CN110952311A - Preparation method of large-area flexible electroluminescent nano fiber net - Google Patents

Preparation method of large-area flexible electroluminescent nano fiber net Download PDF

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CN110952311A
CN110952311A CN201911290358.1A CN201911290358A CN110952311A CN 110952311 A CN110952311 A CN 110952311A CN 201911290358 A CN201911290358 A CN 201911290358A CN 110952311 A CN110952311 A CN 110952311A
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film
nano
fiber net
mask plate
layer
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毕胜
李子兴
卜镜元
陈润泽
李钰
孙业青
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Dalian University of Technology
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Dalian University of Technology
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Abstract

The invention belongs to the technical field of nanofiber light-emitting electrodes, and particularly relates to a preparation method of a large-area flexible electroluminescent nanofiber web. According to the invention, by utilizing the advantage of good flexibility of the PVA1788 material, the large-area flexible nano-fiber net is constructed in an electrostatic spinning mode, and then the nano-fiber net is subjected to thermal evaporation of a specific property material to obtain the large-area flexible electroluminescent nano-fiber net, so that the large-area flexible electroluminescent nano-fiber net has the characteristics of large action area, high flexibility, high luminous intensity and long effective life, and has wide application prospect.

Description

Preparation method of large-area flexible electroluminescent nano fiber net
Technical Field
The invention belongs to the technical field of nanofiber light-emitting electrodes, and particularly relates to a preparation method of a large-area flexible electroluminescent nanofiber web.
Background
The flexible light-emitting material has the advantages of light weight, conformity, extensibility and the like, has wide application prospect in the aspect of flexible electronic devices, has obvious advantages compared with the defects of difficult integration, easy damage, large energy consumption and the like of common electronic equipment, and has become a focus of attention in the current academic and industrial fields. Therefore, the preparation method of the flexible nanofiber web with low cost, high stability and good flexibility is developed, and the flexible nanofiber web is applied to the preparation of the flexible electrode, has important application value to optoelectronic devices, and becomes a key core problem for the development of next-generation flexible electronic devices.
Disclosure of Invention
Aiming at the problems of small available area and poor toughness of the existing luminescent device, the invention provides a preparation method of a large-area flexible electroluminescent nano-fiber net. According to the invention, by utilizing the advantage of good flexibility of the PVA1788 material, the large-area flexible nano-fiber net is constructed in an electrostatic spinning mode, and then the nano-fiber net is subjected to thermal evaporation of a specific property material to obtain the large-area flexible electroluminescent nano-fiber net, so that the large-area flexible electroluminescent nano-fiber net has the characteristics of large action area, high flexibility, high luminous intensity and long effective life, and has wide application prospect.
The technical scheme of the invention is as follows:
a preparation method of a large-area flexible electroluminescent nano-fiber net comprises the following steps:
step 1, electrostatic spinning is carried out by using an electrostatic spinning device, and the generated nanofiber web is laid on a round tray to form a round PVA1788 nanofiber web; wherein the direct current voltage is 1 KV-4 KV, the environmental temperature is 20-28 ℃, the environmental humidity is 35% -45%, and the spinning solution adopts PVA1788 solution with the concentration of 12% -15%.
Step 2, placing a strip-shaped mask plate on the upper surface of the PVA1788 nano-fiber net prepared in the step 1, arranging the strip-shaped mask plate along one side of the nano-fiber net, dividing the nano-fiber net into a covering part and an uncovering part, wherein the area of the covering part accounts for 1/7-1/6 of the whole area of the nano-fiber net, and thermally evaporating a layer of metal Ag on the nano-fiber net uncovered by the mask plate by using an evaporation coating instrument, wherein the thermal evaporation parameters are as follows: the operating current is 30-40A, the pressure of a chamber is 6 multiplied by 10 < -4 > Pa-8 multiplied by 10 < -4 > Pa, and the film thickness forming speed is 0.5-0.8 nm/min; and evaporating and plating a layer of Ag film on the nano-fiber net which is not covered by the mask plate.
Step 3, keeping the position of the mask plate unchanged, continuing to perform thermal evaporation, and sequentially performing thermal evaporation on Alq3And (3) sequentially forming Alq on the Ag thin film of the nano-fiber net uncovered by the mask plate by using the NPB material and thermal evaporation parameters in the same step (2)3Film and NPB film.
And 4, removing the mask plate, covering the symmetrical side of the position of the mask plate in the step 2 relative to the circle center by using the mask plate with the same size and shape on the nano-fiber net, and thermally evaporating ITO materials on the part which is not covered by the mask plate, wherein the thermal evaporation parameters are the same as those in the step 2 to form a layer of ITO film, and finally obtaining the large-area flexible electroluminescent nano-fiber net.
