CN101968594A - Electrochromic device containing polyaniline composite nanofiber membrane and preparation method thereof - Google Patents
Electrochromic device containing polyaniline composite nanofiber membrane and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an electrochromic device containing a polyaniline composite nanofiber membrane and a preparation method thereof. The electrochromic device is characterized by comprising an epoxy resin sealing layer, a conducting glass layer, the polyaniline composite nanofiber membrane, a gel electrolyte layer and a DC stabilized power supply. The preparation method comprises the following specific steps of: stirring and dissolving polyaniline in a solvent at a room temperature, adding a polymer blend to obtain a polyaniline electrospinning blending solution; electrospinning under certain temperature, humidity and voltage conditions to prepare nanofibers, depositing the nanofibers on conducting glass, coating an gel electrolyte, covering conducting glass with the same size, and connecting with a conducting wire; and finally sealing with epoxy resin to obtain the electrochromic device. The electrochromic device has the advantages of low cost, rapid electrochromic response, wide color change interval and good repeatability, the equipment is simple.
Description
Technical field
The present invention relates to a kind of electrochromic device that contains the polyaniline composite nano-fiber membrane and preparation method thereof, belong to colour change function material technology field.
Background technology
Electrochromism (Electrochromism) is meant under impressed current or effect of electric field, the optical property of material (transmissivity, reflectivity, absorptivity and emissivity etc.) produces stable reversible variation in visible wavelength range, show as the reversible variation of optical properties such as color in appearance.Electrochromic material can be divided into inorganic material and organic material generally, and the latter is divided into organic small molecule material and conducting polymer materials again.The research of early stage electrochromic material mainly concentrates on inorganic material and organic small molecule material, but all there is defective in they at the aspects such as processibility, compatibility and colour rendering of material.Conducting polymer is as a kind of novel electrochromic material, existing metal and semi-conductive photoelectric property, have the mechanical property and the processibility of polymers flexible again concurrently, have more superior coloration efficiency and fast the response time change color have a wide reach, and be easy to preparation, become a new focus of electrochromic material research field gradually.At aspects such as smart window, camouflage clothes, a new generation's no visual angle restriction display devices great application potential is arranged.In numerous conducting polymers, polyaniline is owing to raw material is easy to get, synthetic easy, high temperature resistant and advantages such as antioxygenic property good, Heat stability is good, mechanism of doping effect uniqueness are subjected to paying close attention to widely, be generally acknowledge at present have one of electrochromic conducting macromolecular material of application potential most.But because the existence of benzene ring structure on the polyaniline molecule main chain, strand has stronger rigidity and chain interphase interaction, make that its dissolubility and film forming are poor, corresponding processing characteristics also is affected, existing polyaniline nano membrane material mechanical strength is relatively poor, be difficult to form homogeneous system, it is inhomogeneous to develop the color, and has limited it in the electrochromism broad application.
Summary of the invention
The purpose of this invention is to provide a kind of electrochromic device that contains the polyaniline composite nano-fiber membrane and preparation method thereof with good mechanical properties, discoloration.
In order to achieve the above object, the invention provides a kind of electrochromic device that contains the polyaniline composite nano-fiber membrane, it is characterized in that, comprise following electro-conductive glass, polyaniline composite nano fiber layer, the gel electrolyte layer that sets gradually from top to bottom and go up electro-conductive glass, the outside of polyaniline composite nano fiber layer and gel electrolyte layer is provided with the epoxy sealing layer, and the positive pole of D.C. regulated power supply connects electro-conductive glass, negative pole connection down and goes up electro-conductive glass.
The present invention also provides the above-mentioned preparation method who contains the electrochromic device of polyaniline composite nano-fiber membrane, it is characterized in that, concrete steps are:
The first step: at ambient temperature, in stirred tank the polyaniline in eigenstate raw material is dissolved in the solvent, speed of agitator is 50-200rpm, obtains the polyaniline solutions that massfraction is 0.2%-15%; The blending polymkeric substance is joined in the polyaniline solutions, speed of agitator is 200-1000rpm, mixes again, and obtains the blending solution that blending polymer quality mark is 0.5%-30%; In room temperature and relative humidity is under the condition of 20%-60%, the flow velocity of blending solution with 0.1-4mL/h is input on the spinning head, simultaneously spinning head is connected the 10-40KV power supply and carry out electrostatic spinning, electro-conductive glass is as receiving trap under adopting, distance between receiving trap and the spinning head is 5-30cm, nano fibrous membrane dry 1-12 h in 25-80 ℃ of vacuum with depositing on the following electro-conductive glass promptly obtains the polyaniline composite nano-fiber membrane;
Second step: with propylene carbonate and vinyl carbonate by volume 1:1 evenly mix, use the 4A molecular sieve drying, the high chloro acid dissolution is configured to the homogeneous solution that concentration is 0.15mol/L in acetonitrile, use the 4A molecular sieve drying, in beaker, add the propylene carbonate-vinyl carbonate mixed solution of 2 weight portions, the perchloric acid-acetonitrile solution of 7 weight portions, the polymethylmethacrylate of 0.7 weight portion, the lithium perchlorate of 0.3 weight portion successively, mix, obtain gelatinous electrolyte;
The 3rd step: the second gelatinous electrolyte that obtain of step is coated on the polyaniline composite nano-fiber membrane that the first step obtains uniformly forms gel electrolyte layer, cover electro-conductive glass again, electro-conductive glass is to get rid of the bubble in the gel electrolyte layer in the extruding, to go up electro-conductive glass and be connected lead respectively with following electro-conductive glass, with epoxy resin the entire device sealing is formed the epoxy sealing layer, last electro-conductive glass is linked to each other with anodal with the negative pole of D.C. regulated power supply respectively with following electro-conductive glass, promptly obtain containing the electrochromic device of polyaniline composite nano-fiber membrane.
