CN107602890A - The preparation method of cerium titanyl cluster/poly- 3,4 ethene dioxythiophene laminated film - Google Patents
The preparation method of cerium titanyl cluster/poly- 3,4 ethene dioxythiophene laminated film Download PDFInfo
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- CN107602890A CN107602890A CN201710767660.6A CN201710767660A CN107602890A CN 107602890 A CN107602890 A CN 107602890A CN 201710767660 A CN201710767660 A CN 201710767660A CN 107602890 A CN107602890 A CN 107602890A
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Abstract
The invention discloses a kind of cerium titanyl cluster/poly- 3,4 ethene dioxythiophene laminated film and its application.The laminated film is prepared by the following method：To being pre-loaded with adding 3 in the container of acetonitrile and dichloromethane, 4 ethene dioxythiophenes, the cerium titanyl cluster prepared using hydrothermal synthesis method, with rubber tip sealing container, under magnetic stirring, into container, injection is dissolved with the acetonitrile of p-methyl benzenesulfonic acid iron, the mixed solution of dichloromethane, 6~10h of stirring reaction, obtains polymeric solution；Polymeric solution is poured into spray gun, and takes the ito glass of cleaning, is sprayed on the conducting surface of ito glass and produces the cerium titanyl cluster/poly- 3,4 ethene dioxythiophene laminated film.The laminated film of preparation can be applied in the fields such as smart window as electrochromic material.
Description
Technical field
The present invention relates to a kind of novel thin film, and in particular to a kind of cerium titanyl cluster/poly- 3,4-rthylene dioxythiophene THIN COMPOSITE
Film (Ce@TiO2/ PEDOT) film and preparation method and application.
Background technology
As a kind of new research field, it has had the advantage that for electrochromism：Suitable operating temperature range is big；Power consumption
It is small, easily matched with integrated circuit；Color tunable scope is very wide and can realize continuous discoloration；With memory function, change colour and opening
It can still be kept in the state of road.
Cerium titanyl cluster belongs to a kind of multi-metal oxygen cluster, and the thulium in its structure is filled in transition metal
In the omission of its anion.Its structure will not change upon dissolution, and especially for organic polar solvent, its structure will not change
The characteristics of make it that its application is wider.Multi-metal oxygen cluster has excellent photoelectric property, electrochemical properties and electrochromism
Matter, its electrochromism mechanism are when a sufficiently large voltage is applied, electronics, metal ion to be injected on the unoccupied orbital of metal ion
Lower valency is changed into from high-valence state, color changes；When applied voltage changes, metal ion loses electronics, metal ion by
Lower valency returns to high-valence state, and color reverts to the color of script.
3,4-rthylene dioxythiophene (EDOT) is as a kind of common conducting polymer monomer, its polymer (PEDOT) tool
Some conductances are high, and stability is good, and contrast is big, fast response time, it is seen that the features such as light transmission rate is high, becomes electroluminescent change
The focus of color research field.
The content of the invention
It is an object of the invention to provide a kind of simple method to prepare cerium titanyl cluster/poly- 3 with excellent photoelectric properties,
4- ethene dioxythiophene laminated films.
The present invention adopts the following technical scheme that to solve technical problem：
A kind of cerium titanyl cluster/poly- 3,4-rthylene dioxythiophene laminated film, the preparation method of the laminated film include with
Lower step：
(1) cerium titanyl cluster is prepared using hydrothermal synthesis method：Tetraethyl titanate, anhydrous cerium chloride and absolute ethyl alcohol are added into table
Face is scribbled in the inner bag of polytetrafluoroethylene (PTFE), then described inner bag is put into hydrothermal reaction kettle, anti-at a temperature of 100~200 DEG C
Answer 48~96 hours, after described inner bag taking-up reactor is cooled into room temperature afterwards, obtain orange-red solution, will be orange red molten
Liquid takes out from described inner bag, stands slow solvent flashing at room temperature, red crystals are obtained after 30~60 days, is described
Cerium titanyl cluster；The volume ratio of the tetraethyl titanate and absolute ethyl alcohol is 1:1~4；The amount of the anhydrous cerium chloride material is with titanium
The volume of sour tetra-ethyl ester is calculated as 0.05~0.15mmol/mL；
(2)Ce@TiO2/ PEDOT chemical polymerizations：To be pre-loaded with the container of acetonitrile and dichloromethane add 3,4- ethene
Cerium titanyl cluster prepared by dioxy thiophene, step (1), obtains initial soln, sealing container, under magnetic stirring, is noted into container
Enter acetonitrile, the mixed solution of dichloromethane dissolved with p-methyl benzenesulfonic acid iron, 6~10h of stirring reaction, obtain polymeric solution；
(3)Ce@TiO2The preparation of/PEDOT films：The polymeric solution obtained in (2) is poured into spray gun, and takes cleaning
Ito glass, it is sprayed on the conducting surface of ito glass and produces the cerium titanyl cluster/poly- 3,4-rthylene dioxythiophene THIN COMPOSITE
Film.