The prepared large-area flexible electroluminescent nano-fiber net comprises five layers which are sequentially from bottom to top: the first layer is a PVA1788 nano-fiber net with the thickness of 200-500 nm; the second layer is an Ag film and an ITO film, the thickness of the Ag film and the ITO film is 80-150 nm, the Ag film and the ITO film are arranged in parallel, and the Ag film and the ITO film jointly cover the whole PVA1788A nanofiber web; the third layer is Alq3Film, fourth layer of NPB film, Alq3The thickness of the film and the thickness of the NPB film are both 80-150 nm, and the sizes of the film and the NPB film are the same as those of the Ag film; the fifth layer is an ITO film and is positioned in the center of the whole nanofiber net, and the covered part is the position of the whole PVA1788 nanofiber net except the positions covered by the mask plates on the two sides.
The invention has the beneficial effects that:
1. the flexible electroluminescent nano-fiber net prepared by the invention has the characteristics of good flexibility, high luminous intensity, large luminous area, long effective life and the like, and can be applied to the manufacture of large-area flexible luminous electrodes.
2. The flexible electroluminescent nano-fiber net prepared by the invention has the advantages of controllable film thickness, simple process and easy implementation.
3. Compared with some existing flexible devices, the flexible electroluminescent nano-fiber net prepared by the invention has the advantages of excellent conductivity, optical transmittance and mechanical flexibility, good luminous effect, large luminous area, long effective life and the like, has good repeatability, and has wide application prospect in the development of flexible photoelectric devices.
Drawings
FIG. 1 is an isometric view of a large area flexible electroluminescent nanoweb;
FIG. 2 is a front view of a large area flexible electroluminescent nanoweb;
FIG. 3 is an exploded front view of a large area flexible electroluminescent nanoweb;
fig. 4 is an exploded isometric view of a large area flexible electroluminescent nanoweb.
In the figure: 1 round tray, 2PVA 1788 nanoweb, 3Ag film, 4Alq3Film, 5NPB film, 6ITO film.
Detailed Description
The large-area flexible electroluminescent nano-fiber web prepared by the method of the present invention is shown in fig. 1 and 2, and the explosion view of the large-area flexible electroluminescent nano-fiber web is shown in fig. 3 and 4.
Prepared large areaFlexible electroluminescent nanofiber net forms on circular tray 1, including five layers, from supreme down is in proper order: the first layer is a PVA1788 nano-fiber net 2 with the thickness of 200-500 nm; the second layer is an Ag film 3 and an ITO film 6, the thicknesses of the Ag film 3 and the ITO film 6 are 80-150 nm, and the Ag film and the ITO film are arranged in parallel and cover the whole PVA1788 nano-fiber net 2 together; the third layer is Alq3Film 4, fourth layer NPB film 5, Alq3The thickness of the film 4 and the thickness of the NPB film 5 are both 80-150 nm, and the sizes of the film 4 and the NPB film are the same as those of the Ag film 3; the fifth layer is an ITO film 6 which is positioned in the center of the whole nanofiber net, and the covered part is the position of the whole nanofiber net except two sides covered by the mask plate. Wherein, Ag film 3, Alq3The thicknesses of the thin film 4, the NPB thin film 5, and the ITO thin film 6 may be the same or different.
Example 1:
step 1, regulating the direct current voltage to 1KV, selecting a needle of an electrostatic spinning device with the specification of 0.5mm, feeding the spinning solution at the speed of 5ul/min, in an environment with the temperature of 20 ℃ and the humidity of 35%, adopting a PVA1788 solution with the concentration of 12%, spraying the spinning solution in a strong electric field after melting in a jet orifice, changing liquid drops at the needle from a spherical shape to a conical shape under the action of the electric field, and extending from the conical tip to obtain fiber filaments, so that polymer filaments with the nanometer diameter can be produced, and finally, the polymer filaments are laid on a circular tray with the outer diameter of 300mm and the inner diameter of 250mm to obtain a PVA1788 nanometer fiber net with the thickness of 200 nm.
And 2, preparing a 200nm PVA1788 nano-fiber net based on the step 1, placing a striped mask plate with the length of 320mm and the width of 40mm at one end of the nano-fiber net to cover part of the nano-fiber net (the covering area accounts for 1/7 of the whole area of the nano-fiber net), performing thermal evaporation on the nano-fiber net which is not covered by the mask plate by using an evaporation coating machine to form a layer of metal Ag, wherein the operating current is 30A, the chamber pressure is 6 multiplied by 10 < -4 > PaPa, the film thickness forming speed is 0.5nm/min, finally forming an Ag film with the thickness of 80nm by evaporation, and the part of the nano-fiber net which is covered by the mask plate does not have the Ag film.
Step 3, after a layer of Ag film with the thickness of 80nm is prepared based on the step 2, keeping the position of the mask plate unchangedContinuing to perform thermal evaporation process, and respectively performing thermal evaporation Alq3NPB (hole transport layer material), and Alq is formed on Ag film of nano-fiber net uncovered by mask plate3The film and NPB film (thickness is 80nm), and the part of the nano-fiber net covered by the mask plate has no Alq3Film and NPB film.