The solvent of the described first step is formic acid, trifluoroacetic acid, perfluoro caprylic acid, hexafluoroisopropanol, N-Methyl pyrrolidone, N, the potpourri of one or more in dinethylformamide, N,N-dimethylacetamide, tetrahydrofuran, dimethyl sulfoxide (DMSO), methenyl choloride, ethanol and the methylene chloride.
Blending polymkeric substance in the described first step is nylon 6, polymethylmethacrylate, polyvinyl alcohol (PVA), polyacrylamide, cellulose acetate, ethyl cellulose, polyacrylic acid, polyacrylonitrile, the potpourri of one or more in polyoxyethylene, PLA and the polyvinylpyrrolidone.
Advantage compared with prior art of the present invention is as follows:
(1) the present invention spins static silk technology by solution blending, has realized that the homogeneous phase of polyaniline and blending polymkeric substance is blended into fibre.Mix by polyaniline and blending component in the nano-composite fiber film of this method preparation, do not have the situation that is separated and take place.Therefore improve the mechanical property of polyaniline nano film greatly, demonstrated fabulous pliability.Polyaniline molecule is dispersed in the nano fibrous membrane uniformly, makes the tunica fibrosa colour developing evenly, the color saturation height.
(2) electrochromic device employing polyaniline composite nano-fiber membrane provided by the invention is an off-color material, specific surface area than common solid membrane improves 1-2 the order of magnitude, make electrolyte bigger contact area be arranged with polyaniline, help the ionic charge transmission in the electrochemical reaction process, the variable color response speed is faster, good reproducibility.
(3) the invention provides the electrochromic device discoloration test result that contains the polyaniline composite nano-fiber membrane is: in volt-ampere scan round test, when adding current potential from-0.7V to the 1.2V change procedure, can observe the device color and present successively from the change procedure of pale yellow-light yellow green-light green-light blue-blueness-bluish violet-purple.20 circulations of accordion seek, device color are significantly decay not, has good repeatability.
Description of drawings
Fig. 1 is the electrochromic device structural representation that contains the polyaniline composite nano-fiber membrane.
Embodiment
Below in conjunction with embodiment, further set forth the present invention.Polyaniline in following examples can Co., Ltd buy in Sigma; Spinning can buy in Shanghai crystalline substance pure reagent company limited with blending polymkeric substance and reagent; High-voltage power supply is the DW-P303-1ACD8 type that east, Tianjin civilian high-voltage power supply factory produces; Transfusion system is the LSP02-113 type that Baoding LanGe constant flow pump Co., Ltd produces; D.C. regulated power supply is the E3614A type that Anjelen Sci. ﹠ Tech. Inc produces.Last electro-conductive glass and following electro-conductive glass are the ITO electro-conductive glass, and manufacturer is auspicious grace Tyke, a Beijing Electron Technology Co., Ltd.
As shown in Figure 1, for containing the electrochromic device structural representation of polyaniline composite nano-fiber membrane, the described electrochromic device that contains the polyaniline composite nano-fiber membrane, comprise following electro-conductive glass 2a, polyaniline composite nano fiber layer 3, the gel electrolyte layer 4 that sets gradually from top to bottom and go up electro-conductive glass 2b, the outside of polyaniline composite nano fiber layer 3 and gel electrolyte layer 4 is provided with epoxy sealing layer 1, and the positive pole of D.C. regulated power supply 5 connects electro-conductive glass 2a, negative pole connection down and goes up electro-conductive glass 2b.Its preparation method is as follows:
Under 25 ℃ of conditions of room temperature, in stirred tank with 0.02g polyaniline (molecular weight 65000) with rotating speed 50rpm stirring and dissolving in 9.93g formic acid and acetate mixed solvent (weight ratio is 5:1), after treating that polyaniline dissolves fully, in solution, add 0.05g polyacrylamide (molecular weight 2000000), 200rpm stirs with rotating speed, obtains the polyaniline massfraction and be 0.2%, the polyacrylamide massfraction is 0.5% co-blended spinning solution.Under the condition of 25 ℃ of room temperatures, humidity 30%, the flow velocity of co-blended spinning solution with 1.5mL/h is input on the spinning head, simultaneously spinning head is connected the 20kV power supply and carry out electrostatic spinning and prepare polyaniline/polyacrylamide blended nanofibre; To following electro-conductive glass 2a, the distance between following electro-conductive glass 2a and the spinning head is 10cm with spun fiber laydown; After treating that spinning is finished, will descend electro-conductive glass 2a to put into vacuum drying oven with 40 ℃ of dry 4h.With propylene carbonate and vinyl carbonate by volume 1:1 evenly mix, use the 4A molecular sieve drying.The high chloro acid dissolution is configured to the homogeneous solution that concentration is 0.15mol/L in acetonitrile, uses the 4A molecular sieve drying.In beaker, add 2g propylene carbonate-vinyl carbonate mixed solution, 7g perchloric acid-acetonitrile solution, 0.7g polymethylmethacrylate, 0.3g lithium perchlorate successively, mix gel.Gel electrolyte is coated on the polyaniline composite nano-fiber membrane uniformly, covers the last electro-conductive glass 2b of same size again, get rid of the bubble in the electrolyte.Electro-conductive glass is continuous up and down together respectively with lead, and with epoxy resin entire device is sealed, and lead is connected to constant voltage dc source, promptly gets required electrochromic device.The volt-ampere loop test shows that current potential, can be observed the device color and present successively from the change procedure of pale yellow-light yellow green-light green-light blue-blueness-bluish violet-purple from-0.7V to the 1.2V change procedure.20 circulations of accordion seek, device color are obviously decay not.
