CN103387343B - A kind of preparation method of nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane - Google Patents
A kind of preparation method of nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane Download PDFInfo
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Abstract
The present invention relates to a kind of nickel oxide/poly-(3,4 ethylenedioxy thiophenes) preparation method of compound electrochromic membrane, including: four water nickel acetates, carbamide are added in dehydrated alcohol, obtains reaction solution, then the FTO electro-conductive glass after supersound washing is immersed in the water heating kettle of reaction solution, at 160～180 DEG C, insulation 6～12h, is cooled to room temperature, cleans, calcining, obtains the FTO electro-conductive glass with NiO layer；By 3,4 ethylenedioxy thiophene monomers are dissolved in the carbonic allyl ester solution of lithium perchlorate and obtain depositing liquid, then insert in precipitated liquid the above-mentioned FTO electro-conductive glass with NiO layer as working electrode, carry out electro-deposition with platinized platinum for electrode, to obtain final product.The inventive method preparation technology is simple, low cost, can realize the structure design on micro-nano level of the organic/inorganic composite electrochromic material, makes the organic and respective advantage of inorganic electrochromic material be not fully exerted.
Description
Technical field
The invention belongs to the preparation field of electrochomeric films, multiple particularly to a kind of nickel oxide/poly-(3,4-ethylene dioxythiophene)
Close the preparation method of electrochomeric films.
Background technology
Electrochromic material is widely studied as one of intellectual material having application prospect most, and especially with transition metal
Oxide research is the most deep.But the transition metal oxide studied at present is applied to electrochromism color variable display device
A lot of problem is there is also in field.First, transition metal oxide electrochomeric films facing conductive Polymer Electrochromic material
Color change response time slower.Transition metal oxide or derivatives thereof, the change of its color is double due to ion and electronics
Injecting and black soy sauce goes out and causes, controlled by ion migration speed, therefore response time is slow；Furthermore, oxo transition metal
Although the stability of thin film organic electrochromic film relatively is high, but sull in use still suffers from electroluminescent
The phenomenon of discoloration decline, cyclical stability needs to be improved further.Electrochomeric films electrochemistry in use and chemistry
Dissolve and as the ion of the charge compensation accumulation the two chief reason in electrochomeric films so that electrochromism is thin
In use there is the phenomenon that electrochromic property is gradually lowered in film；Finally, transition metal oxide electrochomeric films
Colour efficiency is low, and color change is single, it is impossible to more comprehensively meet practical application request.
In the face of the deficiency of above inorganic electrochromic thin film, organic/inorganic nano complex technique is used for electrochromic material, preparation
Organic/inorganic compound electrochromic membrane is probably effective solution.As CN101891402A discloses a kind of colloidal sol
-gel method prepares WO3The method of/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane, F.Marystela et al. is at J.
Report a kind of LBL embrane method on Phys.Chem.B107 (2003) 8351 and prepare the side of organic/inorganic compound electrochromic membrane
Method, but compound electrochromic membrane prepared by these methods is generally multiple structure, and complex form is single, and contact with each other area
Less, organo-mineral complexing is the most insufficient, it is impossible to merges completely and plays respective advantage.Therefore there will be each film interlayer thing
Instability that Physicochemical combines, the problem such as incompatibility of preparation technology.Organic/inorganic is prepared in conjunction with hydro-thermal method and electrodeposition process
This method of compound electrochromic membrane can realize the structure design on micro-nano level of the organic/inorganic composite electrochromic material,
Make the organic and respective advantage of inorganic electrochromic material obtain comprehensive and give full play to, can obtain the electrochromic property highlighted.
Summary of the invention
It is thin that the technical problem to be solved is to provide a kind of nickel oxide/poly-(3,4-ethylene dioxythiophene) composite electrochromic
The preparation method of film, the method preparation technology is simple, and low cost can realize organic/inorganic composite electrochromic material micro-nano
Structure design on level, makes the organic and respective advantage of inorganic electrochromic material be not fully exerted.