Step 4, preparing Alq based on the step 33After the thin film and the NPB thin film are formed, the first mask plate is removed, the opposite end of the position of the first mask plate, which is relative to the circle center, is covered by the mask plates with the same size and shape on the nano-fiber net (the covering area accounts for 1/7 the whole area of the nano-fiber net), the process of thermally evaporating an ITO material is carried out, finally, an ITO thin film with the thickness of 80nm is formed, and finally, the large-area flexible electroluminescence nano-fiber net is obtained
Example 2:
step 1, regulating the direct current voltage to 2.5KV, selecting a needle of an electrostatic spinning device with the specification of 0.6mm, feeding the spinning solution at the flow rate of 8ul/min, spraying and spinning the spinning solution in a strong electric field after the spinning solution is melted in a jet orifice in the environment range of 24 ℃ and 40% humidity, changing the liquid drop at the needle from a spherical shape to a conical shape under the action of the electric field, and extending the liquid drop from the conical tip to obtain a fiber filament, so that a polymer filament with a nano-scale diameter can be produced, and finally, the polymer filament is laid on a circular tray with the outer diameter of 300mm and the inner diameter of 250mm to obtain a PVA1788 nano-fiber net with the thickness of 350 nm.
Step 2, after preparing a 350nm PVA1788 nano-fiber net based on the step 1, placing a striped mask plate with the length of 320mm and the width of 40mm at one end of the nano-fiber net to cover part of the nano-fiber net (the covering area accounts for 13/84 of the whole area of the nano-fiber net), carrying out thermal evaporation on the nano-fiber net which is not covered by the mask plate by using an evaporation coating machine to form a layer of metal Ag, wherein the operating current is 35A, the chamber pressure is 7 multiplied by 10 < -4 > Pa, the film thickness forming speed is 0.7nm/min, finally forming an Ag film with the thickness of 120nm by evaporation, and the part of the nano-fiber net which is covered by the mask plate does not have the Ag film.
Step 3, preparation based on step 2After a layer of Ag film with the thickness of 120nm is formed, the position of the mask plate is kept unchanged, the thermal evaporation process is continued, and Alq is thermally evaporated respectively3NPB (hole transport layer material), and Alq is formed on Ag film of nano-fiber net uncovered by mask plate3The film and NPB film (thickness is 120nm), and the part of the nano-fiber net covered by the mask plate has no Alq3Film and NPB film.
Step 4, preparing Alq based on the step 33And after the film and the NPB film are formed, removing the first mask plate, covering the opposite end of the position of the first mask plate, which is relative to the circle center, on the nano-fiber net by using the mask plates with the same size and shape (the covering area accounts for 13/84 of the whole area of the nano-fiber net), performing a process of thermally evaporating an ITO material, finally forming a layer of ITO film with the thickness of 120nm, and finally obtaining the large-area flexible electroluminescent nano-fiber net.
Example 3:
step 1, adjusting the direct current voltage to 4KV, selecting a 0.6mm needle of an electrostatic spinning device, feeding the flow at the speed of 10ul/min, spraying and spinning the spinning solution in a strong electric field after the spinning solution is melted in a jet orifice in the environment range of 28 ℃ and 45% humidity, changing the liquid drops at the needle from a spherical shape to a conical shape under the action of the electric field, and extending from the conical tip to obtain fiber filaments, so that polymer filaments with nanoscale diameters can be produced, and finally, the polymer filaments are laid on a circular tray with the outer diameter of 300mm and the inner diameter of 250mm to obtain a PVA1788 nano-fiber net with the thickness of 500 nm.
Step 2, after preparing and obtaining a PVA1788 nano-fiber net with the thickness of 500nm based on the step 1, using a striped mask plate with the length of 320mm and the width of 40mm to be arranged at one end of the nano-fiber net to cover part of the nano-fiber net (the covering area accounts for 1/6 of the whole area of the nano-fiber net), carrying out thermal evaporation on a layer of metal Ag on the nano-fiber net which is not covered by the mask plate by using an evaporation coating machine, wherein the operating current is 40A, the chamber pressure is 8 multiplied by 10 < -4 > Pa, the film thickness forming speed is 0.8nm/min, finally forming an Ag film with the thickness of 150nm by evaporation, and the part of the nano-fiber net which is covered by the mask plate is not provided with.
Step 3, after a layer of Ag film with the thickness of 150nm is prepared based on the step 2, keeping the position of the mask plate unchanged, continuing to perform the thermal evaporation process, and respectively performing thermal evaporation on Alq3NPB (hole transport layer material), and Alq is formed on Ag film of nano-fiber net uncovered by mask plate3The film and NPB film (thickness is 150nm), and the part of the nano-fiber net covered by the mask plate has no Alq3Film and NPB film.
Step 4, preparing Alq based on the step 33And after the film and the NPB film are formed, removing the first mask plate, covering the opposite end of the position of the first mask plate, which is relative to the circle center, on the nano-fiber net by using the mask plates with the same size and shape (the covering area accounts for 1/6 of the whole area of the nano-fiber net), performing a process of thermally evaporating an ITO material, finally forming a layer of ITO film with the thickness of 150nm, and finally obtaining the large-area flexible electroluminescent nano-fiber net.