Further, the mass ratio of 3,4-rthylene dioxythiophene described in step (2) and cerium titanyl cluster is 1~2:1, be preferably
1:1。
Further, the body of acetonitrile and dichloromethane in the container of acetonitrile and dichloromethane is pre-loaded with described in step (2)
Product is than being 1~2:1, preferably 1:1.
Further, the cumulative volume of acetonitrile and dichloromethane is pre-loaded with described in step (2) with 3,4-rthylene dioxythiophene
Quality be calculated as 80~120mL/g, preferably 110mL/g.
Further, described in step (2) dissolved with the acetonitrile of p-methyl benzenesulfonic acid iron, the mixed solution of dichloromethane to toluene
Sulfonic acid iron is solute, and concentration is 0.01~0.02g/mL, preferably 0.01g/ml, and acetonitrile and dichloromethane are solvent, both bodies
Product is than being 1~2:1, preferably 1:1.
Further, the volume ratio of mixed solution and initial soln described in step (2) is 1~2:1, preferably 1:1.
Further, the speed in the injection of mixed solution described in step (2) container is 1~5mL/min, preferably 2.5ml/
min。
Further, the stirring reaction time described in step (2) is 6~10h, preferably 8h.
Further, the present invention provides described cerium titanyl cluster/poly- 3,4-rthylene dioxythiophene laminated film as electroluminescent change
The application of color material.
The present invention characterizes the surface topography of laminated film by ESEM (SEM), passes through uv-visible absorption spectroscopy
Its photophysical property is characterized, its electrochromism and stability are characterized by electrochemical workstation.
Compared with prior art, the beneficial effects are mainly as follows：
(1) preparation method of the present invention is simple and easy, it is not necessary to exacting terms.
(2) spraying and electrochemical polymerization method make it that the laminated film of gained is uniform and stable used by.
(3) there is the laminated film obtained by excellent electrochromic property can be used for the fields such as smart window.
Brief description of the drawings
Fig. 1 is that the SEM of laminated film made from embodiment 1 schemes.
Fig. 2 is the UV absorption figure of laminated film made from embodiment 1.
Fig. 3 is the contrast figure of laminated film made from embodiment 1.
Fig. 4 is the cyclical stability figure of laminated film made from embodiment 1.
Fig. 5 is electrochromism color diagram of the laminated film made from embodiment 1 under -1V voltages.
Fig. 6 is electrochromism color diagram of the laminated film made from embodiment 1 under 2V voltages.
Embodiment
With reference to specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in
This.
Embodiment 1
(1) cerium titanyl cluster is prepared using hydrothermal synthesis method：By tetraethyl titanate 3.5ml, anhydrous cerium chloride 1mmol
(0.246g), absolute ethyl alcohol 7ml are added in the inner bag of polytetrafluoroethylene (PTFE), are placed into hydrothermal reaction kettle, be put into baking oven with 150
DEG C reaction three days, afterwards take out reactor be cooled to room temperature after can obtain orange-red solution.By orange-red solution from inner bag
Taking-up is placed in sample bottle, stands slow solvent flashing at room temperature, and red crystals, as cerium titanyl are can obtain after the several months
Cluster.
(2)Ce@TiO2/ PEDOT chemical polymerizations：0.5gEDOT, 20ml are added into the round-bottomed flask equipped with 20ml acetonitriles
Dichloromethane, 0.55g cerium titanyl clusters and rotor, stirring is opened after being sealed with rubber tip, with about 2.5ml/min speed to flask
Interior injection 50ml p-methyl benzenesulfonic acid iron acetonitrile dichloromethane mixed solution, wherein acetonitrile 25ml, dichloromethane 25ml, to toluene sulphur
Sour iron 1g, stirring reaction 8 hours.
(3)Ce@TiO2The preparation of/PEDOT films：The polymeric solution obtained in (2) is poured into spray gun, and takes cleaning
Ito glass, it is sprayed on the conducting surface of ito glass and produces Ce@TiO2/ PEDOT films.
SEM tests are carried out to laminated film prepared by embodiment 1, such as Fig. 1, illustrate that cerium titanyl cluster and PEDOT successes are compound.