Embodiment 2
As shown in Figure 1, for containing the electrochromic device structural representation of polyaniline composite nano-fiber membrane, the described electrochromic device that contains the polyaniline composite nano-fiber membrane, comprise following electro-conductive glass 2a, polyaniline composite nano fiber layer 3, the gel electrolyte layer 4 that sets gradually from top to bottom and go up electro-conductive glass 2b, the outside of polyaniline composite nano fiber layer 3 and gel electrolyte layer 4 is provided with epoxy sealing layer 1, and the positive pole of D.C. regulated power supply 5 connects electro-conductive glass 2a, negative pole connection down and goes up electro-conductive glass 2b.Its preparation method is as follows:
Under 25 ℃ of conditions of room temperature, in stirred tank with 0.5g polyaniline (molecular weight 65000) with rotating speed 100rpm stirring and dissolving in 8.5g formic acid, after treating that polyaniline dissolves fully, in solution, add 1g ethyl cellulose (molecular weight 200000), 400rpm stirs with rotating speed, obtains the polyaniline massfraction and be 5%, the ethyl cellulose massfraction is 10% co-blended spinning solution.Under the condition of 25 ℃ of room temperatures, humidity 42%, the flow velocity of co-blended spinning solution with 1.2mL/h is input on the spinning head, simultaneously spinning head is connected the 18kV power supply and carry out electrostatic spinning and prepare polyaniline/ethyl cellulose blended nanofibre; To following electro-conductive glass 2a, the distance between following electro-conductive glass 2a and the spinning head is 15cm with spun fiber laydown; After treating that spinning is finished, will descend electro-conductive glass 2a to put into vacuum drying oven with 40 ℃ of dry 4h.With propylene carbonate and vinyl carbonate by volume 1:1 evenly mix, use the 4A molecular sieve drying.The high chloro acid dissolution is configured to the homogeneous solution that concentration is 0.15mol/L in acetonitrile, uses the 4A molecular sieve drying.In beaker, add 2g propylene carbonate-vinyl carbonate mixed solution, 7g perchloric acid-acetonitrile solution, 0.7g polymethylmethacrylate, 0.3g lithium perchlorate successively, mix gel.Gel electrolyte is coated on the polyaniline composite nano-fiber membrane uniformly, covers the last electro-conductive glass 2b of same size again, get rid of the bubble in the electrolyte.Electro-conductive glass is continuous up and down together respectively with lead, and with epoxy resin entire device is sealed, and lead is connected to constant voltage dc source, promptly gets required electrochromic device.The volt-ampere loop test shows that current potential, can be observed the device color and present successively from the change procedure of pale yellow-light yellow green-light green-light blue-blueness-bluish violet-purple from-0.7V to the 1.2V change procedure.20 circulations of accordion seek, device color are obviously decay not.
As shown in Figure 1, for containing the electrochromic device structural representation of polyaniline composite nano-fiber membrane, the described electrochromic device that contains the polyaniline composite nano-fiber membrane, comprise following electro-conductive glass 2a, polyaniline composite nano fiber layer 3, the gel electrolyte layer 4 that sets gradually from top to bottom and go up electro-conductive glass 2b, the outside of polyaniline composite nano fiber layer 3 and gel electrolyte layer 4 is provided with epoxy sealing layer 1, and the positive pole of D.C. regulated power supply 5 connects electro-conductive glass 2a, negative pole connection down and goes up electro-conductive glass 2b.Its preparation method is as follows:
Under 25 ℃ of conditions of room temperature, in stirred tank with 1.5g polyaniline (molecular weight 65000) with rotating speed 200rpm stirring and dissolving in 7g formic acid and acetate mixed solvent (mass ratio is 10:1), after treating that polyaniline dissolves fully, in solution, add 1.5g nylon 6(molecular weight 180000), 500rpm stirs with rotating speed, obtains the polyaniline massfraction and be 15%, nylon 6 massfractions are 15% co-blended spinning solution.Under the condition of 25 ℃ of room temperatures, humidity 33%, the flow velocity of co-blended spinning solution with 0.4mL/h is input on the spinning head, simultaneously spinning head is connected the 30kV power supply and carry out electrostatic spinning and prepare polyaniline/nylon 6 blended nanofibres; To following electro-conductive glass 2a, the distance between following electro-conductive glass 2a and the spinning head is 16cm with spun fiber laydown; After treating that spinning is finished, will descend electro-conductive glass 2a to put into vacuum drying oven with 40 ℃ of dry 4h.With propylene carbonate and vinyl carbonate by volume 1:1 evenly mix, use the 4A molecular sieve drying.The high chloro acid dissolution is configured to the homogeneous solution that concentration is 0.15mol/L in acetonitrile, uses the 4A molecular sieve drying.In beaker, add 2g propylene carbonate-vinyl carbonate mixed solution, 7g perchloric acid-acetonitrile solution, 0.7g polymethylmethacrylate, 0.3g lithium perchlorate successively, mix gel.Gel electrolyte is coated on the polyaniline composite nano-fiber membrane uniformly, covers the last electro-conductive glass 2b of same size again, get rid of the bubble in the electrolyte.Electro-conductive glass is continuous up and down together respectively with lead, and with epoxy resin entire device is sealed, and lead is connected to constant voltage dc source, promptly gets required electrochromic device.The volt-ampere loop test shows that current potential, can be observed the device color and present successively from the change procedure of pale yellow-light yellow green-light green-light blue-blueness-bluish violet-purple from-0.7V to the 1.2V change procedure.20 circulations of accordion seek, device color are obviously decay not.
