CN117822162A - Electroluminescent and thermochromic color-adjustable luminescent fiber and preparation method thereof - Google Patents
Electroluminescent and thermochromic color-adjustable luminescent fiber and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of intelligent electronic fibers, in particular to an electroluminescent and thermochromic color-adjustable luminescent fiber and a preparation method thereof, wherein the luminescent fiber comprises at least two conductive layers, a luminescent color-changing layer and an insulating packaging layer, the luminescent color-changing layer is a layer of material with both luminescent function and thermochromic function, or the luminescent color-changing layer comprises an electroluminescent active layer and a thermochromic active layer; the luminescent color-changing layer is adjacent to the conductive layer, and the insulating packaging layer is positioned on the outermost layer of the luminescent fiber. The electroluminescent mode and the thermochromic mode in the luminescent fiber can work independently or simultaneously, can realize relatively stable control of the luminescent effect, can regulate and control the color of the color-changing fiber in real time, and provides a solution for future intelligent color-changing luminescent fiber materials.
Description
Technical Field
The invention relates to an electroluminescent and thermochromic color-adjustable luminous fiber and a preparation method thereof, belonging to the technical field of intelligent electronic fibers.
Background
Intelligent wearable electronic devices are attracting attention for their portability, flexibility, portability, low power consumption, and the like. By combining various functional materials physical or chemical strategies, wearable electronic products can possess various basic functions such as lighting, heating, power generation, and sensing. Conventional planar and thin film wearable electronics exhibit excellent and stable optoelectronic performance, but trade off air permeability and comfort for a better use experience. In contrast, the emerging wearable electronic device based on the functional fiber effectively combines the technical advantages of the wearable performance, the expandability, the miniaturization, the high adaptability, the multifunction and the like, and has more development potential.
Among them, the light-emitting fiber electronic device has many applications in portable lighting, displays, warning signs, warning clothing and fashion apparel (such as traffic safety vests and entertainment apparel). Furthermore, through reasonable composition material selection and device structural design, light emitting fiber electronic devices have exhibited unique advantages of high strength and highlighting, good stretchability, excellent abrasion resistance, and excellent water resistance, but they generally emit monochromatic light. In order to widen the luminous color of the device, on one hand, luminous powder with different characteristics can be simply and physically blended, and different mixing ratios can be regulated and controlled to obtain the luminous device with mixed colors, or a light conversion layer such as red fluorescent dye is introduced, and the content of the luminous powder is regulated to realize the luminous of different colors. However, the color change achieved by these methods is essentially a non-real-time and static process, and it is difficult to implement a dynamic change of adjusting and controlling multiple light emission colors of a single light emitting device in real time. Research into multicolor and even color-changing luminescent fiber devices is still in the early stage. The search for fiber dynamic electroluminescent devices with multi-color displays is an important basis for future intelligent and wearable textiles.
Therefore, an electroluminescent fiber capable of realizing dynamic color change is needed, the preparation process is simple, mass production is realized, and the characteristics of controllable wire diameter, controllable structure and the like are needed in the fiber preparation process, so that the market demand for the electroluminescent fiber can be met.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides the electroluminescent and thermochromic color-adjustable luminescent fiber and the preparation method thereof, wherein an electroluminescent mode and a thermochromic mode in the luminescent fiber can work independently or simultaneously, can realize relatively stable control of a luminescent effect, can regulate and control the color of the color-changing fiber in real time, and provides a solution for future intelligent color-changing luminescent fiber materials.
The technical scheme for solving the technical problems is as follows: an electroluminescent and thermochromic color-adjustable luminescent fiber, wherein the luminescent fiber comprises at least two conductive layers, a luminescent color-changing layer and an insulating packaging layer, the luminescent color-changing layer is a layer of material with both luminescent function and thermochromic function, or the luminescent color-changing layer comprises an electroluminescent active layer and a thermochromic active layer;
the luminescent color-changing layer is adjacent to the conductive layer, and the insulating packaging layer is positioned on the outermost layer of the luminescent fiber.
Further, the conductive layer comprises a core fiber electrode and an outer electrode conductive layer, wherein the core fiber electrode is the innermost layer of the luminescent fiber.
Further, the luminous fiber sequentially comprises a core fiber electrode, an electroluminescent active layer, a thermochromic active layer, an outer electrode conductive layer and an insulating packaging layer from inside to outside;
or the luminous fiber sequentially comprises a core fiber electrode, an electroluminescent active layer, an outer electrode conductive layer, a thermochromic active layer and an insulating packaging layer from inside to outside;
or the luminous fiber comprises a core fiber electrode, a luminous color-changing layer, an outer electrode conductive layer and an insulating packaging layer from inside to outside.
Further, the core fiber electrode is any one or more of metal conductive fibers, metal composite fibers and carbon material fibers; the diameter of the core fiber electrode is 100-300 mu m, and the conductivity is 10 -2 -10 2 S/cm；
The external electrode conductive layer is any one or more of silver nanowires, adhesive containing metal particles, metal wires, chemical fibers containing metal particles and carbon nanofibers.
