CN109445220A - A kind of spray coating method preparation large area P3HT base flexible electro-chromic device - Google Patents
A kind of spray coating method preparation large area P3HT base flexible electro-chromic device Download PDFInfo
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- CN109445220A CN109445220A CN201811456371.5A CN201811456371A CN109445220A CN 109445220 A CN109445220 A CN 109445220A CN 201811456371 A CN201811456371 A CN 201811456371A CN 109445220 A CN109445220 A CN 109445220A
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/153—Constructional details
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
- B05D5/06—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain multicolour or other optical effects
- B05D5/065—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain multicolour or other optical effects having colour interferences or colour shifts or opalescent looking, flip-flop, two tones
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
- B05D5/12—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain a coating with specific electrical properties
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/1506—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect caused by electrodeposition, e.g. electrolytic deposition of an inorganic material on or close to an electrode
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/153—Constructional details
- G02F1/155—Electrodes
Abstract
The present invention relates to a kind of methods of spray coating method preparation large area P3HT base flexible electro-chromic device.This method comprises: the good solvent under room temperature using chlorobenzene as P3HT obtains P3HT spray solution, PET-ITO substrate is pre-processed, it preheats again, by P3HT spray solution even application preheating PET-ITO conducting surface, it is dry, it is to electrode with another PET-ITO then using the PET-ITO after drying as working electrode, gel electrolyte is injected, hot pressing is encapsulated.This method is easy to operate, and required equipment is simple, at low cost, is suitble to the preparation of broad area device, and the good solvent using chlorobenzene as P3HT facilitates the dissolution and film forming of P3HT, to improve electrochromic device performance；The large area flexible P3HT electrochromic device being prepared has bistable property, and has preferable flexibility, has good application prospect in fields such as flexible electronics.
Description
Technical field
The invention belongs to electrochromic device preparation field, in particular to a kind of spray coating method preparation large area P3HT base is flexible
Electrochromic device.
Background technique
Electrochromism refers to that material under DC Electric Field, occurs redox reaction and shows and stablize, is reversible
Color change the phenomenon that.Early in 19th-century just it has been proposed that electrochromism concept, but at twentieth century end, Lampert and
After Svesson et al. proposes the idea about electrochromic intelligent window, electrochromism is just rapidly developed.Electrochromic material
It is broadly divided into inorganic electrochromic material and organic electrochromic material two major classes.Organic electrochromic material mainly has oxidation also
Prototype small molecule and conducting polymer.Its major advantage is that the color category of material is more, and molecule designability is high, the response time
It is short.
P3HT (poly- 3- hexyl thiophene) is used as a kind of thiofuran polymer electrochromic material, and synthetic method is simple, hole
Mobility is high, has a good application prospect.But the methods of thiophene-based device preparation method such as spin-coating method, electropolymerization of mainstream
Broad area device, and mostly rigid device cannot be prepared, the demand of diversified device is unable to satisfy.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of spray coating methods to prepare the flexibility electrochromism of large area P3HT base
Device, to overcome the defect that polythiophene class is bad with spray coating method film forming electrochromic device performance in the prior art.
Compared with prior art, polythiophene class is formed a film with spray coating method, and the solvent of selection is largely chloroform, but this kind
Solvent is not at normal temperature that very well, the present invention selects solvent of the chlorobenzene as P3HT to polythiophene class dissolubility, chlorobenzene and
P3HT has better dissolubility, and more P3HT are dissolved under room temperature, and the conformation more stretched is taken in good solvent, can pass through increasing
Add the concentration of P3HT, the drop of spraying contains more P3HT molecules, and P3HT strand is accumulated closer on PET, current-carrying
Son transmits between strand and segment to be more easier, so that the response time, the performances such as light modulation range are more preferably.
Meanwhile the volatilization of solvent will affect the orientation of molecule, the boiling point of chlorobenzene is higher, and P3HT tends to take perpendicular to substrate
To also will increase the surface roughness of film, have with gel electrolyte and more contact, the insertion of ion and abjection are more held
Easily.The final electrochromic property for improving device.
A kind of method of spray coating method preparation large area P3HT base flexible electro-chromic device of the invention, comprising:
(1) PET-ITO conductive substrates are pre-processed；
(2) poly- (3- hexyl thiophene) P3HT is dissolved in chlorobenzene (under room temperature), is stirred, ultrasonic treatment obtains P3HT spraying
Solution, wherein P3HT spray solution concentration is 1~1.5mg/mL；
(3) PET-ITO conductive substrates pretreated in step (1) are preheated, P3HT spray solution in step (2) is equal
The even PET-ITO conductive substrates conducting surface for being sprayed on preheating, dry, wherein the quantity for spray of P3HT is 0.20~1.5mg/cm2；
It (4) is to electrode, injection with another PET-ITO using the PET-ITO after drying in step (3) as working electrode
Gel electrolyte encapsulates hot pressing, obtains P3HT base flexible electro-chromic device.
