pencil structure polyaniline/Graphene composite nano fiber described in embodiment 1, the first step: described polyaniline is dissolved in solvent, utilizing high-voltage electrostatic spinning technology to prepare polyaniline/Graphene composite nano-fiber material is by poly-[2,7-(9,9-dioctyl fluorene)-alternately-N-phenyl-N-(4-Phenoxyphenyl) aniline] be dissolved in toluene (or oxolane) solvent, content is 1.0～12.0% (wt.%); Second step: the concentration of ethanol (or water) solution of described solubility Graphene is 0.5～6.0% (wt.%), by bushing type syringe needle, the flow velocity ratio of utilizing micro-injection pump to control two kinds of solution is 1:0.2～1:3.0(polyaniline: Graphene), wherein, polyaniline solutions is as shell, and graphene solution is as core (or core) layer; The 3rd step: under 18～30 ℃ of conditions, utilize high-voltage electrostatic spinning technology, adjusting spinning voltage is 10～30kV, and the distance between emission electrode and collecting electrode is 8～23cm.As shown in Figure 2, can on collecting electrode, obtain lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material, the average diameter of composite nano-fiber material is 100～600nm; Fibre length is 15 μ m～15cm.
embodiment 3:
according to the preparation method of the lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material described in embodiment 1 or 2, described polyaniline is the polyaniline containing phenoxy group fluorine-triphenylamine structure, its structural representation is shown in Fig. 1, its preparation method is that the triphenylamine monomer (Mon) containing phenoxy group purify the obtaining one-step polymerization of going forward side by side is obtained to poly-[2,7-(9,9-dioctyl fluorene)-alternately-N-phenyl-N-(4-Phenoxyphenyl) aniline]; Concrete steps are: take refined toluene as solvent (1mmol triphenylamine monomer adds toluene 10～25mL), adopt 9,9-dioctyl fluorene-2,7-hypoboric acid, along (1,3-PD) ester with containing the triphenylamine of phenoxy group, is that 1:1.0～1:1.05 adds according to mol ratio; Adding part by weight is the palladium catalyst Pd (PPh of 1:25～1:30
3
)
4
, described palladium catalyst Pd (PPh
3
)
4
with 9,9-dioctyl fluorene-2,7-hypoboric acid is along (1; ammediol) ratio of ester is 1:25～1:30; add the sodium carbonate liquor with the isopyknic 2.5～3.0M of toluene, under high-purity argon gas or nitrogen protection, the polyaniline by the preparation of Suzuki coupling reaction containing phenoxy group fluorine-triphenylamine structure.
embodiment 4:
according to the preparation method of the lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material described in embodiment 1 or 2 or 3, (1) preparation process of graphene oxide comprises: take crystalline flake graphite, the concentrated sulfuric acid and phosphoric acid, join in reaction vessel, then reaction vessel being placed in to cryosel bathes, cryosel bath temperature is 2～4 ℃, stir 15～20min, then take rate of addition as 0.5～1.0g/min, in reaction vessel, add potassium permanganate, stir 2.0～2.5h, reaction vessel is shifted out to cryosel bathes, being heated to temperature is 35～40 ℃, constant temperature stirs 23～24h, in reaction vessel, add deionized water, after stirring, add hydrogen peroxide, under room temperature condition, stir 12～15min, obtain graphite oxide, (2) preparation process of Graphene comprises: utilize above-mentioned graphene oxide modulation to obtain the graphite oxide aqueous solution that concentration is about 8mgmL-1, get this graphite oxide aqueous solution of 26mL and join in three-necked bottle, be heated to 80～85 ℃, add the TGA of 1mL to carry out redox under stirring condition, the time is 2.0～3.0h, obtains the aqueous solution of Graphene (T-RGO), 200 μ L ammoniacal liquor are added dropwise in above-mentioned graphene aqueous solution, and ultrasonic 10～15min adds 0.4g hydroxylamine hydrochloride under 80 ℃ of stirring conditions, and reaction 2.0h, obtains Graphene, cleans standby.
embodiment 5:
according to the preparation method of the lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material described in embodiment 1 or 2 or 3 or 4, the ratio of the volume of the described concentrated sulfuric acid and the quality of crystalline flake graphite is 4mL:1g～6mL:1g, the described concentrated sulfuric acid and the volume ratio of phosphoric acid are 8:1～10:1, described potassium permanganate and the mass ratio of crystalline flake graphite are 7:1～8:1, described deionized water and the volume ratio of the concentrated sulfuric acid are 4:1～6:1, the described concentrated sulfuric acid and the volume ratio of hydrogen peroxide are 1:1～3:1, described hydrogen peroxide mass concentration is 25～35%, described mixing speed is 200～300rpm, described heating-up temperature is 80～85 ℃.
embodiment 6:
according to the preparation method of the lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material described in embodiment 1 or 2 or 3 or 4 or 5, as shown in Figure 1, the described chemical formula containing phenoxy group polyaniline polymer is poly-[2,7-(9,9-dioctyl fluorene)-alternately-N-phenyl-N-(4-Phenoxyphenyl) aniline], polymer number-average molecular weight is 13,302～31,235.