The invention also discloses a preparation method of the electroluminescent and thermochromic color-adjustable luminescent fiber, which comprises the following steps:
s1, preparing electroluminescent slurry, thermochromic slurry and mixed luminescent slurry: uniformly mixing an electroluminescent material, a solvent, a polymer binder and a dispersing agent to obtain electroluminescent slurry; uniformly mixing a thermochromic material, a solvent, a polymer binder and a dispersing agent to obtain thermochromic slurry; uniformly mixing an electroluminescent material, a thermochromic material, a solvent, a polymer binder and a dispersing agent to obtain electroluminescent slurry;
s2, constructing a luminescent color-changing layer and an outer electrode conductive layer: coating the mixed luminous slurry on the outer surface of the core layer fiber electrode, drying to obtain a luminous color-changing layer, and loading the outer electrode conductive layer material on the outer surface of the luminous color-changing layer;
or sequentially coating the electroluminescent slurry and the thermochromic slurry on the outer surface of the core layer fiber electrode, drying to obtain a luminescent color-changing layer, and loading the outer electrode conductive layer material on the outer surface of the luminescent color-changing layer;
or coating the electroluminescent slurry on the outer surface of the core fiber electrode, drying to obtain an electroluminescent active layer, loading the outer electrode conductive layer material on the outer surface of the thermochromic active layer to form an outer electrode conductive layer, coating the thermochromic slurry on the outer surface of the outer electrode conductive layer, and drying to obtain the thermochromic active layer;
s3, constructing an insulating packaging layer: insulating transparent polymer is used for insulating encapsulation, and the electroluminescent and thermochromic color-adjustable luminescent fiber is obtained after drying and winding.
Further, the electroluminescent material is SiO 2 Base phosphor, metal sulfide phosphor, gaN or Zn 2 SiO 4 One or more of the following; the particle size of the electroluminescent material is 5-40 mu m, and the mass content of the electroluminescent material in the electroluminescent slurry is 10-80wt%;
the thermochromic material is a thermochromic material with a microcapsule structure, and the mass content of the thermochromic material in the thermochromic slurry is 10-30wt%;
the mass content of the electroluminescent material in the luminescent mixed slurry is 20-70wt%, and the mass content of the thermochromic material in the luminescent mixed slurry is 10-30wt%.
Further, the polymer binder is any one or more of polyvinyl alcohol, polyurethane, vinyl acetate, acrylic acid, epoxy resin binders, phenolic resin binders and organic silicon resin binders; the mass content of the polymer binder in the electroluminescent slurry, the thermochromic slurry or the luminescent mixed slurry is 1-50wt%;
the dispersing agent is any one or more of aqueous siloxane, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, tween 80 and hexadecyl trimethyl ammonium chloride, and the mass content of the dispersing agent in electroluminescent slurry, thermochromic slurry or luminescent mixed slurry is 0.5-1wt%;
the solvent is any one or more of water, ethanol, acetone or N-methyl pyrrolidone.
Further, the insulating transparent polymer is any one or more of epoxy resin, acrylic resin, polyurethane resin, polytetrafluoroethylene resin, polyvinylidene fluoride resin and organic silicon resin.
Further, the thickness of the electroluminescent active layer is 20-150 μm;
the thickness of the thermochromic active layer is 10-50 mu m;
the thickness of the outer electrode conductive layer is 5-50 mu m;
the thickness of the insulating packaging layer is 10-80 mu m.
Further, the drying temperature is 60-180 ℃ and the drying time is 5-15s.
The beneficial effects of the invention are as follows:
the thermochromic material added in the luminescent fiber can realize color conversion by responding to the change of the ambient temperature, has the excellent characteristic of wide spectrum adjustment range, and can realize the reversible adjustment and control of the optical performance and color change of the luminescent fiber in a direct and indirect mode.
The electroluminescent mode and the thermochromic mode in the luminescent fiber can work independently or simultaneously. When the two modes work simultaneously, the color of the electroluminescent active layer can achieve the harmonious luminous effect with the changing color of the thermochromic active layer, and the color real-time variable and multicolor display can be achieved on a single luminous fiber by controlling the direct current power supply voltage in the thermochromic mode, so that a solution is provided for the future intelligent color-changing luminous fiber material.
Compared with the prior art, the luminescent fiber has the advantages of simple structure, simple preparation method, mass production, controllable wire diameter and capability of realizing real-time color mixing. The luminous fiber has good luminous effect, the electroluminescent active layer and the thermochromic active layer are combined, the colors of the two luminous layers are mutually blended, the relatively stable luminous effect can be controlled, and meanwhile, the color change of the luminous fiber can be regulated and controlled in real time, so that the demand of the market on the luminous fiber capable of changing color in real time is effectively met.
Drawings
FIG. 1 is a schematic diagram of the operation of a luminescent fiber;
FIG. 2 is a schematic cross-sectional view of a luminescent fiber of example 1;
FIG. 3 is a schematic cross-sectional view of a luminescent fiber of example 2;
FIG. 4 is a schematic cross-sectional view of a luminescent fiber of example 3;
in the figure, 1, a core fiber electrode; 2. a luminescent color-changing layer; 3. an external electrode conductive layer; 4. an insulating encapsulation layer; 5. an electroluminescent active layer; 6. thermochromic active layer.