PET-ITO conductive substrates are pre-processed in the step (1) are as follows: PET-ITO conductive substrates are put into ethyl alcohol
Middle immersion 5-10min is dried with nitrogen conductive be placed in UV ozone instrument up of rear PET-ITO and irradiates 30~60min.
Mixing time is 60~120min in the step (2)；Sonication treatment time is 60~120min, and ultrasonic power is
60~110W.
PET-ITO conductive substrates pretreated in step (1) are preheated in the step (3) are as follows: will be pre- in step (1)
Conductive be placed in thermal station up of treated PET-ITO conductive substrates preheats, and thermal station temperature is 100~120 DEG C, when heating
Between be 10~20min.
Spraying in the step (3) are as follows: spray spray gun using loading P3HT spray solution after ethyl alcohol, acetone cleaning
It applies, wherein spray gun air pump pressure is 0.2~1MPa, and spray gun face PET-ITO base conductive face height is 5~20cm.
Drying temperature is 120~130 DEG C in the step (3), and drying time is 30~60min.
Gel electrolyte component includes: lithium perchlorate 4~10%, polyvinylidene fluoride according to mass fraction in the step (4)
Alkene 15~30%, propene carbonate 40~67% and ionic liquid 0~20%.
In the step (4) working electrode with to the distance between electrode be 0.2~1mm.
Hot pressing temperature is 80~120 DEG C, hot pressing pressure 5MPa in the step (4), and hot pressing time is 2~10min.
The present invention prepares large area P3HT film by spray coating method, P3HT raw material ultrasonic agitation is dissolved in chlorobenzene, institute
It obtains on solution spraying to conducting PET-ITO.Compared with traditional chloroform solvent, spray that resulting film is more uniform and light modulation model
It encloses to be bigger, the device of assembling is expected to be used for the wearable field of intelligence.
Beneficial effect
(1) operation of the present invention is easy, and required equipment is simple, at low cost, is suitble to the preparation of broad area device.
(2) present invention can control the thickness and uniformity of P3HT film by regulating and controlling experiment condition, change device
Performance.
(3) large area flexible P3HT electrochromic device prepared by the present invention has bistable property, and voltage is being not added
Shi Yanse remains to maintain.When applying low-voltage, the switching between aubergine and sky blue is may be implemented in device, and has response
The advantages that time is short, and color contrast is high, wearable in intelligence, intelligent display field is with a wide range of applications.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of P3HT base flexible electro-chromic device of the invention, and wherein PET-ITO is electrically conducting transparent
Layer, P3HT photochromic layer are electrochromic layer, and gel electrolyte is ion storage layer.
Fig. 2 is the SEM surface picture of P3HT film prepared by embodiment 1.
Fig. 3 is the cyclic voltammetry curve of large area P3HT base flexible electro-chromic device prepared by embodiment 1.
Fig. 4 is transmission of the large area P3HT base flexible electro-chromic device of the preparation of embodiment 2 when applying generating positive and negative voltage
Rate curve.
Fig. 5 is the transmitance time changing curve of large area P3HT base flexible electro-chromic device prepared by embodiment 3.
Fig. 6 is large area P3HT base flexible electro-chromic device pictorial diagram prepared by embodiment 3.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
(1) PET-ITO is pre-processed, impregnates 5min in ethanol, it is conductive after being dried with nitrogen to be placed in UV ozone up
40min is irradiated in instrument.
(2) P3HT (being purchased from Xi'an Bao Laite) is dispersed using magnetic agitation and ultrasound, chlorobenzene (purchase is added in P3HT
From traditional Chinese medicines) in pass through magnetic agitation 60min, be ultrasonically treated 60min, ultrasonic power 80W obtains P3HT spray solution, solution concentration
For 1mg/mL.
(3) spray gun is subjected to spraying operation using step (2) gained P3HT spray coating liquor is packed into after ethyl alcohol, acetone cleaning.It will
Conductive be placed in 120 DEG C of thermal station up of PET-ITO preheats 20min；Spray gun face PET-ITO base conductive face, from
Spraying operation is carried out in PET-ITO 5cm height, wherein spray gun air pump pressure is 0.2MPa, and P3HT quantity for spray is 0.2mg/
cm2；PET-ITO conducting surface is put into 120 DEG C of baking ovens dry 30min after the completion of spraying and obtains PET-ITO electrode.