The ultraviolet test of three-electrode system is carried out to laminated film prepared by embodiment 1, such as Fig. 2, illustrates that laminated film is true
Real storage is in electrochromism phenomenon.
The contrast that three-electrode system is carried out to laminated film prepared by embodiment 1 is tested, and such as Fig. 3, illustrates laminated film
Change color contrast it is higher.
The cyclic voltammetric stability test of three-electrode system, such as Fig. 4, explanation are carried out to laminated film prepared by embodiment 1
Laminated film has certain cyclical stability.
Three-electrode system：Working electrode is the ito glass for being loaded with laminated film, is platinum electrode to electrode, reference electrode
For Ag/AgCl electrodes, the electrolyte used is the dichloromethane solution of 1mol/L tetrabutyl ammonium hexafluorophosphate.
Embodiment 2
(1) step is the same as embodiment 1.
(2)Ce@TiO2/ PEDOT chemical polymerizations：0.5gEDOT, 20ml are added into the round-bottomed flask equipped with 20ml acetonitriles
Dichloromethane, 0.56g cerium titanyl clusters and rotor, stirring is opened after being sealed with rubber tip, with about 5ml/min speed into flask
Inject 50ml p-methyl benzenesulfonic acid iron acetonitrile dichloromethane mixed solutions, wherein acetonitrile 25ml, dichloromethane 25ml, p-methyl benzenesulfonic acid
Iron 1g, stirring reaction 8 hours.
(3) step is the same as embodiment 1.
Embodiment 3
(1) step is the same as embodiment 1.
(2)Ce@TiO2/ PEDOT chemical polymerizations：0.5g EDOT, 20ml are added into the round-bottomed flask equipped with 20ml acetonitriles
Dichloromethane, 0.56g cerium titanyl clusters and rotor, stirring is opened after being sealed with rubber tip, with about 1ml/min speed into flask
Inject 50ml p-methyl benzenesulfonic acid iron acetonitrile dichloromethane mixed solutions, wherein acetonitrile 25ml, dichloromethane 25ml, p-methyl benzenesulfonic acid
Iron 1g, stirring reaction 8 hours.
(3) step is the same as embodiment 1.
Embodiment 4
(1) step is the same as embodiment 1.
(2)Ce@TiO2/ PEDOT chemical polymerizations：0.5gEDOT, 20ml are added into the round-bottomed flask equipped with 20ml acetonitriles
Dichloromethane, 0.56g cerium titanyl clusters and rotor, stirring is opened after being sealed with rubber tip, with about 2.5ml/min speed to flask
Interior injection 50ml p-methyl benzenesulfonic acid iron acetonitrile dichloromethane mixed solution, wherein acetonitrile 25ml, dichloromethane 25ml, to toluene sulphur
Sour iron 1g, stirring reaction 6 hours.
(3) step is the same as embodiment 1.
Embodiment 5
(1) step is the same as embodiment 1
(2)Ce@TiO2/ PEDOT chemical polymerizations：0.5gEDOT, 20ml are added into the round-bottomed flask equipped with 20ml acetonitriles
Dichloromethane, 0.56g cerium titanyl clusters and rotor, stirring is opened after being sealed with rubber tip, with about 2.5ml/min speed to flask
Interior injection 50ml p-methyl benzenesulfonic acid iron acetonitrile dichloromethane mixed solution, wherein acetonitrile 25ml, dichloromethane 25ml, to toluene sulphur
Sour iron 1g, stirring reaction 8 hours.
(3) step is the same as embodiment 1.
Embodiment 6
(1) cerium titanyl cluster is prepared using hydrothermal synthesis method：By tetraethyl titanate 3.5ml, anhydrous cerium chloride 1mmol is anhydrous
Ethanol 14ml is added in the inner bag of polytetrafluoroethylene (PTFE), is placed into hydrothermal reaction kettle, is put into baking oven and is reacted three days with 150 DEG C,
Orange-red solution can be obtained by taking out afterwards after reactor is cooled to room temperature.Orange-red solution is taken out from inner bag and is placed in sample
In bottle, slow solvent flashing at room temperature is stood, red crystals, as cerium titanyl cluster are can obtain after the several months.