As shown in Figure 1, for containing the electrochromic device structural representation of polyaniline composite nano-fiber membrane, the described electrochromic device that contains the polyaniline composite nano-fiber membrane, comprise following electro-conductive glass 2a, polyaniline composite nano fiber layer 3, the gel electrolyte layer 4 that sets gradually from top to bottom and go up electro-conductive glass 2b, the outside of polyaniline composite nano fiber layer 3 and gel electrolyte layer 4 is provided with epoxy sealing layer 1, and the positive pole of D.C. regulated power supply 5 connects electro-conductive glass 2a, negative pole connection down and goes up electro-conductive glass 2b.Its preparation method is as follows:
Under 25 ℃ of conditions of room temperature, in stirred tank with 0.2g polyaniline (molecular weight 65000) with rotating speed 100rpm stirring and dissolving in 9.6g formic acid and alcohol mixed solvent (mass ratio is 8:1), after treating that polyaniline dissolves fully, in solution, add 0.2g polyoxyethylene (molecular weight 200000), 300rpm stirs with rotating speed, obtains the polyaniline massfraction and be 2%, the polyoxyethylene massfraction is 2% co-blended spinning solution.Under the condition of 25 ℃ of room temperatures, humidity 25%, the flow velocity of co-blended spinning solution with 0.8mL/h is input on the spinning head, simultaneously spinning head is connected the 16kV power supply and carry out electrostatic spinning and prepare polyaniline/polyoxyethylene blended nanofibre; To following electro-conductive glass 2a, the distance between following electro-conductive glass 2a and the spinning head is 10cm with spun fiber laydown; After treating that spinning is finished, will descend electro-conductive glass 2a to put into vacuum drying oven with 40 ℃ of dry 4h.With propylene carbonate and vinyl carbonate by volume 1:1 evenly mix, use the 4A molecular sieve drying.The high chloro acid dissolution is configured to the homogeneous solution that concentration is 0.15mol/L in acetonitrile, uses the 4A molecular sieve drying.In beaker, add 2g propylene carbonate-vinyl carbonate mixed solution, 7g perchloric acid-acetonitrile solution, 0.7g polymethylmethacrylate, 0.3g lithium perchlorate successively, mix gel.Gel electrolyte is coated on the polyaniline composite nano-fiber membrane uniformly, covers the last electro-conductive glass 2b of same size again, get rid of the bubble in the electrolyte.Electro-conductive glass is continuous up and down together respectively with lead, and with epoxy resin entire device is sealed, and lead is connected to constant voltage dc source, promptly gets required electrochromic device.The volt-ampere loop test shows that current potential, can be observed the device color and present successively from the change procedure of pale yellow-light yellow green-light green-light blue-blueness-bluish violet-purple from-0.7V to the 1.2V change procedure.20 circulations of accordion seek, device color are obviously decay not.
As shown in Figure 1, for containing the electrochromic device structural representation of polyaniline composite nano-fiber membrane, the described electrochromic device that contains the polyaniline composite nano-fiber membrane, comprise following electro-conductive glass 2a, polyaniline composite nano fiber layer 3, the gel electrolyte layer 4 that sets gradually from top to bottom and go up electro-conductive glass 2b, the outside of polyaniline composite nano fiber layer 3 and gel electrolyte layer 4 is provided with epoxy sealing layer 1, and the positive pole of D.C. regulated power supply 5 connects electro-conductive glass 2a, negative pole connection down and goes up electro-conductive glass 2b.Its preparation method is as follows:
Under 25 ℃ of conditions of room temperature, in stirred tank with 0.5g polyaniline (molecular weight 65000) with rotating speed 100rpm stirring and dissolving in 8.5g formic acid and trifluoroacetic acid mixed solvent (mass ratio is 8:1), after treating that polyaniline dissolves fully, in solution, add 1g cellulose acetate (molecular weight 30000), 600rpm stirs with rotating speed, obtains the polyaniline massfraction and be 5%, the cellulose acetate massfraction is 10% co-blended spinning solution.Under the condition of 25 ℃ of room temperatures, humidity 40%, the flow velocity of co-blended spinning solution with 4mL/h is input on the spinning head, simultaneously spinning head is connected the 10kV power supply and carry out electrostatic spinning and prepare polyaniline/acetyl cellulose blend nanofiber; To following electro-conductive glass 2a, the distance between following electro-conductive glass 2a and the spinning head is 15cm with spun fiber laydown; After treating that spinning is finished, will descend electro-conductive glass 2a to put into vacuum drying oven with 40 ℃ of dry 4h.With propylene carbonate and vinyl carbonate by volume 1:1 evenly mix, use the 4A molecular sieve drying.The high chloro acid dissolution is configured to the homogeneous solution that concentration is 0.15mol/L in acetonitrile, uses the 4A molecular sieve drying.In beaker, add 2g propylene carbonate-vinyl carbonate mixed solution, 7g perchloric acid-acetonitrile solution, 0.7g polymethylmethacrylate, 0.3g lithium perchlorate successively, mix gel.Gel electrolyte is coated on the polyaniline composite nano-fiber membrane uniformly, covers the last electro-conductive glass 2b of same size again, get rid of the bubble in the electrolyte.Electro-conductive glass is continuous up and down together respectively with lead, and with epoxy resin entire device is sealed, and lead is connected to constant voltage dc source, promptly gets required electrochromic device.The volt-ampere loop test shows that current potential, can be observed the device color and present successively from the change procedure of pale yellow-light yellow green-light green-light blue-blueness-bluish violet-purple from-0.7V to the 1.2V change procedure.20 circulations of accordion seek, device color are obviously decay not.
