CN103387343A - Preparation method of nickel oxide/poly(3,4- ethylenedioxythiophene) compound electrochromic film - Google Patents
Preparation method of nickel oxide/poly(3,4- ethylenedioxythiophene) compound electrochromic film Download PDFInfo
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Abstract
The invention relates to a preparation method of nickel oxide/poly(3,4- ethylenedioxythiophene) compound electrochromic film. The preparation method comprises following steps: adding nickel acetate tetrahydrate and urea into absolute ethanol to prepare a reaction solution, putting FTO conductive glass, which has been washed by ultrasonic, into a hydrothermal reactor filled with the reaction solution, controlling the temperature in the range of 160 and 180 DEG C, maintaining the temperature for 6 to 12 hours, cooling to the room temperature, washing, burning so as to obtain FTO conductive glass with a NiO layer, dissolving 4- ethylenedioxythiophene monomers into a propylene carbonate solution of lithium perchlorate to obtain deposition liquid, then putting the FTO conductive glass with a NiO layer into the deposition liquid to play as a work electrode, taking a platinum slice as the counter electrode, then performing electro-deposition reactions so as the obtain the product. The preparation method has the advantages of simple technology and low cost, structure design in the micro-nano grade of the inorganic/organic compound electrochromic materials can be achieved, so the respective advantages of the organic and inorganic electrochromic materials can be fully utilized.
Description
Technical field
The invention belongs to the preparation field of electrochomeric films, particularly the preparation method of a kind of nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane.
Background technology
Electrochromic material is widely studied as one of intelligent material that application prospect is arranged at present most, and especially deep with transition metal oxide research.But the present transition metal oxide of studying is applied to the fields such as the changeable color display device of electrochromism and also has a lot of problems.The first, it is slower that the relative electrochromic conducting polymer of transition metal oxide electrochomeric films causes the colour-change time of response of off-color material.Transition metal oxide or derivatives thereof, its colour-change are to inject and black soy sauce goes out to cause due to ion and electronics two, be subjected to the control of ion migration speed, so the time of response are slow; Moreover although organic electrochromic film is high relatively for the stability of transition metal oxide film, in use still there is the phenomenon of electrochromic property decline in sull, and cyclical stability remains further to be improved.Electrochomeric films electrochemistry and chemical dissolution and as these two chief reasons of the accumulation of ion in electrochomeric films of charge compensation, the phenomenon that makes electrochomeric films in use exist electrochromic property to reduce gradually in use; Finally, transition metal oxide electrochomeric films coloration efficiency is low, and colour-change is single, can not more comprehensively meet practical application request.
In the face of the deficiency of above inorganic electrochromic film, the organic/inorganic nano compounding technology is used for electrochromic material, preparing organic/inorganic compound electrochromic membrane may be effective solution.Disclose a kind of sol-gel method as CN101891402A and prepared WO
3/ poly-(3, the 4-ethylenedioxy thiophene) method of compound electrochromic membrane, the people such as F.Marystela have reported that on J.Phys.Chem.B107 (2003) 8351 a kind of LBL embrane method prepares the method for organic/inorganic compound electrochromic membrane, but the compound electrochromic membrane of these method preparations is generally multilayered structure, complex form is single, be in contact with one another area less, organic and inorganic compound merges insufficient, can not merge and bring into play advantage separately fully.Therefore the problems such as non-compatibility that there will be unstable, the preparation technology of physical chemistry combination between each rete.Prepare this method of organic/inorganic compound electrochromic membrane in conjunction with hydrothermal method and electrodip process and can realize the structure design of organic/inorganic composite electrochromic material on micro-nano level, make organic and inorganic electrochromic material advantage separately obtain comprehensive and give full play to, can obtain the electrochromic property of giving prominence to.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of nickel oxide/poly-(3, the 4-ethylenedioxy thiophene) preparation method of compound electrochromic membrane, the method preparation technology is simple, cost is low, can realize the structure design of organic/inorganic composite electrochromic material on micro-nano level, organic and inorganic electrochromic material advantage separately is not fully exerted.