(2) step is the same as embodiment 1
(3) step is the same as embodiment 1
Embodiment 7
(1) cerium titanyl cluster is prepared using hydrothermal synthesis method：By tetraethyl titanate 3.5ml, anhydrous cerium chloride 1mmol is anhydrous
Ethanol 7ml is added in the inner bag of polytetrafluoroethylene (PTFE), is placed into hydrothermal reaction kettle, is put into baking oven and is reacted three days with 100 DEG C, it
Orange-red solution can be obtained by taking out afterwards after reactor is cooled to room temperature.Orange-red solution is taken out from inner bag and is placed in sample bottle
In, slow solvent flashing at room temperature is stood, red crystals, as cerium titanyl cluster are can obtain after the several months.
(2) step is the same as embodiment 1
(3) step is the same as embodiment 1
Embodiment 8
(1) cerium titanyl cluster is prepared using hydrothermal synthesis method：By tetraethyl titanate 3.5ml, anhydrous cerium chloride 1mmol is anhydrous
Ethanol 7ml is added in the inner bag of polytetrafluoroethylene (PTFE), is placed into hydrothermal reaction kettle, is put into baking oven and is reacted three days with 200 DEG C, it
Orange-red solution can be obtained by taking out afterwards after reactor is cooled to room temperature.Orange-red solution is taken out from inner bag and is placed in sample bottle
In, slow solvent flashing at room temperature is stood, red crystals, as cerium titanyl cluster are can obtain after the several months.
(2) step is the same as embodiment 1
(3) step is the same as embodiment 1
Embodiment 9
(1) step is the same as embodiment 1.
(2)Ce@TiO2/ PEDOT chemical polymerizations：0.3g EDOT, 20ml are added into the round-bottomed flask equipped with 20ml acetonitriles
Dichloromethane, 0.3g cerium titanyl clusters and rotor, stirring is opened after being sealed with rubber tip, with about 2.5ml/min speed to flask
Interior injection 50ml p-methyl benzenesulfonic acid iron acetonitrile dichloromethane mixed solution, wherein acetonitrile 25ml, dichloromethane 25ml, to toluene sulphur
Sour iron 1g, stirring reaction 8 hours.
(3) step is the same as embodiment 1.
Embodiment 10
(1) step is the same as embodiment 1.
(2)Ce@TiO2/ PEDOT chemical polymerizations：0.5g EDOT, 13ml are added into the round-bottomed flask equipped with 26ml acetonitriles
Dichloromethane, 0.56g cerium titanyl clusters and rotor, stirring is opened after being sealed with rubber tip, with about 2,5ml/min speed to flask
Interior injection 50ml p-methyl benzenesulfonic acid iron acetonitrile dichloromethane mixed solution, wherein acetonitrile 25ml, dichloromethane 25ml, to toluene sulphur
Sour iron 1g, stirring reaction 8 hours.
(3) step is the same as embodiment 1.
Embodiment 11
(1) step is the same as embodiment 1.
(2)Ce@TiO2/ PEDOT chemical polymerizations：0.5gEDOT, 20ml are added into the round-bottomed flask equipped with 20ml acetonitriles
Dichloromethane, 0.25g cerium titanyl clusters and rotor, stirring is opened after being sealed with rubber tip, with about 2.5ml/min speed to flask
Interior injection 50ml p-methyl benzenesulfonic acid iron acetonitrile dichloromethane mixed solution, wherein acetonitrile 25ml, dichloromethane 25ml, to toluene sulphur
Sour iron 1g, stirring reaction 8 hours.
(3) step is the same as embodiment 1.
Embodiment 12
(1) step is the same as embodiment 1.
(2)Ce@TiO2/ PEDOT chemical polymerizations：0.5gEDOT, 20ml are added into the round-bottomed flask equipped with 20ml acetonitriles
Dichloromethane, 0.56g cerium titanyl clusters and rotor, stirring is opened after being sealed with rubber tip, with about 2.5ml/min speed to flask
Interior injection 50ml p-methyl benzenesulfonic acid iron acetonitrile dichloromethane mixed solution, wherein acetonitrile 33ml, dichloromethane 17ml, to toluene sulphur
Sour iron 1g, stirring reaction 8 hours.
(3) step is the same as embodiment 1.
Embodiment 13
(1) step is the same as embodiment 1.
(2)Ce@TiO2/ PEDOT chemical polymerizations：0.5gEDOT, 20ml are added into the round-bottomed flask equipped with 20ml acetonitriles
Dichloromethane, 0.56g cerium titanyl clusters and rotor, stirring is opened after being sealed with rubber tip, with about 2.5ml/min speed to flask
Interior injection 50ml p-methyl benzenesulfonic acid iron acetonitrile dichloromethane mixed solution, wherein acetonitrile 25ml, dichloromethane 25ml, to toluene sulphur
Sour iron 0.5g, stirring reaction 8 hours.