A kind of preparation method of the nickel oxide of the present invention/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane, including:
(1) four water nickel acetates, carbamide are added in dehydrated alcohol, obtain reaction solution, then the FTO after supersound washing is conducted electricity
Glass immerses in the water heating kettle of reaction solution, at 160-180 DEG C, is incubated 6-12h, is cooled to room temperature, cleans, calcining,
Obtain the FTO electro-conductive glass with NiO layer；Wherein four water nickel acetates, the mass ratio of carbamide are 62:3, nickel acetate
Molar concentration be 0.060～0.080mol/L；
(2) 3,4-ethylene dioxythiophene monomer and lithium perchlorate are dissolved in carbonic allyl ester solution obtain deposit liquid, then by above-mentioned
FTO electro-conductive glass with NiO layer is inserted in precipitated liquid as working electrode, carries out electro-deposition with platinized platinum for electrode,
Obtain nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane；Wherein in carbonic allyl ester solution 3,
4-ethylenedioxy thiophene monomer and lithium perchlorate mol ratio be: 1:30～3:10.
Described reaction solution accounts for the 70%～80% of water heating kettle volume, and the volume of reactor is 75mL.
Supersound washing in described step (1) is to wash through deionized water, acetone and EtOH Sonicate successively, and the supersound washing time is
20～30min.
In described step (1), calcining heat is 400-600 DEG C, and calcination time is 2-4h.
In described step (2), in carbonic allyl ester solution, the concentration of lithium perchlorate is 0.1～0.3mol/L, 3,4-ethylene dioxythiophene list
The concentration of body is 0.01～0.03mol/L.
In described step (2), electro-deposition is that cyclic voltammetry carries out electro-deposition or constant voltage method carries out electro-deposition.
Described cyclic voltammetry carries out the parameter of electro-deposition: sweep limits is-1～1.5V, scanning speed 50～100mV/s, deposits 2～4
Individual circulation.
Described constant voltage method carries out the parameter of electro-deposition: voltage is 1.3～1.5V, and sedimentation time is 15～30s.
The present invention combines hydro-thermal method and electrodeposition process to prepare nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane,
Obtained thin film not only improves the shortcomings such as inorganic electrochromic material poor optical properties, color conversion is slow, cyclic reversibility is poor,
Also overcome that organic electrochromic material capability of resistance to radiation is poor and substrate adheres to loosely shortcoming simultaneously, can be assembled into all kinds of electroluminescent
Electrochromic device, has wide practical use in fields such as large screen displaies.
Beneficial effect
(1) preparation method of the present invention is simple, low cost, is suitable for large-scale production；
(2) present invention combines hydro-thermal method and electrodeposition process achieves organic and inorganic electrochromic material answering on micro-nano level
Close, structure design can be carried out by controlling technological parameter, provide real for the most open novel electrochromic thin-film material
Test and theoretical basis；
(3) nickel oxide of the present invention/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane not only overcomes inorganic electroluminescence change
The shortcomings such as color device for Optical Properties of Materials is poor, color conversion is slow, cyclic reversibility is poor, also overcome organic electrochromic material simultaneously
Capability of resistance to radiation is poor and substrate adheres to the shortcoming such as loosely for material, can be assembled into all kinds of electrochromic device, aobvious at giant-screen
Show etc. that field has wide practical use.
Accompanying drawing explanation
The stereoscan photograph of the electro-allochromatic nickel oxide film of Fig. 1 embodiment 1 preparation；
The stereoscan photograph of nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane of Fig. 2 embodiment 1 preparation；
Nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane of Fig. 3 embodiment 1 preparation is at oxidation state and reduction-state
The digital photograph of variable color under (negative voltage and positive voltage)；
The cyclic voltammetry curve figure of nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane of Fig. 4 embodiment 1 preparation；
Nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane of Fig. 5 embodiment 1 preparation electricity under different voltages
Stream time plot.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments be merely to illustrate the present invention and not
For limiting the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, those skilled in the art can
To make various changes or modifications the present invention, these equivalent form of values fall within the application appended claims limited range equally.
Embodiment 1
FTO electro-conductive glass is immersed successively respective supersound washing 20 minutes, dry for standby in deionized water, acetone and ethanol.