The preparation method of a kind of nickel oxide of the present invention/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane comprises:
(1) four water nickelous acetates, urea are added in dehydrated alcohol, obtain reaction soln, then the FTO conductive glass after supersound washing is immersed in the water heating kettle of reaction soln, at 160-180 ℃, insulation 6-12h, be cooled to room temperature, clean, calcining, obtain the FTO conductive glass with the NiO layer; Wherein the mass ratio of four water nickelous acetates, urea is 62:3, and the volumetric molar concentration of nickelous acetate is 0.060～0.080mol/L;
(2) with 3,4-ethylenedioxy thiophene monomer and lithium perchlorate are dissolved in carbonic allyl ester solution and obtain deposit fluid, then the above-mentioned conductive glass of FTO with the NiO layer is inserted in precipitated liquid as working electrode, take platinized platinum as electrode is carried out galvanic deposit, obtain nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane; Wherein 3,4-ethylene dioxythiophene monomer and lithium perchlorate mol ratio are in carbonic allyl ester solution: 1:30～3:10.
Described reaction soln accounts for 70%～80% of water heating kettle volume, and the volume of reactor is 75mL.
Supersound washing in described step (1) is for successively through deionized water, acetone and ethanol supersound washing, and the supersound washing time is 20～30min.
In described step (1), calcining temperature is 400-600 ℃, and calcination time is 2-4h.
In the middle carbonic allyl ester solution of described step (2), the concentration of lithium perchlorate is 0.1～0.3mol/L, and the concentration of 3,4-ethylene dioxythiophene monomer is 0.01～0.03mol/L.
In described step (2), galvanic deposit is that cyclic voltammetry is carried out galvanic deposit or the constant voltage method is carried out galvanic deposit.
The parameter that described cyclic voltammetry is carried out galvanic deposit is: sweep limit is-1～1.5V, and sweep velocity 50～100mV/s deposits 2～4 circulations.
The parameter that described constant voltage method is carried out galvanic deposit is: voltage is 1.3～1.5V, and depositing time is 15～30s.
The present invention prepares nickel oxide/poly-(3 in conjunction with hydrothermal method and electrodip process, the 4-ethylenedioxy thiophene) compound electrochromic membrane, prepared film has not only improved the inorganic electrochromic material poor optical properties, color transforms the shortcomings such as slow, that cyclic reversibility is poor, also overcome simultaneously the organic electrochromic material capability of resistance to radiation poor, adhere to not firm shortcoming with substrate, can be assembled into all kinds of electrochromic devices, in fields such as large screen displaies, have wide practical use.
Beneficial effect
(1) preparation method of the present invention is simple, and cost is low, is fit to large-scale production;
(2) the present invention has realized compound on micro-nano level of organic and inorganic electrochromic material in conjunction with hydrothermal method and electrodip process, can carry out structure design by controlling processing parameter, for further open novel electrochromic thin-film material provides experiment and theoretical basis;
(3) nickel oxide of the present invention/poly-(3, the 4-ethylenedioxy thiophene) compound electrochromic membrane has not only overcome the inorganic electrochromic material poor optical properties, color transforms the shortcomings such as slow, that cyclic reversibility is poor, also overcome simultaneously the organic electrochromic material capability of resistance to radiation poor, adhere to the shortcomings such as not firm with substrate, can be assembled into all kinds of electrochromic devices, in fields such as large screen displaies, have wide practical use.
Description of drawings
The stereoscan photograph of the electro-allochromatic nickel oxide film of Fig. 1 embodiment 1 preparation;
The stereoscan photograph of the nickel oxide of Fig. 2 embodiment 1 preparation/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane;
The nickel oxide of Fig. 3 embodiment 1 preparation/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane is at the digital photograph of oxidation state and the lower variable color of reduction-state (negative voltage and positive voltage);
The cyclic voltammetry curve figure of the nickel oxide of Fig. 4 embodiment 1 preparation/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane;
The nickel oxide of Fig. 5 embodiment 1 preparation/poly-current-time curvel figure of (3,4-ethylene dioxythiophene) compound electrochromic membrane under different voltages.