Claims (2)

1. A preparation method of a large-area flexible electroluminescent nano-fiber net is characterized by comprising the following steps:
step 1, electrostatic spinning is carried out by using an electrostatic spinning device, and the generated nanofiber web is laid on a round tray to form a round PVA1788 nanofiber web; wherein the direct current voltage is 1 KV-4 KV, the environmental temperature is 20-28 ℃, the environmental humidity is 35% -45%, and the spinning solution adopts PVA1788 solution with the concentration of 12% -15%;
step 2, placing a strip-shaped mask plate on the upper surface of the PVA1788 nano-fiber net prepared in the step 1, arranging the strip-shaped mask plate along one side of the nano-fiber net, dividing the nano-fiber net into a covering part and an uncovering part, wherein the area of the covering part accounts for 1/7-1/6 of the whole area of the nano-fiber net, and thermally evaporating a layer of metal Ag on the nano-fiber net uncovered by the mask plate by using an evaporation coating instrument, wherein the thermal evaporation parameters are as follows: the operating current is 30-40A, the pressure of a chamber is 6 multiplied by 10 < -4 > Pa-8 multiplied by 10 < -4 > Pa, and the film thickness forming speed is 0.5-0.8 nm/min; evaporating and plating a layer of Ag film on the nano-fiber net which is not covered by the mask plate;
step 3, keeping the mask plateContinuously performing thermal evaporation while keeping the position unchanged, and sequentially performing thermal evaporation on Alq3And (3) sequentially forming Alq on the Ag thin film of the nano-fiber net uncovered by the mask plate by using the NPB material and thermal evaporation parameters in the same step (2)3A film and an NPB film;
and 4, removing the mask plate, covering the symmetrical side of the position of the mask plate in the step 2 relative to the circle center by using the mask plate with the same size and shape on the nano-fiber net, and thermally evaporating ITO materials on the part which is not covered by the mask plate, wherein the thermal evaporation parameters are the same as those in the step 2 to form a layer of ITO film, and finally obtaining the large-area flexible electroluminescent nano-fiber net.
2. The preparation method of the large-area flexible electroluminescent nano-fiber net according to claim 1, wherein the prepared large-area flexible electroluminescent nano-fiber net comprises five layers, which are sequentially from bottom to top: the first layer is a PVA1788 nano-fiber net with the thickness of 200-500 nm; the second layer is an Ag film and an ITO film, the thickness of the Ag film and the thickness of the ITO film are both 80-150 nm, and the Ag film and the ITO film are arranged in parallel and cover the whole PVA1788 nano-fiber net together; the third layer is Alq3Film, fourth layer of NPB film, Alq3The thickness of the film and the thickness of the NPB film are both 80-150 nm, and the sizes of the film and the NPB film are the same as those of the Ag film; the fifth layer is an ITO film and is positioned in the center of the whole nanofiber net, and the covered part is the position of the whole PVA1788 nanofiber net except the positions covered by the mask plates on the two sides.
CN201911290358.1A 2019-12-16 2019-12-16 Preparation method of large-area flexible electroluminescent nano fiber net Pending CN110952311A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111761980A (en) * 2020-06-03 2020-10-13 台州金珏网布有限公司 Gold stamping process of metal wire mesh-like cloth

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101022156A (en) * 2007-03-16 2007-08-22 电子科技大学 Blue organic electroluminescent device and producing method thereof
CN104300082A (en) * 2014-09-02 2015-01-21 电子科技大学 Organic photoelectron integration device with electroluminescence and ultraviolet detection performance and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101022156A (en) * 2007-03-16 2007-08-22 电子科技大学 Blue organic electroluminescent device and producing method thereof
CN104300082A (en) * 2014-09-02 2015-01-21 电子科技大学 Organic photoelectron integration device with electroluminescence and ultraviolet detection performance and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
于军胜等: "柔性有机电致发光器件的制备", 《半导体光电》 *
王娜娜等: "柔性有机电致发光器件导电基板的工艺性能", 《发光学报》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111761980A (en) * 2020-06-03 2020-10-13 台州金珏网布有限公司 Gold stamping process of metal wire mesh-like cloth

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