Weigh 1.24g tetra-water nickel acetate and 0.6g carbamide is dissolved in 56mL dehydrated alcohol, then by the FTO conduction glass of ultrasonic cleaning
Glass invades in the water heating kettle filling reaction solution, and reaction solution accounts for the 75% of water heating kettle volume, is incubated 6 hours in 180 DEG C,
After naturally cool to room temperature, take out FTO electro-conductive glass, after cleaning successively with water and ethanol, dry, at 400 DEG C, calcine 2
Hour obtain the FTO electro-conductive glass with NiO layer；Take 0.425mL3,4-ethylenedioxy thiophene monomer and be dissolved in 200mL
The carbonic allyl ester solution of the lithium perchlorate of 0.1mol/L obtains deposit liquid, the FTO with NiO layer obtained above is conducted electricity
Glass is inserted in deposition liquid as working electrode, with platinized platinum for electrode, at cyclic voltammetry-1V～1.5V, scanning speed
50mV/s, deposits and obtains nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane under 2 cycling conditions.Fig. 1
Stereoscan photograph for obtained NiO layer, it can be seen that this thin film is made up of porous flake NiO, its aperture is about
0.5～3 μm.Fig. 2 is that the scanning electron microscope of obtained nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane shines
Sheet, it can be seen that poly-(3,4-ethylene dioxythiophene) is attached to porous laminar NiO surface.Fig. 3 is made nickel oxide
/ poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane is the digital photograph of variable color under reduction-state with oxidation state.Fig. 4 is will
Nickel oxide/poly-(3,4-ethylene dioxythiophene) laminated film is as working electrode, and Ag/AgCl is reference electrode, and platinized platinum is right
The cyclic voltammetry curve figure that electrode is tested in the polycarbonate solution of the lithium perchlorate of 1mol/L, it can be seen that have obvious oxygen
Change reduction peak, it was demonstrated that gained thin film has electrochromism phenomenon in the voltage range of-1～1.6V.Fig. 5 be obtained nickel oxide/
Poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane current-time curvel figure under different voltages, it can be seen that just
Under negative voltage, color transformation time is different, but all in 3s, more much faster than single oxide electrochomeric films.
Embodiment 2
FTO electro-conductive glass is immersed successively respective supersound washing 25 minutes, dry for standby in deionized water, acetone and ethanol.
Weigh 1.24g tetra-water nickel acetate and 0.6g carbamide is dissolved in 56mL dehydrated alcohol, then by the FTO conduction glass of ultrasonic cleaning
Glass invades in the water heating kettle filling reaction solution, and reaction solution accounts for the 70% of water heating kettle volume, is incubated 12 hours in 170 DEG C,
Finally naturally cool to room temperature, take out FTO electro-conductive glass, after cleaning successively with water and ethanol, dry, calcine at 400 DEG C
Within 4 hours, obtain the FTO electro-conductive glass with NiO layer；Take 0.425mL3,4-ethylenedioxy thiophene monomer and be dissolved in 200mL
Obtaining in the carbonic allyl ester solution of the lithium perchlorate of 0.3mol/L depositing liquid, the FTO with NiO layer the most obtained above leads
Electricity glass is inserted in deposition liquid as working electrode, with platinized platinum for electrode, at cyclic voltammetry-1V～1.5V, scanning speed
50mV/s, deposits and obtains nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane under 4 cycling conditions.Sweep
Retouch electromicroscopic photograph and show to have obtained nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane, poly-in thin film (3,
4-ethylenedioxy thiophene) attachment pattern is roughly the same with enforcement row 1, but poly-(3,4-ethylene dioxythiophene) of attachment is many
In embodiment 1, electrochromic property test shows that the color change under different voltages of this thin film is compounded with NiO and poly-(3,4-
Ethylenedioxy thiophene) electrochromic effect.
Embodiment 3
FTO electro-conductive glass is immersed successively respective supersound washing 25 minutes, dry for standby in deionized water, acetone and ethanol.