embodiment 7:
according to the preparation method of the lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material described in embodiment 1-6, the diameter of described lead for retractable pencil structure polyaniline/Graphene composite nano fiber is 100～600nm, wherein gather [2,7-(9,9-dioctyl fluorene)-alternately-N-phenyl-N-(4-Phenoxyphenyl) aniline] as the shell of composite nano-fiber material, thickness is 20～100nm; Graphene is as core (or core) layer of lead for retractable pencil structure composite nano-fiber material, and diameter is 60～400nm; The thickness of described lead for retractable pencil structure poly-[2,7-(9,9-dioctyl fluorene)-alternately-N-phenyl-N-(4-Phenoxyphenyl) aniline]/Graphene composite nano-fiber material film is 100nm～75 μ m.
embodiment 8
according to the preparation method of the lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material described in embodiment 1-7, as shown in Figure 3, described composite nano-fiber material device light emitting layer thickness is 100nm～75 μ m, the excitation voltage adopting is 30mV～50V, room temperature condition, emission wavelength is adjustable, and wave-length coverage is 340～450nm, and luminous efficiency is 5.5～25.0lm/W.
embodiment 9:
according to the manufacture method of the lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material described in embodiment 1-8, containing the synthetic of three arylamine structure polyanilines, be by 9 of purifying, 9-dioctyl fluorene-2, 7-hypoboric acid is along (1, ammediol) ester and triphenylamine monomer, the ratio that is 1:1.0～1:1.05 according to mol ratio, adding weight ratio is the palladium catalyst Pd (PPh3) 4 of 1:20～1:25, add again the sodium carbonate liquor with the isopyknic 2.5～3.0M of solvent (toluene), under high-purity argon gas or nitrogen protection, by Suzuki coupling reaction, obtain containing the substituent polyaniline of aryl oxide, infrared spectrum Fig. 4 of polyaniline, nuclear magnetic resonance spectrum figure is shown in Fig. 5, 6.
embodiment 10:
according to the manufacture method of the lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material one of embodiment 1-9 Suo Shu, the molecular weight characterization analysis containing the substituent polyaniline of aryl oxide, characterizes aniline polymer with gel permeation chromatography (GPC).Take oxolane as mobile phase, with the standard specimen of polystyrene, demarcate.The number-average molecular weight Mn=13 of the aniline polymer recording with gel permeation chromatography, 302～31,235, profile exponent (D) is between 1.9523～2.3255.
embodiment 11:
manufacture method according to the lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material one of embodiment 1-10 Suo Shu, can be used as blue-light device material and is widely used; Also other luminescent material can be entrained in to the luminescent device that obtains other color in this electroluminescent material.Aspect luminescence generated by light, electroluminescent device, can be widely used.
Claims (8)
1. the method for making of lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material, it is characterized in that: the solubility Graphene obtaining of take is sandwich layer, polyaniline is shell, by bushing type device, utilize high-voltage electrostatic spinning technology to prepare a kind of lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material, and this composite nano-fiber material is made to luminescence generated by light, electroluminescent device.
2. the method for making of lead for retractable pencil structure polyaniline/Graphene composite nano fiber according to claim 1, it is characterized in that: the first step: described polyaniline is dissolved in solvent, to gather [2,7-(9,9-dioctyl fluorene)-alternately-N-phenyl-N-(4-Phenoxyphenyl) aniline] be dissolved in toluene or tetrahydrofuran solvent, content is 1.0～12.0% (wt.%); Second step: the described ethanol of solubility Graphene or the concentration of the aqueous solution are 0.5～6.0% (wt.%), by bushing type syringe needle, the flow velocity ratio of utilizing micro-injection pump to control two kinds of solution is 1:0.2～1:3.0, polyaniline: Graphene, wherein, polyaniline solutions is as shell, and graphene solution is as core or sandwich layer; The 3rd step: under 18～30 ℃ of conditions, utilize high-voltage electrostatic spinning technology, adjusting spinning voltage is 10～30kV, and the distance between emission electrode and collecting electrode is 8～23cm, can on collecting electrode, obtain lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material.
3. the method for making of lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material according to claim 1 and 2, it is characterized in that: described polyaniline is the polyaniline containing phenoxy group fluorine-triphenylamine structure, its preparation method is that the triphenylamine monomer (Mon) containing phenoxy group that purify the to obtain one-step polymerization of going forward side by side obtains poly-[2,7-(9,9-dioctyl fluorene)-alternately-N-phenyl-N-(4-Phenoxyphenyl) aniline]; Concrete steps are: take refined toluene as solvent, 1mmol triphenylamine monomer adds the ratio of toluene 10～25mL, adopt 9,9-dioctyl fluorene-2,7-hypoboric acid, along (1,3-PD) ester with containing the triphenylamine of phenoxy group, is that 1:1.0～1:1.05 adds according to mol ratio; Adding part by weight is the palladium catalyst Pd (PPh of 1:25～1:30
3)
4, described palladium catalyst Pd (PPh
3)
4with 9,9-dioctyl fluorene-2,7-hypoboric acid is along (1; ammediol) ratio of ester is 1:25～1:30; add the sodium carbonate liquor with the isopyknic 2.5～3.0M of toluene, under high-purity argon gas or nitrogen protection, the polyaniline by the preparation of Suzuki coupling reaction containing phenoxy group fluorine-triphenylamine structure.