Detailed Description
The following describes the present invention in detail. The present invention may be embodied in many other forms than described herein and similarly modified by those skilled in the art without departing from the spirit of the invention, so that the invention is not limited to the specific embodiments disclosed.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
An electroluminescent and thermochromic color-adjustable luminescent fiber, wherein the luminescent fiber comprises at least two conductive layers, a luminescent color-changing layer and an insulating packaging layer, the luminescent color-changing layer is a layer of material with both luminescent function and thermochromic function, or the luminescent color-changing layer comprises an electroluminescent active layer and a thermochromic active layer;
the luminescent color-changing layer is adjacent to the conductive layer, and the insulating packaging layer is positioned on the outermost layer of the luminescent fiber.
Specifically, the conductive layer comprises a core fiber electrode and an outer electrode conductive layer, wherein the core fiber electrode is the innermost layer of the luminescent fiber.
Specifically, the luminous fiber sequentially comprises a core fiber electrode, an electroluminescent active layer, a thermochromic active layer, an outer electrode conductive layer and an insulating packaging layer from inside to outside;
or the luminous fiber sequentially comprises a core fiber electrode, an electroluminescent active layer, an outer electrode conductive layer, a thermochromic active layer and an insulating packaging layer from inside to outside;
or the luminous fiber comprises a core fiber electrode, a luminous color-changing layer, an outer electrode conductive layer and an insulating packaging layer from inside to outside.
Specifically, the core fiber electrode is any one or more of metal conductive fibers, metal composite fibers and carbon material fibers; the diameter of the core fiber electrode is 100-300 mu m, and the conductivity is 10 -2 -10 2 S/cm。
Preferably, the conductivity of the core fiber electrode is 10-10 2 S/cm。
The external electrode conductive layer is any one or more of silver nanowires, adhesive containing metal particles, metal wires, chemical fibers containing metal particles and carbon nanofibers.
When the silver nanowire or the adhesive containing metal particles forms a conductive layer, the thickness of the conductive layer is 5-20 mu m;
the diameter of the metal wire is 20-50 mu m; the diameter of the chemical fiber containing metal particles is 20-50 mu m, and the diameter of the carbon nanofiber is 20-50 mu m; wherein the chemical fiber containing metal particles is any one of copper plated yarn, tin plated yarn and stainless steel yarn.
A preparation method of electroluminescent and thermochromic color-adjustable luminescent fiber comprises the following steps:
s1, preparing electroluminescent slurry, thermochromic slurry and mixed luminescent slurry: uniformly mixing an electroluminescent material, a solvent, a polymer binder and a dispersing agent to obtain electroluminescent slurry; uniformly mixing a thermochromic material, a solvent, a polymer binder and a dispersing agent to obtain thermochromic slurry; uniformly mixing an electroluminescent material, a thermochromic material, a solvent, a polymer binder and a dispersing agent to obtain electroluminescent slurry;
s2, constructing a luminescent color-changing layer and an outer electrode conductive layer: coating the mixed luminous slurry on the outer surface of the core layer fiber electrode, drying to obtain a luminous color-changing layer, and loading the outer electrode conductive layer material on the outer surface of the luminous color-changing layer;
or sequentially coating the electroluminescent slurry and the thermochromic slurry on the outer surface of the core layer fiber electrode, drying to obtain a luminescent color-changing layer, and loading the outer electrode conductive layer material on the outer surface of the luminescent color-changing layer;
or coating the electroluminescent slurry on the outer surface of the core fiber electrode, drying to obtain an electroluminescent active layer, loading the outer electrode conductive layer material on the outer surface of the thermochromic active layer to form an outer electrode conductive layer, coating the thermochromic slurry on the outer surface of the outer electrode conductive layer, and drying to obtain the thermochromic active layer;
s3, constructing an insulating packaging layer: insulating transparent polymer is used for insulating encapsulation, and the electroluminescent and thermochromic color-adjustable luminescent fiber is obtained after drying and winding.
Specifically, the electroluminescent material is SiO 2 Base phosphor, metal sulfide phosphor, gaN or Zn 2 SiO 4 One or more of the following; the particle size of the electroluminescent material is 5-40 mu m, and the mass content of the electroluminescent material in the electroluminescent slurry is 10-80wt%.
Preferably, the mass content of the electroluminescent material in the electroluminescent slurry is 30-50wt%.
Wherein the SiO is 2 The base luminescent powder comprises but is not limited to SiO 2 :Ge、SiO 2 Er; the metal sulfide type luminescent powder comprises, but is not limited to CaS, srS, znS, caGa 2 S 4 、SrGa 2 S 4 (Zn, cd) S: cu luminescent powder.
The thermochromic material is an organic or inorganic thermochromic material capable of reversible color change with temperature change. The thermochromic material may be a single or composite thermochromic material including, but not limited to, different types of thermochromic materials having different response temperatures, and/or different types of thermochromic materials having the same response temperature, but having different response colors at the same time.
The thermochromic material is of a microcapsule structure, and can be better protected from being damaged easily in use. The mass content of the thermochromic material in the thermochromic slurry is 10-30wt%;
the mass content of the electroluminescent material in the luminescent mixed slurry is 20-70wt%, and the mass content of the thermochromic material in the luminescent mixed slurry is 10-30wt%.