Embodiment 6
As shown in Figure 1, for containing the electrochromic device structural representation of polyaniline composite nano-fiber membrane, the described electrochromic device that contains the polyaniline composite nano-fiber membrane, comprise following electro-conductive glass 2a, polyaniline composite nano fiber layer 3, the gel electrolyte layer 4 that sets gradually from top to bottom and go up electro-conductive glass 2b, the outside of polyaniline composite nano fiber layer 3 and gel electrolyte layer 4 is provided with epoxy sealing layer 1, and the positive pole of D.C. regulated power supply 5 connects electro-conductive glass 2a, negative pole connection down and goes up electro-conductive glass 2b.Its preparation method is as follows:
Under 25 ℃ of conditions of room temperature, in stirred tank with 0.4g polyaniline (molecular weight 65000) with rotating speed 100rpm stirring and dissolving in 8.6g formic acid and hexafluoroisopropanol mixed solvent (mass ratio is 4:1), after treating that polyaniline dissolves fully, in solution, add 1g PLA (molecular weight 150000), 500rpm stirs with rotating speed, obtains the polyaniline massfraction and be 4%, the PLA massfraction is 10% co-blended spinning solution.Under the condition of 25 ℃ of room temperatures, humidity 50%, the flow velocity of co-blended spinning solution with 2mL/h is input on the spinning head, simultaneously spinning head is connected the 25kV power supply and carry out electrostatic spinning and prepare polyaniline/polylactic acid blend nanofiber; To following electro-conductive glass 2a, the distance between following electro-conductive glass 2a and the spinning head is 5cm with spun fiber laydown; After treating that spinning is finished, will descend electro-conductive glass 2a to put into vacuum drying oven with 40 ℃ of dry 4h.With propylene carbonate and vinyl carbonate by volume 1:1 evenly mix, use the 4A molecular sieve drying.The high chloro acid dissolution is configured to the homogeneous solution that concentration is 0.15mol/L in acetonitrile, uses the 4A molecular sieve drying.In beaker, add 2g propylene carbonate-vinyl carbonate mixed solution, 7g perchloric acid-acetonitrile solution, 0.7g polymethylmethacrylate, 0.3g lithium perchlorate successively, mix gel.Gel electrolyte is coated on the polyaniline composite nano-fiber membrane uniformly, covers the last electro-conductive glass 2b of same size again, get rid of the bubble in the electrolyte.Electro-conductive glass is continuous up and down together respectively with lead, and with epoxy resin entire device is sealed, and lead is connected to constant voltage dc source, promptly gets required electrochromic device.The volt-ampere loop test shows that current potential, can be observed the device color and present successively from the change procedure of pale yellow-light yellow green-light green-light blue-blueness-bluish violet-purple from-0.7V to the 1.2V change procedure.20 circulations of accordion seek, device color are obviously decay not.
Embodiment 7
As shown in Figure 1, for containing the electrochromic device structural representation of polyaniline composite nano-fiber membrane, the described electrochromic device that contains the polyaniline composite nano-fiber membrane, comprise following electro-conductive glass 2a, polyaniline composite nano fiber layer 3, the gel electrolyte layer 4 that sets gradually from top to bottom and go up electro-conductive glass 2b, the outside of polyaniline composite nano fiber layer 3 and gel electrolyte layer 4 is provided with epoxy sealing layer 1, and the positive pole of D.C. regulated power supply 5 connects electro-conductive glass 2a, negative pole connection down and goes up electro-conductive glass 2b.Its preparation method is as follows:
Under 25 ℃ of conditions of room temperature, in stirred tank with 0.6g polyaniline (molecular weight 65000) with rotating speed 100rpm stirring and dissolving in 8.4g formic acid and alcohol mixed solvent (mass ratio is 9:1), after treating that polyaniline dissolves fully, in solution, add 1g polymethylmethacrylate (molecular weight 700000), 1000rpm stirs with rotating speed, obtains the polyaniline massfraction and be 6%, the polymethylmethacrylate massfraction is 10% co-blended spinning solution.Under the condition of 25 ℃ of room temperatures, humidity 60%, the flow velocity of co-blended spinning solution with 4mL/h is input on the spinning head, simultaneously spinning head is connected the 40kV power supply and carry out electrostatic spinning and prepare polyaniline/polymethylmethacrylate blended nanofibre; To following electro-conductive glass 2a, the distance between following electro-conductive glass 2a and the spinning head is 30cm with spun fiber laydown; After treating that spinning is finished, will descend electro-conductive glass 2a to put into vacuum drying oven with 40 ℃ of dry 4h.With propylene carbonate and vinyl carbonate by volume 1:1 evenly mix, use the 4A molecular sieve drying.The high chloro acid dissolution is configured to the homogeneous solution that concentration is 0.15mol/L in acetonitrile, uses the 4A molecular sieve drying.In beaker, add 2g propylene carbonate-vinyl carbonate mixed solution, 7g perchloric acid-acetonitrile solution, 0.7g polymethylmethacrylate, 0.3g lithium perchlorate successively, mix gel.Gel electrolyte is coated on the polyaniline composite nano-fiber membrane uniformly, covers the last electro-conductive glass 2b of same size again, get rid of the bubble in the electrolyte.Electro-conductive glass is continuous up and down together respectively with lead, and with epoxy resin entire device is sealed, and lead is connected to constant voltage dc source, promptly gets required electrochromic device.The volt-ampere loop test shows that current potential, can be observed the device color and present successively from the change procedure of pale yellow-light yellow green-light green-light blue-blueness-bluish violet-purple from-0.7V to the 1.2V change procedure.20 circulations of accordion seek, device color are obviously decay not.