(3) step is the same as embodiment 1.
Embodiment 14
(1) cerium titanyl cluster is prepared using hydrothermal synthesis method：By tetraethyl titanate 7ml, anhydrous cerium chloride 1mmol, anhydrous second
Alcohol 7ml add polytetrafluoroethylene (PTFE) inner bag in, place into hydrothermal reaction kettle, be put into baking oven with 150 DEG C react three days, afterwards
Orange-red solution can be obtained by taking out after reactor is cooled to room temperature.Orange-red solution is taken out from inner bag and is placed in sample bottle
In, slow solvent flashing at room temperature is stood, red crystals, as cerium titanyl cluster are can obtain after the several months.
(2) step is the same as embodiment 1
(3) step is the same as embodiment 1.
Claims (9)
- A kind of 1. cerium titanyl cluster/poly- 3,4-rthylene dioxythiophene laminated film, it is characterised in that the preparation side of the laminated film Method comprises the following steps：(1) cerium titanyl cluster is prepared using hydrothermal synthesis method：Tetraethyl titanate, anhydrous cerium chloride and absolute ethyl alcohol are added into surface to apply Have in the inner bag of polytetrafluoroethylene (PTFE), then described inner bag is put into hydrothermal reaction kettle, react 48 at a temperature of 100~200 DEG C ~96 hour, described inner bag is taken out after reactor is cooled to room temperature afterwards, obtains orange-red solution, by orange-red solution from Taken out in described inner bag, stand slow solvent flashing at room temperature, red crystals are obtained after 30~60 days, as described cerium titanium Oxygen cluster；The volume ratio of the tetraethyl titanate and absolute ethyl alcohol is 1:1~4；The amount of the anhydrous cerium chloride material is with metatitanic acid four The volume of ethyl ester is calculated as 0.142~0.285mmol/mL；(2)Ce@TiO2/ PEDOT chemical polymerizations：To be pre-loaded with the container of acetonitrile and dichloromethane add 3,4- ethylene dioxies Cerium titanyl cluster prepared by thiophene, step (1), obtains initial soln, sealing container, under magnetic stirring, is injected into container molten There are acetonitrile, the mixed solution of dichloromethane of p-methyl benzenesulfonic acid iron, 6~10h of stirring reaction, obtain polymeric solution；(3)Ce@TiO2The preparation of/PEDOT films：The polymeric solution obtained in (2) is poured into spray gun, and takes the ITO glass of cleaning Glass, it is sprayed on the conducting surface of ito glass and produces the cerium titanyl cluster/poly- 3,4-rthylene dioxythiophene laminated film.
- 2. laminated film as claimed in claim 1, it is characterised in that：3,4- ethene dioxythiophenes and cerium described in step (2) The mass ratio of titanyl cluster is 1~2:1.
- 3. laminated film as claimed in claim 1, it is characterised in that：Step is pre-loaded with acetonitrile and dichloromethane described in (2) The volume ratio of acetonitrile and dichloromethane is 1~2 in the container of alkane:1.
- 4. laminated film as claimed in claim 1, it is characterised in that：The cumulative volume for being pre-loaded with acetonitrile and dichloromethane 80~120mL/g is calculated as with the quality of 3,4- ethene dioxythiophenes.
- 5. laminated film as claimed in claim 1, it is characterised in that：Dissolved with the second of p-methyl benzenesulfonic acid iron described in step (2) Nitrile, dichloromethane mixed solution in p-methyl benzenesulfonic acid iron be solute, concentration is 0.01~0.02g/mL, acetonitrile and dichloromethane For solvent, both volume ratios are 1~2:1.
- 6. laminated film as claimed in claim 1, it is characterised in that：Mixed solution described in step (2) and initial soln Volume ratio is 1~2:1.
- 7. laminated film as claimed in claim 1, it is characterised in that：Speed in mixed solution injection container for 1~ 5mL/min。
- 8. laminated film as claimed in claim 1, it is characterised in that：3,4- ethene dioxythiophenes and cerium described in step (2) The mass ratio of titanyl cluster is 1:1.
- 9. application of the laminated film as claimed in claim 1 as electrochromic material.
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| US20070153355A1 (en) * | 2005-12-29 | 2007-07-05 | Industrial Technology Research Institute | Electrochromic film |
| CN101210090A (en) * | 2007-12-24 | 2008-07-02 | 重庆弈派因化工产品有限公司 | Method for preparing polyaniline/polystyrene sulfonic acid-polyvinyl alcohol electrochromism film |
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