Weigh 1.44g tetra-water nickel acetate and 0.70g carbamide is dissolved in 56mL dehydrated alcohol, then the FTO of ultrasonic cleaning is conducted electricity
Glass invades in the water heating kettle filling reaction solution, and reaction solution accounts for the 75% of water heating kettle volume, is incubated 12 hours in 160 DEG C,
Finally naturally cool to room temperature, take out FTO electro-conductive glass, after cleaning successively with water and ethanol, dry, calcine at 500 DEG C
Within 3 hours, obtain the FTO electro-conductive glass with NiO layer；Take 0.213mL3,4-ethylenedioxy thiophene monomer and be dissolved in 200mL0.2
Obtaining depositing liquid in the carbonic allyl ester solution of the lithium perchlorate of mol/L, the FTO with NiO layer the most obtained above conducts electricity
Glass is inserted in deposition liquid as working electrode, with platinized platinum for electrode, at cyclic voltammetry-1V～1.5V, scanning speed
100mV/s, deposits and obtains nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane under 3 cycling conditions.Sweep
Retouch electromicroscopic photograph and show to have obtained nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane, poly-in thin film (3,
4-ethylenedioxy thiophene) attachment pattern is roughly the same with implement in row 1, and electrochromic property is tested and is shown that this thin film is in difference
Color change under voltage is compounded with NiO and poly-(3,4-ethylene dioxythiophene) electrochromic effect.
Embodiment 4
FTO electro-conductive glass is immersed successively respective supersound washing 30 minutes, dry for standby in deionized water, acetone and ethanol.
Weigh 1.08g tetra-water nickel acetate and 0.52g carbamide is dissolved in 56mL dehydrated alcohol, then the FTO of ultrasonic cleaning is conducted electricity
Glass invades in the water heating kettle filling reaction solution, and reaction solution accounts for the 80% of water heating kettle volume, is incubated 9 hours in 170 DEG C,
Finally naturally cool to room temperature, take out FTO electro-conductive glass, after cleaning successively with water and ethanol, dry, calcine at 600 DEG C
Within 2 hours, obtain the FTO electro-conductive glass with NiO layer；Take 0.638mL3,4-ethylenedioxy thiophene monomer and be dissolved in 200mL
The carbonic allyl ester solution of the lithium perchlorate of 0.3mol/L obtains deposit liquid, the FTO with NiO layer obtained above is conducted electricity
Glass is inserted in deposition liquid as working electrode, with platinized platinum for electrode, constant voltage 1.3V electro-deposition 30s obtain nickel oxide/
Poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane.Stereoscan photograph shows to have obtained nickel oxide/poly-(3,4-second
Support dioxy thiophene) compound electrochromic membrane, but poly-in thin film (3,4-ethylene dioxythiophene) adheres to pattern and implements in row 1
Differ, can entirety load onto in partially porous NiO hole, electrochromic property test shows that this thin film is under different voltages
Color change be compounded with NiO and poly-(3,4-ethylene dioxythiophene) electrochromic effect.
Embodiment 5
FTO electro-conductive glass is immersed successively respective supersound washing 25 minutes, dry for standby in deionized water, acetone and ethanol.
Weigh 1.08g tetra-water nickel acetate and 0.52g carbamide is dissolved in 56mL dehydrated alcohol, then the FTO of ultrasonic cleaning is conducted electricity
Glass invades in the water heating kettle filling reaction solution, and reaction solution accounts for the 75% of water heating kettle volume, is incubated 9 hours in 180 DEG C,
Finally naturally cool to room temperature, take out FTO electro-conductive glass, after cleaning successively with water and ethanol, dry, calcine at 400 DEG C
Within 4 hours, obtain the FTO electro-conductive glass with NiO layer；Take 0.425mL3,4-ethylenedioxy thiophene monomer and be dissolved in 200mL
Obtaining in the carbonic allyl ester solution of the lithium perchlorate of 0.2mol/L depositing liquid, the FTO with NiO layer the most obtained above leads
Electricity glass is inserted in deposition liquid as working electrode, with platinized platinum for electrode, obtains under the conditions of constant voltage 1.4V electro-deposition 25s
Nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane.Stereoscan photograph show to have obtained nickel oxide/poly-(3,
4-ethylenedioxy thiophene) compound electrochromic membrane, but poly-in thin film (3,4-ethylene dioxythiophene) attachment pattern and enforcement row
Different in 1, can entirety load onto in partially porous NiO hole, and electrochromic property test shows that this thin film is at different electricity
The color change of pressure is compounded with NiO and poly-(3,4-ethylene dioxythiophene) electrochromic effect.