Embodiment 8
As shown in Figure 1, for containing the electrochromic device structural representation of polyaniline composite nano-fiber membrane, the described electrochromic device that contains the polyaniline composite nano-fiber membrane, comprise following electro-conductive glass 2a, polyaniline composite nano fiber layer 3, the gel electrolyte layer 4 that sets gradually from top to bottom and go up electro-conductive glass 2b, the outside of polyaniline composite nano fiber layer 3 and gel electrolyte layer 4 is provided with epoxy sealing layer 1, and the positive pole of D.C. regulated power supply 5 connects electro-conductive glass 2a, negative pole connection down and goes up electro-conductive glass 2b.Its preparation method is as follows:
Under 25 ℃ of conditions of room temperature, in stirred tank with 0.2g polyaniline (molecular weight 65000) with rotating speed 100rpm stirring and dissolving in 9g perfluoro caprylic acid and hexafluoroisopropanol mixed solvent (mass ratio is 1:3), after treating that polyaniline dissolves fully, in solution, add 0.8g polyacrylic acid (molecular weight 250000), 1000rpm stirs with rotating speed, obtains the polyaniline massfraction and be 2%, the polyacrylic acid massfraction is 8% co-blended spinning solution.Under the condition of 25 ℃ of room temperatures, humidity 40%, the flow velocity of co-blended spinning solution with 0.1mL/h is input on the spinning head, simultaneously spinning head is connected the 25kV power supply and carry out electrostatic spinning and prepare polyaniline/polyacrylic acid blended nanofibre; To following electro-conductive glass 2a, the distance between following electro-conductive glass 2a and the spinning head is 12cm with spun fiber laydown; After treating that spinning is finished, will descend electro-conductive glass 2a to put into vacuum drying oven with 40 ℃ of dry 4h.With propylene carbonate and vinyl carbonate by volume 1:1 evenly mix, use the 4A molecular sieve drying.The high chloro acid dissolution is configured to the homogeneous solution that concentration is 0.15mol/L in acetonitrile, uses the 4A molecular sieve drying.In beaker, add 2g propylene carbonate-vinyl carbonate mixed solution, 7g perchloric acid-acetonitrile solution, 0.7g polymethylmethacrylate, 0.3g lithium perchlorate successively, mix gel.Gel electrolyte is coated on the polyaniline composite nano-fiber membrane uniformly, covers the last electro-conductive glass 2b of same size again, get rid of the bubble in the electrolyte.Electro-conductive glass is continuous up and down together respectively with lead, and with epoxy resin entire device is sealed, and lead is connected to constant voltage dc source, promptly gets required electrochromic device.The volt-ampere loop test shows that current potential, can be observed the device color and present successively from the change procedure of pale yellow-light yellow green-light green-light blue-blueness-bluish violet-purple from-0.7V to the 1.2V change procedure.20 circulations of accordion seek, device color are obviously decay not.
Embodiment 9
As shown in Figure 1, for containing the electrochromic device structural representation of polyaniline composite nano-fiber membrane, the described electrochromic device that contains the polyaniline composite nano-fiber membrane, comprise following electro-conductive glass 2a, polyaniline composite nano fiber layer 3, the gel electrolyte layer 4 that sets gradually from top to bottom and go up electro-conductive glass 2b, the outside of polyaniline composite nano fiber layer 3 and gel electrolyte layer 4 is provided with epoxy sealing layer 1, and the positive pole of D.C. regulated power supply 5 connects electro-conductive glass 2a, negative pole connection down and goes up electro-conductive glass 2b.Its preparation method is as follows:
Under 25 ℃ of conditions of room temperature, in stirred tank with 0.8g polyaniline (molecular weight 65000) with rotating speed 100rpm stirring and dissolving in 8.4g formic acid and dimethyl sulfoxide (DMSO) mixed solvent (mass ratio is 6:1), after treating that polyaniline dissolves fully, in solution, add 0.8g polyvinyl alcohol (PVA) (molecular weight 200000), 500rpm stirs with rotating speed, obtains the polyaniline massfraction and be 8%, the polyvinyl alcohol (PVA) massfraction is 8% co-blended spinning solution.Under the condition of 25 ℃ of room temperatures, humidity 30%, the flow velocity of co-blended spinning solution with 1.8mL/h is input on the spinning head, simultaneously spinning head is connected the 25kV power supply and carry out electrostatic spinning and prepare the polyaniline/polyvinyl alcohol blended nanofibre; To following electro-conductive glass 2a, the distance between following electro-conductive glass 2a and the spinning head is 15cm with spun fiber laydown; After treating that spinning is finished, will descend electro-conductive glass 2a to put into vacuum drying oven with 40 ℃ of dry 4h.With propylene carbonate and vinyl carbonate by volume 1:1 evenly mix, use the 4A molecular sieve drying.The high chloro acid dissolution is configured to the homogeneous solution that concentration is 0.15mol/L in acetonitrile, uses the 4A molecular sieve drying.In beaker, add 2g propylene carbonate-vinyl carbonate mixed solution, 7g perchloric acid-acetonitrile solution, 0.7g polymethylmethacrylate, 0.3g lithium perchlorate successively, mix gel.Gel electrolyte is coated on the polyaniline composite nano-fiber membrane uniformly, covers the last electro-conductive glass 2b of same size again, get rid of the bubble in the electrolyte.Electro-conductive glass is continuous up and down together respectively with lead, and with epoxy resin entire device is sealed, and lead is connected to constant voltage dc source, promptly gets required electrochromic device.The volt-ampere loop test shows that current potential, can be observed the device color and present successively from the change procedure of pale yellow-light yellow green-light green-light blue-blueness-bluish violet-purple from-0.7V to the 1.2V change procedure.20 circulations of accordion seek, device color are obviously decay not.