More specifically, in the actual production and application process, a functional modifying material may be added to the thermochromic active layer according to the requirement, where the modifying material is one or more of a heat stabilizer, a plasticizer, an antistatic agent, and an anti-ultraviolet agent, but not limited to these.
Specifically, the polymer binder is any one or more of polyvinyl alcohol, polyurethane, vinyl acetate, acrylic acid, epoxy resin binders, phenolic resin binders and organic silicon resin binders; the mass content of the polymer binder in the electroluminescent slurry, the thermochromic slurry or the luminescent mixed slurry is 1-50wt%;
preferably, the mass content of the polymer binder in the electroluminescent paste or the thermochromic paste is 2-10wt%. Wherein the polymeric binder should be chemically compatible with the corresponding solvent.
The dispersing agent is any one or more of aqueous siloxane, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, tween 80 and hexadecyl trimethyl ammonium chloride, and the mass content of the dispersing agent in electroluminescent slurry, thermochromic slurry or luminescent mixed slurry is 0.5-1wt%;
the solvent is any one or more of water, ethanol, acetone or N-methyl pyrrolidone.
Specifically, the insulating transparent polymer is any one or more of epoxy resin, acrylic resin, polyurethane resin, polytetrafluoroethylene resin, polyvinylidene fluoride resin and organic silicon resin.
Specifically, the thickness of the electroluminescent active layer is 20-150 μm; preferably, the electroluminescent active layer has a thickness of 40-100 μm
Specifically, the thickness of the thermochromic active layer is 10-50 mu m; preferably, the thickness of the thermochromic active layer is 10-30 μm.
Still more preferably, the thermochromic active layer has a thickness of (h±5) μm, h=0.3h+5, wherein H is the thickness of the electroluminescent active layer, and H is in μm. The thickness of the electroluminescent active layer and the thickness of the thermochromic active layer are coordinated, so that the luminescent performance and the color-changing performance of the luminescent fiber can be better facilitated.
Specifically, the thickness of the outer electrode conductive layer is 5-50 mu m;
specifically, the thickness of the insulating packaging layer is 10-80 mu m; preferably, the thickness of the insulating packaging layer is 20-50 μm.
Specifically, the drying temperature is 60-180 ℃, the drying time is 5-15s, and the winding speed is 5-20m/min
Preferably, the drying temperature is 100-140 ℃.
The electroluminescent mode and the thermochromic mode in the luminescent fiber can work independently or simultaneously.
Electroluminescent mode: a driving device with a driving alternating voltage of 30-500V and a driving frequency of 50-8000Hz is used for connecting a core fiber electrode at one end of the luminescent fiber and an electrode conducting layer to light the luminescent fiber.
Thermochromic mode: the power supply device with the direct-current voltage of 0-50V is used for connecting the two ends of the electrode conductive layer of the luminescent fiber, the electrode conductive layer has resistance, the Joule heat generated by the luminescent fiber can be controlled by adjusting the direct-current power supply voltage, the temperature of the luminescent fiber is further adjusted in real time, and the color of the thermochromic active layer in the middle is changed through temperature change, so that the color change effect is realized. The specific working principle is shown in figure 1.
Specifically, the reagents used in the examples were all outsourced reagents, and various solvents were purchased from national chemical reagents, inc. The thermochromic material used in the examples is from Shenzhen color-changing technology Co., ltd, and is specifically a thermochromic microcapsule, the particles are spherical, the average diameter is 2-7 μm, the inside of the thermochromic material is a color-changing substance, the outside of the thermochromic material is a transparent shell which is about 0.2-0.5 μm thick and can not be dissolved or melted, and the color-changing substance is protected from being corroded by other chemical substances. In the examples, the various devices are commercially available devices. Room temperature means an ambient temperature of 10 ℃ to 30 ℃.
The thermochromic materials described in the examples are respectively: thermochromic material a: changing from colorless to red at 40 ℃; thermochromic material B: the violet color changes to be colorless at 31 ℃; thermochromic material C: the color changes at multiple temperatures, the color is dark green below 25 ℃, the color changes into orange yellow along with the temperature rise, and the material changes into light pink when the temperature rises to above 31 ℃. Wherein the temperature is the temperature at which the final transition is completed.
And (3) carrying out color test on the luminescent fiber prepared in the embodiment, wherein a pantongvelc color card is used as a color standard.
Example 1
The first step: 50g (Zn, cd) S were added at room temperature 25 ℃): cu luminescent powder (average particle diameter 25 μm, national standard brand D522, shanghai Keyan photoelectric technology Co., ltd.) was added to 30g of ethanol solvent, then 19.5g of polyvinyl alcohol binder (Coleus International trade Shanghai Co., ltd.) and 0.5g of sodium dodecylbenzene sulfonate were added, and magnetically stirred for 30min at a stirring speed of 300rpm, to obtain an electroluminescent paste uniformly dispersed. 20g of thermoluminescent material A is added into 30g of water, then 19.5g of polyvinyl alcohol binder and 0.5g of sodium dodecyl benzene sulfonate are added, and the mixture is magnetically stirred for 30min at the stirring speed of 300rpm, so as to obtain the uniformly dispersed thermochromic paste.