(4) photochromic layer of the PET-ITO after will be dry in step (3) is pair with another PET-ITO as working electrode
Electrode.The lithium perchlorate for being 5.8% by mass fraction (being purchased from Aladdin), 27.6% PVDF's (being purchased from Su Wei) and 66.6%
Propene carbonate (be purchased from traditional Chinese medicines) mixing, stirring are configured to gel electrolyte for gel electrolyte and are injected into working electrode and right
Between electrode, working electrode with to the distance between electrode be 0.2mm, encapsulation, 5MPa, 120 DEG C of hot pressing 4min obtain large area
P3HT base flexible electro-chromic device.P3HT surface topography as shown in Fig. 2, spraying P3HT film crystalline region and amorphous area coexist,
Surface thickness is uniform.The cyclic voltammetry curve of large area P3HT base flexible device as shown in figure 3, have occurred oxidation also under voltage
Original reaction, realizes the doping of ion.
Embodiment 2
(1) PET-ITO is pre-processed, impregnates 8min in ethanol, it is conductive after being dried with nitrogen to be placed in UV ozone up
30min is irradiated in instrument.
(2) P3HT (being purchased from Xi'an Bao Laite) is dispersed using magnetic agitation and ultrasound, chlorobenzene (purchase is added in P3HT
From traditional Chinese medicines) in pass through magnetic agitation 120min, be ultrasonically treated 120min, ultrasonic power 60W obtains P3HT spray solution, and solution is dense
Degree is 1.2mg/mL.
(3) spray gun is subjected to spraying operation using step (2) gained P3HT spray coating liquor is packed into after ethyl alcohol, acetone cleaning.It will
Conductive be placed in 120 DEG C of thermal station up of PET-ITO preheats 15min；Spray gun face PET-ITO base conductive face, from
Spraying operation is carried out in PET-ITO 20cm height, wherein spray gun air pump pressure is 1MPa, and P3HT quantity for spray is 1.2mg/cm2；
PET-ITO conducting surface is put into 130 DEG C of baking ovens dry 60min after the completion of spraying and obtains PET-ITO electrode.
(4) photochromic layer of the PET-ITO after will be dry in step (3) is pair with another PET-ITO as working electrode
Electrode.The lithium perchlorate for being 8% by mass fraction (being purchased from Aladdin), the carbonic acid third of 22% PVDF (being purchased from Su Wei) and 50%
Enester (be purchased from traditional Chinese medicines) and 20% ionic liquid [Emim] BF4(purchased from silent Buddhist nun's chemical industry) mixing, stirring are configured to gel electricity
Gel electrolyte is injected into working electrode and between electrode by solution matter, working electrode be 0.5mm to the distance between electrode,
Encapsulation, 5MPa, 110 DEG C of hot pressing 10min obtain large area P3HT base flexible electro-chromic device.As shown in figure 4, in positive negative electricity
Different colors is presented in pressure P3HT film, and maximum light modulation range is 31% under 2V and -2V, after removing voltage, a few minutes
It inside can also maintain the color of pressurization.
Embodiment 3
(1) PET-ITO is pre-processed, impregnates 10min in ethanol, it is conductive after being dried with nitrogen to be placed in UV ozone up
60min is irradiated in instrument.
(2) P3HT (being purchased from Xi'an Bao Laite) is dispersed using magnetic agitation and ultrasound, chlorobenzene (purchase is added in P3HT
From traditional Chinese medicines) in pass through magnetic agitation 60min, be ultrasonically treated 120min, ultrasonic power 110W obtains P3HT spray solution, and solution is dense
Degree is 1.5mg/mL.
(3) spray gun is subjected to spraying operation using step (2) gained P3HT spray coating liquor is packed into after ethyl alcohol, acetone cleaning.It will
PET-ITO is placed in 100 DEG C of thermal station and preheats 10min；Spray gun face PET-ITO base conductive face, from PET-ITO 15cm
Spraying operation is carried out in height, wherein spray gun air pump pressure is 0.8MPa, and P3HT quantity for spray is 1.5mg/cm2；After the completion of spraying
PET-ITO conducting surface is put into 125 DEG C of baking ovens dry 50min and obtains PET-ITO electrode.