4. according to the preparation method of the lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material described in claim 1 or 2 or 3, it is characterized in that: the preparation process of described solubility Graphene: take the reagent such as crystalline flake graphite, the concentrated sulfuric acid, phosphoric acid, potassium permanganate and hydrogen peroxide and prepare graphene oxide; Utilize above-mentioned graphene oxide modulation to obtain the graphite oxide aqueous solution that concentration is 8mgmL-1; Get this graphite oxide aqueous solution of 26mL and join in three-necked bottle, under heating, stirring condition, add the TGA of 1mL to carry out redox, the time is 2～3h, obtains the aqueous solution of Graphene (T-RGO); 200 μ L ammoniacal liquor are added dropwise in above-mentioned graphene aqueous solution, more than ultrasonic 10min, under heating, stirring condition, add 0.4g hydroxylamine hydrochloride, reaction 2h, obtains Graphene, cleans standby; The ratio of the volume of the described concentrated sulfuric acid and the quality of crystalline flake graphite is 4mL:1g～6mL:1g, the described concentrated sulfuric acid and the volume ratio of phosphoric acid are 8:1～10:1, described potassium permanganate and the mass ratio of crystalline flake graphite are 7:1～8:1, described deionized water and the volume ratio of the concentrated sulfuric acid are 4:1～6:1, the described concentrated sulfuric acid and the volume ratio of hydrogen peroxide are 1:1～3:1, described hydrogen peroxide mass concentration is 25～35%, and described mixing speed is 200～300rpm; Described heating-up temperature is 80～85 ℃.
5. according to the preparation method of the lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material described in claim 1 or 2 or 3 or 4, it is characterized in that: the described chemical formula containing phenoxy group polyaniline polymer is poly-[2,7-(9,9-dioctyl fluorene)-alternately-N-phenyl-N-(4-Phenoxyphenyl) aniline], polymer number-average molecular weight is 13,302～31,235.
6. device prepared by lead for retractable pencil structure polyaniline/Graphene composite nano fiber that prepared by the preparation method of a claim 1 or one of 2 or 3 or 4 or 5 described lead for retractable pencil structure polyaniline/Graphene composite nano-fiber materials, it is characterized in that: lead for retractable pencil structure polyaniline/Graphene composite nano fiber diameter is 100～600nm, wherein gather [2,7-(9,9-dioctyl fluorene)-alternately-N-phenyl-N-(4-Phenoxyphenyl) aniline] as the shell of composite nano-fiber material, thickness is 20～100nm; Graphene is as core or the stratum nucleare of lead for retractable pencil structure composite nano-fiber material, and diameter is 60～400nm; The thickness of described lead for retractable pencil structure poly-[2,7-(9,9-dioctyl fluorene)-alternately-N-phenyl-N-(4-Phenoxyphenyl) aniline]/Graphene composite nano-fiber material film is 100nm～75 μ m, and fibre length is 15 μ m～15cm.
7. the device that prepared by lead for retractable pencil structure polyaniline/Graphene composite nano fiber according to claim 6, it is characterized in that: described composite nano-fiber material device light emitting layer thickness is 100nm～75 μ m, the excitation voltage adopting is 30mV～50V, room temperature condition, emission wavelength is adjustable, wave-length coverage is 340～450nm, and luminous efficiency is 5.5～25.0lm/W.
8. the application of lead for retractable pencil structure polyaniline/Graphene composite nano-fiber material of a claim 6 or 7 preparations aspect luminescence generated by light, electroluminescent device.
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| CN106876610A (en) * | 2016-12-22 | 2017-06-20 | 成都新柯力化工科技有限公司 | A kind of indeno compound of fluorene class Graphene oled light electricity display material and preparation method |
| KR102127621B1 (en) * | 2019-02-25 | 2020-06-29 | 강원대학교산학협력단 | Electrospinning Nozzle Inducing Three Dimensional Co-axial And Core-Shell Structured Nano-Fiber Using It |
| WO2022194125A1 (en) * | 2021-03-16 | 2022-09-22 | 南通纺织丝绸产业技术研究院 | Composite electrochromic material, and preparation method therefor and application thereof |
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| KR102127621B1 (en) * | 2019-02-25 | 2020-06-29 | 강원대학교산학협력단 | Electrospinning Nozzle Inducing Three Dimensional Co-axial And Core-Shell Structured Nano-Fiber Using It |
| WO2022194125A1 (en) * | 2021-03-16 | 2022-09-22 | 南通纺织丝绸产业技术研究院 | Composite electrochromic material, and preparation method therefor and application thereof |
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