And a second step of: the dip-coating device was turned on, and the prepared electroluminescent paste and thermochromic paste were uniformly coated on the core fiber electrode copper wire nylon core-spun conductive yarn (diameter 210 μm, laiwu Long Zhi metal yarn Co., ltd.) at a speed of 10m/min in sequence. Drying at 120deg.C, and collecting on roller. Wherein the thickness of the electroluminescent active layer is 70 μm, and the thickness of the thermochromic active layer is 25 μm.
And a third step of: the pair twisting device was turned on and a metallic copper wire (diameter 30 μm) was incorporated into the fiber in a wound manner to form an outer electrode conductive layer having a thickness of 30 μm.
Fourth step: the packaging device is started, a water-based epoxy resin aqueous solution (product model F0716, shenzhen Jitian chemical Co., ltd.) with the mass fraction of 50wt% is uniformly coated on the surface of the fiber at the speed of 8m/min, then the fiber is dried on line at 100 ℃, the thickness of the formed insulating packaging layer is 50 mu m, and finally the luminous fiber is collected and wound on a spool. The resulting luminescent fiber is shown in cross-section in FIG. 2.
Stripping one end of the prepared luminescent fiber to form a core fiber electrode and an outer electrode conductive layer, and connecting the core fiber electrode and the outer electrode conductive layer by using a driving device with an alternating voltage of 80V and a driving frequency of 1000 Hz; the other end of the luminous fiber is stripped to form an outer electrode conductive layer, and a power supply with the direct-current voltage adjusting range of 0-10V is used for connecting the two ends of the outer electrode conductive layer. The high-voltage alternating current driving device is turned on, and the color change effect is realized by adjusting the voltage of the direct current power supply.
Example 2
The first step: at room temperature 25 ℃, 50g ZnS: the Cu luminescent powder (average particle diameter 25 μm, national standard brand is D502, shanghai Keyan photoelectric technology Co., ltd.) and 20g of thermochromic material B are added into 60g of water, then 39g of polyvinyl alcohol binder (Coleus International trade Shanghai Co., ltd.) and 1g of sodium dodecyl benzene sulfonate are added, and the mixture is magnetically stirred for 30min at a stirring speed of 300rpm, so that the uniformly dispersed mixed luminescent slurry is obtained.
And a second step of: starting a dip-coating device, uniformly coating the prepared mixed luminous slurry on the surface of a core fiber electrode copper wire nylon core-spun conductive yarn (with the diameter of 210 mu m, laiwu Long Zhi metal yarn Co., ltd.) at the speed of 10m/min, drying at the temperature of 120 ℃, and finally collecting on a roller. Wherein the total thickness of the luminescent color-changing layer is 100 μm.
And a third step of: starting a dip-coating device, uniformly coating ITO dispersion liquid (the quantity is 13 percent, and the Nicotiana nano industry Co., ltd.) on the surface of the core fiber electrode copper wire composite fiber material at the speed of 10m/min, and drying at the temperature of 120 ℃ to form a conductive coating, wherein the thickness of the conductive coating is 10 mu m; the pair twisting device was turned on, and copper wire fibers (diameter 30 μm) were incorporated into the fibers in a wound manner, forming an outer electrode conductive layer having a thickness of 35 μm.
Fourth step: the packaging device is started, 50wt% of aqueous polyurethane emulsion (product model F0410, shenzhen Jitian chemical Co., ltd.) is uniformly coated on the surface of the fiber at the speed of 8m/min, then the fiber is dried on line at 100 ℃, the thickness of the formed insulating packaging layer is 20 mu m, finally the luminous fiber is collected and wound on a spool, and the sectional view of the luminous fiber is shown in figure 3.
Stripping one end of the prepared luminescent fiber to form a core fiber electrode and an outer electrode conductive layer, and connecting the core fiber electrode and the outer electrode conductive layer by using a driving device with an alternating voltage of 80V and a driving frequency of 1000 Hz; the other end of the luminous fiber is stripped to form an outer electrode conductive layer, and a power supply with the direct-current voltage adjusting range of 0-10V is used for connecting the two ends of the outer electrode conductive layer. The high-voltage alternating current driving device is turned on, and the color change effect is realized by adjusting the voltage of the direct current power supply.
Example 3
The first step: at room temperature 25 ℃, 50g ZnS: cu luminescent powder (average particle diameter 25 μm, national standard brand D502, shanghai Keyan photoelectric technology Co., ltd.) is added into 30g of water, then 19.5g of polyurethane binder (Shenzhen Jitian chemical Co., ltd.) and 0.5g of sodium dodecyl benzene sulfonate are added, and the mixture is magnetically stirred for 30min at a stirring speed of 300rpm, so that the electroluminescent slurry which is uniformly dispersed is obtained. 20g of thermoluminescent material C was added to 30g of water, followed by 19.5g of polyurethane binder, 0.5g of sodium dodecylbenzenesulfonate, and magnetically stirred for 30 minutes at a stirring speed of 300rpm, to obtain a uniformly dispersed thermochromic paste.
And a second step of: the dip-coating device is started, the prepared electroluminescent slurry is uniformly coated on the surface of a core fiber electrode copper wire nylon core-spun conductive yarn (diameter 210 mu m, laiwu Long Zhi metal yarn Co., ltd.) at a speed of 10m/min, dried at a temperature of 120 ℃, and finally collected on a roller. Wherein the thickness of the electroluminescent active layer is 40 μm.