Embodiment
, below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only are not used in and limit the scope of the invention for explanation the present invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
The FTO conductive glass is immersed in deionized water, acetone and ethanol supersound washing separately 20 minutes, dry for standby successively.Taking 1.24g four water nickelous acetates and 0.6g urea is dissolved in the 56mL dehydrated alcohol, then the FTO conductive glass of ultrasonic cleaning is invaded and filled in the water heating kettle of reaction soln, reaction soln accounts for 75% of water heating kettle volume, in 180 ℃ of insulations 6 hours, naturally cool to finally room temperature, take out the FTO conductive glass, after water and ethanol clean successively, dry, the FTO conductive glass that calcining obtained with the NiO layer in 2 hours under 400 ℃; Get 0.425mL3,4-ethylenedioxy thiophene monomer is dissolved in the carbonic allyl ester solution of lithium perchlorate of 200mL0.1mol/L and obtains deposit fluid, FTO with NiO layer conductive glass obtained above is inserted in deposit fluid as working electrode, take platinized platinum as to electrode, at cyclic voltammetry-1V～1.5V, sweep velocity 50mV/s, deposit under 2 cycling conditions and obtain nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane.Fig. 1 is the stereoscan photograph of obtained NiO layer, can find out that this film is comprised of the laminar NiO of porous, and its aperture is approximately 0.5～3 μ m.Fig. 2 is the stereoscan photograph of prepared nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane, can see that poly-(3,4-ethylene dioxythiophene) is attached to the laminar NiO of porous surface.Fig. 3 is the digital photograph of made nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane variable color under reduction-state and oxidation state.Fig. 4 is with nickel oxide/poly-(3, the 4-ethylenedioxy thiophene) laminated film is as working electrode, Ag/AgCl is reference electrode, the cyclic voltammetry curve figure of platinized platinum for electrode is tested in the polycarbonate solution of the lithium perchlorate of 1mol/L, can see obvious redox peak is arranged, prove that the gained film has the electrochromism phenomenon in the voltage range of-1～1.6V.Fig. 5 is prepared nickel oxide/poly-(3, the 4-ethylenedioxy thiophene) the current-time curvel figure of compound electrochromic membrane under different voltages, can find out that the color transformation time is different under generating positive and negative voltage, but all in 3s, than fast many of single oxide compound electrochomeric films.
The FTO conductive glass is immersed in deionized water, acetone and ethanol supersound washing separately 25 minutes, dry for standby successively.Taking 1.24g four water nickelous acetates and 0.6g urea is dissolved in the 56mL dehydrated alcohol, then the FTO conductive glass of ultrasonic cleaning is invaded and filled in the water heating kettle of reaction soln, reaction soln accounts for 70% of water heating kettle volume, in 170 ℃ of insulations 12 hours, naturally cool to finally room temperature, take out the FTO conductive glass, after water and ethanol clean successively, dry, the FTO conductive glass that calcining obtained with the NiO layer in 4 hours under 400 ℃; Get 0.425mL3,4-ethylenedioxy thiophene monomer is dissolved in the carbonic allyl ester solution of lithium perchlorate of 200mL0.3mol/L and obtains deposit fluid, FTO with NiO layer conductive glass just obtained above is inserted in deposit fluid as working electrode, take platinized platinum as to electrode, at cyclic voltammetry-1V～1.5V, sweep velocity 50mV/s, deposit under 4 cycling conditions and obtain nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane.Stereoscan photograph shows and has obtained nickel oxide/poly-(3, the 4-ethylenedioxy thiophene) compound electrochromic membrane, gather (3 in film, the 4-ethylenedioxy thiophene) adhere to roughly the same in pattern and implementation column 1, but that adheres to gathers (3, the 4-ethylenedioxy thiophene) more than embodiment 1, the electrochromic property test shows that the colour-change of this film under different voltages is compounded with NiO and poly-(3,4-ethylene dioxythiophene) electrochromic effect.