Embodiment 10
As shown in Figure 1, for containing the electrochromic device structural representation of polyaniline composite nano-fiber membrane, the described electrochromic device that contains the polyaniline composite nano-fiber membrane, comprise following electro-conductive glass 2a, polyaniline composite nano fiber layer 3, the gel electrolyte layer 4 that sets gradually from top to bottom and go up electro-conductive glass 2b, the outside of polyaniline composite nano fiber layer 3 and gel electrolyte layer 4 is provided with epoxy sealing layer 1, and the positive pole of D.C. regulated power supply 5 connects electro-conductive glass 2a, negative pole connection down and goes up electro-conductive glass 2b.Its preparation method is as follows:
Under 25 ℃ of conditions of room temperature, in stirred tank with 0.4g polyaniline (molecular weight 65000) with rotating speed 100rpm stirring and dissolving in 8.1g formic acid and N-methyl pyrrolidone mixed solvent (mass ratio is 7:1), after treating that polyaniline dissolves fully, in solution, add 1g polyacrylonitrile (molecular weight 35000), 600rpm stirs with rotating speed, obtains the polyaniline massfraction and be 4%, the polyacrylonitrile massfraction is 10% co-blended spinning solution.Under the condition of 25 ℃ of room temperatures, humidity 35%, the flow velocity of co-blended spinning solution with 2mL/h is input on the spinning head, simultaneously spinning head is connected the 20kV power supply and carry out electrostatic spinning and prepare polyaniline/polyacrylonitrile blended nanofiber; To following electro-conductive glass 2a, the distance between following electro-conductive glass 2a and the spinning head is 15cm with spun fiber laydown; After treating that spinning is finished, will descend electro-conductive glass 2a to put into vacuum drying oven with 40 ℃ of dry 4h.With propylene carbonate and vinyl carbonate by volume 1:1 evenly mix, use the 4A molecular sieve drying.The high chloro acid dissolution is configured to the homogeneous solution that concentration is 0.15mol/L in acetonitrile, uses the 4A molecular sieve drying.In beaker, add 2g propylene carbonate-vinyl carbonate mixed solution, 7g perchloric acid-acetonitrile solution, 0.7g polymethylmethacrylate, 0.3g lithium perchlorate successively, mix gel.Gel electrolyte is coated on the polyaniline composite nano-fiber membrane uniformly, covers the last electro-conductive glass 2b of same size again, get rid of the bubble in the electrolyte.Electro-conductive glass is continuous up and down together respectively with lead, and with epoxy resin entire device is sealed, and lead is connected to constant voltage dc source, promptly gets required electrochromic device.The volt-ampere loop test shows that current potential, can be observed the device color and present successively from the change procedure of pale yellow-light yellow green-light green-light blue-blueness-bluish violet-purple from-0.7V to the 1.2V change procedure.20 circulations of accordion seek, device color are obviously decay not.