And a third step of: the pair twisting device was turned on and then copper wire fibers (30 μm in diameter) were wound into the fibers, which together with the conductive coating formed an outer electrode conductive layer having a thickness of 30 μm.
Fourth step: and then starting a dip-coating device, uniformly coating the prepared thermochromic slurry on the surface of the core layer fiber electrode copper wire composite fiber material (with the diameter of 100 mu m) at the speed of 10m/min, drying at the temperature of 120 ℃, and finally collecting on a roller. Wherein the thickness of the thermochromic active layer is 20 μm.
Fifth step: the packaging device is started, 50wt% of aqueous acrylic resin emulsion (product model E0512, shenzhen Jitian chemical Co., ltd.) is uniformly coated on the surface of the fiber at the speed of 8m/min, then the fiber is dried on line at 100 ℃, the thickness of the formed insulating packaging layer is 40 mu m, finally the luminous fiber is collected and wound on a spool, and the section view of the luminous fiber is shown in figure 4.
Stripping one end of the prepared luminescent fiber to form a core fiber electrode and an outer electrode conductive layer, and connecting the core fiber electrode and the outer electrode conductive layer by using a driving device with an alternating voltage of 80V and a driving frequency of 1000 Hz; the other end of the luminous fiber is stripped to form an outer electrode conductive layer, and a power supply with the direct-current voltage adjusting range of 0-10V is used for connecting the two ends of the outer electrode conductive layer. The high-voltage alternating current driving device is turned on, and the color change effect is realized by adjusting the voltage of the direct current power supply.
Example 4
The first step: 40g of CaGa are added at room temperature of 25 DEG C 2 S 4 Adding the luminescent powder into 60g of water, adding 29.4g of polyacrylate binder (Shenzhen Jitian chemical Co., ltd.), 0.6g of Tween 80, magnetically stirring for 30min at 300rpm to obtain electroluminescent lightAnd (3) sizing. 20g of the thermoluminescent material A was added to 50g of water, followed by 29.5g of polyacrylate binder, 0.5g of Tween 80, and magnetically stirred for 30 minutes at a stirring speed of 300rpm, to obtain a uniformly dispersed thermochromic paste.
And a second step of: starting a dip-coating device, uniformly coating the prepared electroluminescent slurry on the surface of conductive fibers (100 μm model T700 SC-12000-50C) of the core fiber electrode carbon material at the speed of 10m/min, drying at the temperature of 100 ℃, and finally collecting on a roller. Wherein the thickness of the electroluminescent active layer is 20 μm.
And a third step of: the pair twisting device was turned on, and a silver-plated yarn (fineness 75D, shenzhen chemical fiber limited) was incorporated into the fiber in a winding manner to form an outer electrode conductive layer having a thickness of 30 μm.
Fourth step: and then starting a dip-coating device, uniformly coating the prepared thermochromic slurry on the surface of the core fiber electrode at the speed of 10m/min, drying at the temperature of 100 ℃, and finally collecting on a roller. Wherein the thickness of the thermochromic active layer is 10 μm.
Fifth step: the packaging device is started, 50wt% of aqueous fluorocarbon emulsion (product model E0802, shenzhen Jitian chemical Co., ltd.) is uniformly coated on the surface of the fiber at the speed of 8m/min, then the fiber is dried on line at 100 ℃, the thickness of the formed insulating packaging layer is 10 mu m, and finally the luminescent fiber is collected and wound on a spool.
Stripping one end of the prepared luminescent fiber to form a core fiber electrode and an outer electrode conductive layer, and connecting the core fiber electrode and the outer electrode conductive layer by using a driving device with an alternating voltage of 80V and a driving frequency of 1000 Hz; the other end of the luminous fiber is stripped to form an outer electrode conductive layer, and a power supply with the direct-current voltage adjusting range of 0-10V is used for connecting the two ends of the outer electrode conductive layer. The high-voltage alternating current driving device is turned on, and the color change effect is realized by adjusting the voltage of the direct current power supply.
Example 5
The first step: 80g of CaN luminescent powder is added into 17.5g of ethanol at room temperature of 25 ℃, then 20g of vinyl acetate binder (Nanjing chime sea commerce and trade company, inc.) and 0.5g of sodium dodecyl sulfate are added, and the mixture is magnetically stirred for 30min, wherein the stirring speed is 300rpm, so that the electroluminescent slurry which is uniformly dispersed is obtained. 50g of the thermoluminescent material A was added to 47g of ethanol, followed by 25g of a vinyl acetate binder, 0.5g of sodium dodecyl sulfate, and magnetically stirred for 30 minutes at a stirring speed of 300rpm, to obtain a uniformly dispersed thermochromic paste.
And a second step of: the dip-coating device is started, the prepared electroluminescent slurry is uniformly coated on the surface of a core fiber electrode copper wire nylon core-spun conductive yarn (diameter 210 mu m, laiwu Long Zhi metal yarn Co., ltd.) at a speed of 10m/min, dried at a temperature of 60 ℃, and finally collected on a roller. Wherein the thickness of the electroluminescent active layer is 80 μm.
And a third step of: the pair twisting device was turned on, and copper-plated yarn (fineness specification 20D/3F, shanghai plain Cheng Jinyin silk textile limited) was incorporated into the fiber in a winding manner to form an outer electrode conductive layer having a thickness of 25 μm.