Embodiment 3
The FTO conductive glass is immersed in deionized water, acetone and ethanol supersound washing separately 25 minutes, dry for standby successively.Taking 1.44g four water nickelous acetates and 0.70g urea is dissolved in the 56mL dehydrated alcohol, then the FTO conductive glass of ultrasonic cleaning is invaded and filled in the water heating kettle of reaction soln, reaction soln accounts for 75% of water heating kettle volume, in 160 ℃ of insulations 12 hours, naturally cool to finally room temperature, take out the FTO conductive glass, after water and ethanol clean successively, dry, the FTO conductive glass that calcining obtained with the NiO layer in 3 hours under 500 ℃; Get 0.213mL3,4-ethylenedioxy thiophene monomer is dissolved in the carbonic allyl ester solution of lithium perchlorate of 200mL0.2mol/L and obtains deposit fluid, FTO with NiO layer conductive glass just obtained above is inserted in deposit fluid as working electrode, take platinized platinum as to electrode, at cyclic voltammetry-1V～1.5V, sweep velocity 100mV/s, deposit under 3 cycling conditions and obtain nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane.Stereoscan photograph shows and has obtained nickel oxide/poly-(3, the 4-ethylenedioxy thiophene) compound electrochromic membrane, gather (3 in film, the 4-ethylenedioxy thiophene) adhere to roughly the same in pattern and implementation column 1, the electrochromic property test shows that the colour-change of this film under different voltages is compounded with NiO and poly-(3,4-ethylene dioxythiophene) electrochromic effect.
The FTO conductive glass is immersed in deionized water, acetone and ethanol supersound washing separately 30 minutes, dry for standby successively.Taking 1.08g four water nickelous acetates and 0.52g urea is dissolved in the 56mL dehydrated alcohol, then the FTO conductive glass of ultrasonic cleaning is invaded and filled in the water heating kettle of reaction soln, reaction soln accounts for 80% of water heating kettle volume, in 170 ℃ of insulations 9 hours, naturally cool to finally room temperature, take out the FTO conductive glass, after water and ethanol clean successively, dry, the FTO conductive glass that calcining obtained with the NiO layer in 2 hours under 600 ℃; Get 0.638mL3,4-ethylenedioxy thiophene monomer is dissolved in the carbonic allyl ester solution of lithium perchlorate of 200mL0.3mol/L and obtains deposit fluid, FTO with NiO layer conductive glass obtained above is inserted in deposit fluid as working electrode, take platinized platinum as to electrode, obtain nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane at constant voltage 1.3V galvanic deposit 30s.Stereoscan photograph shows and has obtained nickel oxide/poly-(3, the 4-ethylenedioxy thiophene) compound electrochromic membrane, but gather (3 in film, the 4-ethylenedioxy thiophene) adhere to not identical in pattern and implementation column 1, can wholely clog in partially porous NiO hole, the electrochromic property test shows that the colour-change of this film under different voltages is compounded with NiO and poly-(3,4-ethylene dioxythiophene) electrochromic effect.
The FTO conductive glass is immersed in deionized water, acetone and ethanol supersound washing separately 25 minutes, dry for standby successively.Taking 1.08g four water nickelous acetates and 0.52g urea is dissolved in the 56mL dehydrated alcohol, then the FTO conductive glass of ultrasonic cleaning is invaded and filled in the water heating kettle of reaction soln, reaction soln accounts for 75% of water heating kettle volume, in 180 ℃ of insulations 9 hours, naturally cool to finally room temperature, take out the FTO conductive glass, after water and ethanol clean successively, dry, the FTO conductive glass that calcining obtained with the NiO layer in 4 hours under 400 ℃; Get 0.425mL3,4-ethylenedioxy thiophene monomer is dissolved in the carbonic allyl ester solution of lithium perchlorate of 200mL0.2mol/L and obtains deposit fluid, FTO with NiO layer conductive glass just obtained above is inserted in deposit fluid as working electrode, take platinized platinum as to electrode, obtain nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane under constant voltage 1.4V galvanic deposit 25s condition.Stereoscan photograph shows and has obtained nickel oxide/poly-(3, the 4-ethylenedioxy thiophene) compound electrochromic membrane, but gather (3 in film, the 4-ethylenedioxy thiophene) adhere to different in pattern and implementation column 1, can wholely clog in partially porous NiO hole, the electrochromic property test shows that the colour-change of this film under different voltages is compounded with NiO and poly-(3,4-ethylene dioxythiophene) electrochromic effect.