Embodiment 11
As shown in Figure 1, for containing the electrochromic device structural representation of polyaniline composite nano-fiber membrane, the described electrochromic device that contains the polyaniline composite nano-fiber membrane, comprise following electro-conductive glass 2a, polyaniline composite nano fiber layer 3, the gel electrolyte layer 4 that sets gradually from top to bottom and go up electro-conductive glass 2b, the outside of polyaniline composite nano fiber layer 3 and gel electrolyte layer 4 is provided with epoxy sealing layer 1, and the positive pole of D.C. regulated power supply 5 connects electro-conductive glass 2a, negative pole connection down and goes up electro-conductive glass 2b.Its preparation method is as follows:
Under 25 ℃ of conditions of room temperature, in stirred tank with 0.5g polyaniline (molecular weight 65000) with rotating speed 100rpm stirring and dissolving in 6.5g formic acid and tetrahydrofuran mixed solvent (mass ratio is 10:1), after treating that polyaniline dissolves fully, in solution, add 3g polyvinylpyrrolidone (molecular weight 40000), 400rpm stirs with rotating speed, obtains the polyaniline massfraction and be 5%, the polyvinylpyrrolidone massfraction is 30% co-blended spinning solution.Under the condition of 25 ℃ of room temperatures, humidity 20%, the flow velocity of co-blended spinning solution with 2mL/h is input on the spinning head, simultaneously spinning head is connected the 22kV power supply and carry out electrostatic spinning and prepare polyaniline/polyvinylpyrrolidone blended nanofibre; To following electro-conductive glass 2a, the distance between following electro-conductive glass 2a and the spinning head is 15cm with spun fiber laydown; After treating that spinning is finished, will descend electro-conductive glass 2a to put into vacuum drying oven with 40 ℃ of dry 4h.With propylene carbonate and vinyl carbonate by volume 1:1 evenly mix, use the 4A molecular sieve drying.The high chloro acid dissolution is configured to the homogeneous solution that concentration is 0.15mol/L in acetonitrile, uses the 4A molecular sieve drying.In beaker, add 2g propylene carbonate-vinyl carbonate mixed solution, 7g perchloric acid-acetonitrile solution, 0.7g polymethylmethacrylate, 0.3g lithium perchlorate successively, mix gel.Gel electrolyte is coated on the polyaniline composite nano-fiber membrane uniformly, covers the last electro-conductive glass 2b of same size again, get rid of the bubble in the electrolyte.Electro-conductive glass is continuous up and down together respectively with lead, and with epoxy resin entire device is sealed, and lead is connected to constant voltage dc source, promptly gets required electrochromic device.The volt-ampere loop test shows that current potential, can be observed the device color and present successively from the change procedure of pale yellow-light yellow green-light green-light blue-blueness-bluish violet-purple from-0.7V to the 1.2V change procedure.20 circulations of accordion seek, device color are obviously decay not.
Claims (4)
1. electrochromic device that contains the polyaniline composite nano-fiber membrane, it is characterized in that, comprise following electro-conductive glass (2a), polyaniline composite nano fiber layer (3), the gel electrolyte layer (4) that sets gradually from top to bottom and go up electro-conductive glass (2b), the outside of polyaniline composite nano fiber layer (3) and gel electrolyte layer (4) is provided with epoxy sealing layer (1), and the positive pole of D.C. regulated power supply (5) connects electro-conductive glass (2a), negative pole connection down and goes up electro-conductive glass (2b).
2. the described preparation method who contains the electrochromic device of polyaniline composite nano-fiber membrane of claim 1 is characterized in that concrete steps are:
The first step: at ambient temperature, in stirred tank the polyaniline in eigenstate raw material is dissolved in the solvent, speed of agitator is 50-200rpm, obtains the polyaniline solutions that massfraction is 0.2%-15%; The blending polymkeric substance is joined in the polyaniline solutions, speed of agitator is 200-1000rpm, mixes again, and obtains the blending solution that blending polymer quality mark is 0.5%-30%; In room temperature and relative humidity is under the condition of 20%-60%, the flow velocity of blending solution with 0.1-4mL/h is input on the spinning head, simultaneously spinning head is connected the 10-40KV power supply and carry out electrostatic spinning, electro-conductive glass (2a) is as receiving trap under adopting, distance between receiving trap and the spinning head is 5-30cm, to descend electro-conductive glass (2a) to go up nano fibrous membrane dry 1-12 h in 25-80 ℃ of vacuum of deposition, promptly obtain polyaniline composite nano-fiber membrane (3);
Second step: with propylene carbonate and vinyl carbonate by volume 1:1 evenly mix, use the 4A molecular sieve drying, the high chloro acid dissolution is configured to the homogeneous solution that concentration is 0.15mol/L in acetonitrile, use the 4A molecular sieve drying, in beaker, add the propylene carbonate-vinyl carbonate mixed solution of 2 weight portions, the perchloric acid-acetonitrile solution of 7 weight portions, the polymethylmethacrylate of 0.7 weight portion, the lithium perchlorate of 0.3 weight portion successively, mix, obtain gelatinous electrolyte;
The 3rd step: the gelatinous electrolyte that second step was obtained is coated to the last gel electrolyte layer (4) that forms of polyaniline composite nano-fiber membrane (3) that the first step obtains uniformly, cover electro-conductive glass (2b) again, electro-conductive glass in the extruding (2b) is to get rid of the bubble in the gel electrolyte layer (4), to go up electro-conductive glass (2b) and be connected lead respectively with following electro-conductive glass (2a), with epoxy resin the entire device sealing is formed epoxy sealing layer (1), to go up electro-conductive glass (2b) and link to each other with anodal with the negative pole of D.C. regulated power supply (5) respectively, promptly obtain containing the electrochromic device of polyaniline composite nano-fiber membrane with following electro-conductive glass (2a).
3. the preparation method who contains the electrochromic device of polyaniline composite nano-fiber membrane as claimed in claim 2, it is characterized in that, the solvent of the described first step is formic acid, trifluoroacetic acid, perfluoro caprylic acid, hexafluoroisopropanol, N-Methyl pyrrolidone, N, the potpourri of one or more in dinethylformamide, N,N-dimethylacetamide, tetrahydrofuran, dimethyl sulfoxide (DMSO), methenyl choloride, ethanol and the methylene chloride.
4. the preparation method who contains the electrochromic device of polyaniline composite nano-fiber membrane as claimed in claim 2, it is characterized in that, blending polymkeric substance in the described first step is nylon 6, polymethylmethacrylate, polyvinyl alcohol (PVA), polyacrylamide, cellulose acetate, ethyl cellulose, polyacrylic acid, polyacrylonitrile, the potpourri of one or more in polyoxyethylene, PLA and the polyvinylpyrrolidone.
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