Fourth step: and then starting a dip-coating device, uniformly coating the prepared thermochromic slurry on the surface of the core fiber electrode at the speed of 10m/min, drying at the temperature of 100 ℃, and finally collecting on a roller. Wherein the thickness of the thermochromic active layer is 25 μm.
Fifth step: the packaging device is started, 50wt% of aqueous acrylic resin emulsion (product model E0512, shenzhen Jitian chemical Co., ltd.) is uniformly coated on the surface of the fiber at the speed of 8m/min, then the fiber is dried on line at 100 ℃, the thickness of the formed insulating packaging layer is 30 mu m, and finally the luminous fiber is collected and wound on a spool.
Stripping one end of the prepared luminescent fiber to form a core fiber electrode and an outer electrode conductive layer, and connecting the core fiber electrode and the outer electrode conductive layer by using a driving device with an alternating voltage of 80V and a driving frequency of 1000 Hz; the other end of the luminous fiber is stripped to form an outer electrode conductive layer, and a power supply with the direct-current voltage adjusting range of 0-10V is used for connecting the two ends of the outer electrode conductive layer. The high-voltage alternating current driving device is turned on, and the color change effect is realized by adjusting the voltage of the direct current power supply.
Comparative example 1
A luminescent fiber was produced in the same manner as in example 3, except that the thermochromic active layer of this comparative example 1 had a thickness of 50 μm. (the thickness of the thermochromic active layer is increased, and the rule is not satisfied: the thickness of the thermochromic active layer is (H+ -5) μm, and H=0.3h+5).
Comparative example 2
A luminescent fiber was produced in the same manner as in example 3, except that the thickness of the electroluminescent active layer of this comparative example 2 was 100 μm. (the thickness of the thermochromic active layer is increased, and the rule is not satisfied: the thickness of the thermochromic active layer is (H+ -5) μm, and H=0.3h+5).
Comparative example 3
A luminescent fiber was manufactured by the same method as in example 3, except that the fifth step was not performed in this comparative example 3, i.e., the luminescent fiber manufactured in this comparative example 5 did not contain an insulating encapsulation layer.
Comparative example 4
A light emitting fiber was produced in the same manner as in example 1 except that in this comparative example 4, the order of the thermochromic active layer and the electroluminescent active layer was reversed.
The color control results of the luminescent fibers prepared in the above examples and comparative examples are shown in table 1 below.
TABLE 1 color Regulation results
The luminescent fibers prepared in the above examples and comparative examples were subjected to a luminescent brightness test and a wear resistance test.
The method for testing the luminous brightness comprises the following steps: normally lighting the prepared luminous fiber, and detecting by adopting a CM-HYPn-I colorimeter; the wear resistance testing method comprises the following steps: the prepared luminescent fiber is sewn on the surface of leather base cloth, and the wear resistance performance test is carried out according to the GBT21196.2-2007 national standard,
the results of the performance tests are shown in Table 2 below.
TABLE 2
As can be seen from the data in tables 1-2, the luminescent fibers prepared in examples 1-5 have both good electroluminescent properties and good color-changing properties, and have high durability and long service life.
From the comparison of the performance data of comparative examples 1-2 and example 3, it can be seen that: if the thickness relation of the thermochromic active layer and the electroluminescent active layer is not proper, the electroluminescent performance and the color-changing performance of the luminescent fiber are deteriorated, because if the thickness of the thermochromic active layer is too large, the electroluminescent performance is affected, and if the thickness of the thermochromic active layer is too small, the electroluminescent performance is higher, the color-changing performance is not obvious, so that the luminescent fiber cannot have the electroluminescent performance and the color-changing performance at the same time.
From comparison of the performance data of comparative example 3 and example 3, it can be seen that: under the condition that the insulating packaging layer exists, the wear resistance of the luminescent fiber can reach 3000 times of circulation without being destroyed; if the insulating packaging layer is not arranged, the luminescent color-changing layer of the luminescent fiber is damaged after 500 times of test, and the service life of the luminescent fiber is greatly reduced.
From the comparison of the performance data of comparative example 4 and example 1, it can be seen that: if the order of the thermochromic active layer and the electroluminescent active layer is reversed, it is almost difficult to exhibit the color-changing property although the brightness of the luminescent fiber is increased. The luminescent fiber prepared by the method can give consideration to both electroluminescent performance and color-changing performance.
The technical features of the above-described embodiments may be arbitrarily combined, and in order to simplify the description, all possible combinations of the technical features in the above-described embodiments are not exhaustive, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the invention as defined in the appended claims.
Claims (10)
1. The electroluminescent and thermochromic color-adjustable luminescent fiber is characterized by comprising at least two conductive layers, a luminescent color-changing layer and an insulating packaging layer, wherein the luminescent color-changing layer is made of one layer of material with both luminescent function and thermochromic function, or comprises an electroluminescent active layer and a thermochromic active layer;
the luminescent color-changing layer is adjacent to the conductive layer, and the insulating packaging layer is positioned on the outermost layer of the luminescent fiber.