(4) photochromic layer of the PET-ITO after will be dry in step (3) is pair with another PET-ITO as working electrode
The lithium perchlorate (being purchased from Aladdin) that electrode is 4.8% by mass fraction, the carbonic acid of 23% PVDF (being purchased from Su Wei) and 55%
Acrylic ester (be purchased from traditional Chinese medicines) and 16.7% ionic liquid [Emim] BF4(purchased from silent Buddhist nun's chemical industry) mixing, stirring are configured to coagulate
Gel electrolyte is injected into working electrode to glue electrolyte and between electrode, working electrode is with to the distance between electrode
1mm, encapsulation, 5MPa, 120 DEG C of hot pressing 6min obtain large area P3HT base flexible electro-chromic device.As shown in figure 5, large area
P3HT base flexible device becomes 17s needed for sky blue from initial aubergine at 2V, 4s needed for becoming aubergine from sky blue.
As shown in fig. 6, being the device pictorial diagram under two kinds of voltage respectively.
Comparative example 1
By compound (poly- [2,3- bis- (3,4- dialkoxy phenyl) -5,8- two (3,4- ethylenedioxy thiophene base) quinoline
Quinoline]) it is dissolved in the solution that 2~3mg/ml is configured in chloroform, using Spray pen for art designer direct spraying in the surface of ito glass
Uniform film is obtained, is different from traditional plating film forming, spraying film forming is simple and easy to do, is more suitable for the preparation of large area film.
Compared with the present invention, the present invention selects solvent of the chlorobenzene as P3HT, can dissolve P3HT at normal temperature, forms a film more after spraying
The uniform and present invention directly prepares the flexible device of large area, still has good discoloration, can be directly applied to
On Flexible Displays.
Claims (9)
1. a kind of method of spray coating method preparation large area P3HT base flexible electro-chromic device, comprising:
(1) PET-ITO conductive substrates are pre-processed；
(2) poly- (3- hexyl thiophene) P3HT is dissolved in chlorobenzene, is stirred, ultrasonic treatment obtains P3HT spray solution, wherein P3HT
Spray solution concentration is 1~1.5mg/mL；
(3) PET-ITO conductive substrates pretreated in step (1) are preheated, P3HT spray solution in step (2) is uniformly sprayed
It is coated in the PET-ITO conductive substrates conducting surface of preheating, dry, wherein the quantity for spray of P3HT is 0.20~1.5mg/cm2；
It (4) is that gel is injected to electrode with another PET-ITO using the PET-ITO after drying in step (3) as working electrode
Electrolyte encapsulates hot pressing, obtains P3HT base flexible electro-chromic device.
2. the method according to claim 1, wherein PET-ITO conductive substrates are carried out in advance in the step (1)
Processing are as follows: PET-ITO conductive substrates are put into ethyl alcohol and impregnate 5-10min, rear PET-ITO conduction is dried with nitrogen and is placed in up
30~60min is irradiated in UV ozone instrument.
3. the method according to claim 1, wherein mixing time is 60~120min in the step (2)；It is super
The sonication time is 60~120min, and ultrasonic power is 60~110W.
4. the method according to claim 1, wherein will be pretreated in step (1) in the step (3)
PET-ITO conductive substrates preheating are as follows: PET-ITO conductive substrates conduction pretreated in step (1) is placed in thermal station up
Upper preheating, thermal station temperature are 100~120 DEG C, and heating time is 10~20min.
5. the method according to claim 1, wherein the step (3) in spraying are as follows: by spray gun using ethyl alcohol,
It is packed into P3HT spray solution after acetone cleaning to be sprayed, wherein spray gun air pump pressure is 0.2~1MPa, spray gun face PET-
ITO substrate conducting surface height is 5~20cm.
6. being done the method according to claim 1, wherein drying temperature is 120~130 DEG C in the step (3)
The dry time is 30~60min.
7. the method according to claim 1, wherein gel electrolyte component is according to quality in the step (4)
Score includes: lithium perchlorate 4~10%, Kynoar 15~30%, and propene carbonate 40~67% and ionic liquid 0~
20%.
8. the method according to claim 1, wherein working electrode and between electrode in the step (4)
Distance is 0.2~1mm.
9. the method according to claim 1, wherein in the step (4) hot pressing temperature be 80~120 DEG C, heat
Pressure pressure is 5MPa, and hot pressing time is 2~10min.
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| CN112666770A (en) * | 2021-01-12 | 2021-04-16 | 浙江工业大学 | Electrochromic flexible device based on P (SPMA-MMA) hydrogel electrolyte and preparation method and application thereof |
| WO2021159773A1 (en) * | 2020-02-14 | 2021-08-19 | 苏州苏大维格科技集团股份有限公司 | Electrochromic device and manufacturing method therefor |
| CN113640636A (en) * | 2021-08-25 | 2021-11-12 | 云南电网有限责任公司电力科学研究院 | Preparation method of film for corona discharge detection of power equipment |
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