Embodiment 6
FTO electro-conductive glass is immersed successively respective supersound washing 20 minutes, dry for standby in deionized water, acetone and ethanol.
Weigh 1.44g tetra-water nickel acetate and 0.70g carbamide is dissolved in 56mL dehydrated alcohol, then the FTO of ultrasonic cleaning is conducted electricity
Glass invades in the water heating kettle filling reaction solution, and reaction solution accounts for the 75% of water heating kettle volume, is incubated 12 hours in 180 DEG C,
Finally naturally cool to room temperature, take out FTO electro-conductive glass, after cleaning successively with water and ethanol, dry, calcine at 500 DEG C
Within 2 hours, obtain the FTO electro-conductive glass with NiO layer；Take 0.638mL3,4-ethylenedioxy thiophene monomer and be dissolved in 200mL
Obtaining in the carbonic allyl ester solution of the lithium perchlorate of 0.1mol/L depositing liquid, the FTO with NiO layer the most obtained above leads
Electricity glass is inserted in deposition liquid as working electrode, with platinized platinum for electrode, with platinized platinum for electrode, electric at constant voltage 1.5V
Nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane is obtained under the conditions of deposition 15s.Stereoscan photograph shows
Obtain nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane, but (3,4-enedioxy thiophenes poly-in thin film
Fen) attachment pattern is different with implement in row 1, can entirety load onto in partially porous NiO hole, electrochromic property survey
This thin film bright color change under different voltages of taking temperature is compounded with NiO and poly-(3,4-ethylene dioxythiophene) electrochromic effect.
Claims (8)
1. the preparation method of nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane, including:
(1) four water nickel acetates, carbamide are added in dehydrated alcohol, obtain reaction solution, then the FTO after supersound washing is conducted electricity
Glass immerses in the water heating kettle of reaction solution, at 160～180 DEG C, is incubated 6～12h, is cooled to room temperature, cleans, calcining,
Obtain the FTO electro-conductive glass with NiO layer；Wherein four water nickel acetates, the mass ratio of carbamide are 62:3, nickel acetate
Molar concentration be 0.060～0.080mol/L；
(2) 3,4-ethylene dioxythiophene monomer and lithium perchlorate are dissolved in carbonic allyl ester solution obtain depositing liquid, then by above-mentioned
FTO electro-conductive glass with NiO layer is inserted in precipitated liquid as working electrode, carries out electro-deposition with platinized platinum for electrode,
Obtain nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane；Wherein in carbonic allyl ester solution 3,
4-ethylenedioxy thiophene monomer and lithium perchlorate mol ratio be: 1:30～3:10.
The preparation side of a kind of nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane the most according to claim 1
Method, it is characterised in that: described reaction solution accounts for the 70%～80% of water heating kettle volume, and the volume of reactor is 75mL.
The preparation side of a kind of nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane the most according to claim 1
Method, it is characterised in that: the supersound washing in described step (1) is to wash through deionized water, acetone and EtOH Sonicate successively,
The supersound washing time is 20～30min.
The preparation side of a kind of nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane the most according to claim 1
Method, it is characterised in that: in described step (1), calcining heat is 400～600 DEG C, and calcination time is 2～4h.
The preparation side of a kind of nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane the most according to claim 1
Method, it is characterised in that: in described step (2), in carbonic allyl ester solution, the concentration of lithium perchlorate is 0.1～0.3mol/L,
The concentration of 3,4-ethylene dioxythiophene monomer is 0.01～0.03mol/L.
The preparation side of a kind of nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane the most according to claim 1
Method, it is characterised in that: in described step (2), electro-deposition is that cyclic voltammetry carries out electro-deposition or constant voltage method carries out electricity and sinks
Long-pending.
The preparation side of a kind of nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane the most according to claim 6
Method, it is characterised in that: described cyclic voltammetry carries out the parameter of electro-deposition and is: sweep limits is-1～1.5V, scanning speed
50～100mV/s, deposit 2～4 circulations.
The preparation side of a kind of nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane the most according to claim 6
Method, it is characterised in that: described constant voltage method carries out the parameter of electro-deposition and is: voltage is 1.3～1.5V, and sedimentation time is 15～30s.
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