2. An electroluminescent and thermochromic color-tunable luminescent fiber as recited in claim 1, wherein the conductive layer comprises a core fiber electrode and an outer electrode conductive layer, the core fiber electrode being an innermost layer of the luminescent fiber.
3. An electroluminescent and thermochromic color-tunable luminescent fiber according to claim 2, wherein the luminescent fiber comprises a core fiber electrode, an electroluminescent active layer, a thermochromic active layer, an outer electrode conductive layer and an insulating encapsulation layer in this order from inside to outside;
or the luminous fiber sequentially comprises a core fiber electrode, an electroluminescent active layer, an outer electrode conductive layer, a thermochromic active layer and an insulating packaging layer from inside to outside;
or the luminous fiber comprises a core fiber electrode, a luminous color-changing layer, an outer electrode conductive layer and an insulating packaging layer from inside to outside.
4. An electroluminescent and thermochromic color-tunable luminescent fiber according to claim 2 or 3, wherein the core fiber electrode is any one or more of a metal conductive fiber, a metal composite fiber, and a carbon material fiber; the diameter of the core fiber electrode is 100-300 mu m, and the conductivity is 10 -2 -10 2 S/cm；
The external electrode conductive layer is any one or more of silver nanowires, adhesive containing metal particles, metal wires, chemical fibers containing metal particles and carbon nanofibers.
5. A method for preparing an electroluminescent and thermochromic color-tunable luminescent fiber according to any one of claims 1 to 4, wherein the preparation method comprises the following steps:
s1, preparing electroluminescent slurry, thermochromic slurry and mixed luminescent slurry: uniformly mixing an electroluminescent material, a solvent, a polymer binder and a dispersing agent to obtain electroluminescent slurry; uniformly mixing a thermochromic material, a solvent, a polymer binder and a dispersing agent to obtain thermochromic slurry; uniformly mixing an electroluminescent material, a thermochromic material, a solvent, a polymer binder and a dispersing agent to obtain electroluminescent slurry;
s2, constructing a luminescent color-changing layer and an outer electrode conductive layer: coating the mixed luminous slurry on the outer surface of the core layer fiber electrode, drying to obtain a luminous color-changing layer, and loading the outer electrode conductive layer material on the outer surface of the luminous color-changing layer;
or sequentially coating the electroluminescent slurry and the thermochromic slurry on the outer surface of the core layer fiber electrode, drying to obtain a luminescent color-changing layer, and loading the outer electrode conductive layer material on the outer surface of the luminescent color-changing layer;
or coating the electroluminescent slurry on the outer surface of the core fiber electrode, drying to obtain an electroluminescent active layer, loading the outer electrode conductive layer material on the outer surface of the thermochromic active layer to form an outer electrode conductive layer, coating the thermochromic slurry on the outer surface of the outer electrode conductive layer, and drying to obtain the thermochromic active layer;
s3, constructing an insulating packaging layer: insulating transparent polymer is used for insulating encapsulation, and the electroluminescent and thermochromic color-adjustable luminescent fiber is obtained after drying and winding.
6. The method for preparing electroluminescent and thermochromic color-tunable luminescent fiber according to claim 5, wherein the electroluminescent material is SiO 2 Base phosphor, metal sulfide phosphor, gaN or Zn 2 SiO 4 One or more of the following; the particle size of the electroluminescent material is 5-40 mu m, and the mass content of the electroluminescent material in the electroluminescent slurry is 10-80wt%;
the thermochromic material is a thermochromic material with a microcapsule structure, and the mass content of the thermochromic material in the thermochromic slurry is 10-30wt%;
the mass content of the electroluminescent material in the luminescent mixed slurry is 20-70wt%, and the mass content of the thermochromic material in the luminescent mixed slurry is 10-30wt%.
7. The method for preparing electroluminescent and thermochromic color-tunable luminescent fiber according to claim 5, wherein the polymer is any one or more of polyvinyl alcohol, polyurethane, vinyl acetate, acrylic acid, epoxy resin binder, phenolic resin binder and silicone resin binder; the mass content of the polymer in the electroluminescent slurry, the thermochromic slurry or the luminescent mixed slurry is 1-50wt%;
the dispersing agent is any one or more of aqueous siloxane, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, tween 80 and hexadecyl trimethyl ammonium chloride, and the mass content of the dispersing agent in electroluminescent slurry, thermochromic slurry or luminescent mixed slurry is 0.5-1wt%;
the solvent is any one or more of water, ethanol, acetone or N-methyl pyrrolidone.
8. The method for preparing the electroluminescent and thermochromic color-adjustable luminescent fiber according to claim 5, wherein the insulating transparent polymer is any one or more of epoxy resin, acrylate resin, polyurethane resin, polytetrafluoroethylene resin, polyvinylidene fluoride resin and organic silicon resin.
9. The method for preparing electroluminescent and thermochromic color-tunable luminescent fiber according to claim 5, wherein the thickness of the electroluminescent active layer is 20-150 μm;
the thickness of the thermochromic active layer is 10-50 mu m;
the thickness of the outer electrode conductive layer is 5-50 mu m;
the thickness of the insulating packaging layer is 10-80 mu m.
10. The method for preparing electroluminescent and thermochromic color-tunable luminescent fiber according to claim 5, wherein the drying temperature is 60-180 ℃ and the drying time is 5-15s.
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