The FTO conductive glass is immersed in deionized water, acetone and ethanol supersound washing separately 20 minutes, dry for standby successively.Taking 1.44g four water nickelous acetates and 0.70g urea is dissolved in the 56mL dehydrated alcohol, then the FTO conductive glass of ultrasonic cleaning is invaded and filled in the water heating kettle of reaction soln, reaction soln accounts for 75% of water heating kettle volume, in 180 ℃ of insulations 12 hours, naturally cool to finally room temperature, take out the FTO conductive glass, after water and ethanol clean successively, dry, the FTO conductive glass that calcining obtained with the NiO layer in 2 hours under 500 ℃; Get 0.638mL3,4-ethylenedioxy thiophene monomer is dissolved in the carbonic allyl ester solution of lithium perchlorate of 200mL0.1mol/L and obtains deposit fluid, FTO with NiO layer conductive glass just obtained above is inserted in deposit fluid as working electrode, take platinized platinum as to electrode, take platinized platinum as to electrode, obtaining nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane under constant voltage 1.5V galvanic deposit 15s condition.Stereoscan photograph shows and has obtained nickel oxide/poly-(3, the 4-ethylenedioxy thiophene) compound electrochromic membrane, but gather (3 in film, the 4-ethylenedioxy thiophene) adhere to different in pattern and implementation column 1, can wholely clog in partially porous NiO hole, the electrochromic property test shows that the colour-change of this film under different voltages is compounded with NiO and poly-(3,4-ethylene dioxythiophene) electrochromic effect.
Claims (8)
1. the preparation method an of nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane comprises:
(1) four water nickelous acetates, urea are added in dehydrated alcohol, obtain reaction soln, then the FTO conductive glass after supersound washing is immersed in the water heating kettle of reaction soln, at 160～180 ℃, insulation 6～12h, be cooled to room temperature, clean, calcining, obtain the FTO conductive glass with the NiO layer; Wherein the mass ratio of four water nickelous acetates, urea is 62:3, and the volumetric molar concentration of nickelous acetate is 0.060～0.080mol/L;
(2) with 3,4-ethylenedioxy thiophene monomer and lithium perchlorate are dissolved in carbonic allyl ester solution and obtain deposit fluid, then the above-mentioned conductive glass of FTO with the NiO layer is inserted in precipitated liquid as working electrode, take platinized platinum as electrode is carried out galvanic deposit, obtain nickel oxide/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane; Wherein 3,4-ethylene dioxythiophene monomer and lithium perchlorate mol ratio are in carbonic allyl ester solution: 1:30～3:10.
2. the preparation method of a kind of nickel oxide according to claim 1/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane, it is characterized in that: described reaction soln accounts for 70%～80% of water heating kettle volume, and the volume of reactor is 75mL.
3. a kind of nickel oxide according to claim 1/poly-(3, the 4-ethylenedioxy thiophene) preparation method of compound electrochromic membrane, it is characterized in that: the supersound washing in described step (1) is for successively through deionized water, acetone and ethanol supersound washing, and the supersound washing time is 20～30min.
4. the preparation method of a kind of nickel oxide according to claim 1/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane, it is characterized in that: in described step (1), calcining temperature is 400～600 ℃, and calcination time is 2～4h.
5. a kind of nickel oxide according to claim 1/poly-(3, the 4-ethylenedioxy thiophene) preparation method of compound electrochromic membrane, it is characterized in that: in described step (2) in carbonic allyl ester solution the concentration of lithium perchlorate be 0.1～0.3mol/L, the concentration of 3,4-ethylene dioxythiophene monomer is 0.01～0.03mol/L.
6. the preparation method of a kind of nickel oxide according to claim 1/poly-(3,4-ethylene dioxythiophene) compound electrochromic membrane, it is characterized in that: in described step (2), galvanic deposit is that cyclic voltammetry is carried out galvanic deposit or the constant voltage method is carried out galvanic deposit.
7. a kind of nickel oxide according to claim 6/poly-(3, the 4-ethylenedioxy thiophene) preparation method of compound electrochromic membrane, it is characterized in that: the parameter that described cyclic voltammetry is carried out galvanic deposit is: sweep limit is-1～1.5V, sweep velocity 50～100mV/s, deposit 2～4 circulations.
8. a kind of nickel oxide according to claim 6/poly-(3, the 4-ethylenedioxy thiophene) preparation method of compound electrochromic membrane, it is characterized in that: the parameter that described constant voltage method is carried out galvanic deposit is: voltage is 1.3～1.5V, and depositing time is 15～30s.
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| CN114563895A (en) * | 2022-03-10 | 2022-05-31 | 四川大学 | Porous conductive polymer-based electrochromic film and preparation method thereof |
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