CN104317129A - High-throughput screening electrochromic device for electrochromic materials and method for manufacturing high-throughput screening electrochromic device - Google Patents
High-throughput screening electrochromic device for electrochromic materials and method for manufacturing high-throughput screening electrochromic device Download PDFInfo
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- CN104317129A CN104317129A CN201410589550.1A CN201410589550A CN104317129A CN 104317129 A CN104317129 A CN 104317129A CN 201410589550 A CN201410589550 A CN 201410589550A CN 104317129 A CN104317129 A CN 104317129A
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- G—PHYSICS
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- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
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- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
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Abstract
The invention provides a high-throughput screening electrochromic device for electrochromic materials and a method for manufacturing the high-throughput screening electrochromic device, and belongs to the technical field of functional devices. The high-throughput screening electrochromic device for the electrochromic materials comprises a substrate and electrochromic device units. The electrochromic device units are arranged on the substrate to form m*n matrixes and comprise working electrodes, titanium dioxide layers, electrolyte layers and counter electrodes which are sequentially arranged on the substrate from bottom to top, each row or column of working electrodes is connected with the same printing electrode and is used as working electrodes to be led out, and the quantity of the printing electrodes is m or n. The high-throughput screening electrochromic device and the method have the advantages that the various electrochromic materials and formulas can be simultaneously screened by the aid of the high-throughput screening electrochromic device, high-throughput electrochromic material screening can be implemented, the development speeds can be increased, and the cost can be reduced.
Description
Technical field
The invention belongs to function element technical field, be specifically related to electrochromic device of a kind of high flux screening electrochromic material and preparation method thereof.
Background technology
High throughput method refers under the support of pertinent instruments, equipment, method, detect number at one time with sample necessarily, and with the technical system of the associated databases support obtained running, it has trace, the feature such as quick, sensitive and accurate, a kind of method of rapid screening, detection, collection material information, among the screening that it was once widely used in medicine and the Human Genome Project.Current, because the requirement of people to material development speed is more and more higher, enterprise and scientific research institutions all want that the introducing by technology, method improves the research and development speed of material on a large scale, the research and development of material are allowed to enter into the high speed research and development track of the large-scale production of factory's formula, in this context, high throughput method enters into Material Field comprehensively.
At present, how to realize to the iron-enriched yeast of various material and screening become increasing scientific research personnel will in the face of and the problem that solves.Because the state (solid, liquid, gas), preparation method, detection characterizing method etc. of different materials system all have difference, therefore the high flux research of material needs to carry out studying (Solid-State High-Throughput Screening for Color Tuning of Electrochromic Polymers-Adv.Mater.2013 for a certain specific material system or a certain class material, 25,6256 – 6260).These researchs both may having related to method, also may being the improvement (publication No. is the Chinese invention patent " for supplying the equipment of reactant liquid " of " CN103619462A ") of equipment.But due to the kind of material, preparation method, technique and equipment more and more numerous and more jumbled, this must cause the research of the high flux of material to become another independently " genome plan ".
Electrochromism (Electrochromism, EC) refer under the effect of external electrical field, materials from oxidizing or reduction causes it to produce reversible change to the transmission of light or reflection, then shows as the phenomenon of the reversible change of color and transparency in appearance.Electrochromic device has good application prospect in actual life, has been widely used in the products such as the energy-conservation smart windows of electrochromism, automotive rear-view antidazzle mirror, electrochromic display device (ECD), electrochromism storer, the sunglasses with colour change function.At present, electro-deposition electrochromic device adopts a preparation individual devices of filling a prescription to carry out sedimentation experiment, to screen material and formula.But the method complicated operation, experimental period is long, and screening effeciency is low, and manpower and financial resources cost is all higher.
Summary of the invention
The present invention is directed to the defect that background technology exists, propose electrochromic device of a kind of high flux screening electrochromic material and preparation method thereof, this electrochromic device can realize the screening to multiple electrochromic material and formula simultaneously, achieve the high flux screening of electrochromic material, accelerate research and development speed, reduce cost.
Technical scheme of the present invention is as follows:
A kind of electrochromic device of high flux screening electrochromic material, comprise the electrochromic device unit that substrate arranges with the m * n matrix be arranged on substrate, described electrochromic device unit is followed successively by the working electrode be arranged on substrate, titanium dioxide layer, electrolyte layer and to electrode from the bottom up, the working electrode of described a row or column is connected with same printing electrode and draws as working electrode, described in the number that prints electrode be m or n.
Further, when a line working electrode with same print electrode be connected and draw time, the number printed electrode is m; When row working electrode with same print electrode be connected and draw time, the number printed electrode is that n is individual.
Further, described is m × n transparency conducting layer to electrode.
Further, described electrolytic solution is the mixed liquor of copper salt solution, silver salt solution and quaternary ammonium salt solution.
Further, print electrode described in as electrocondution slurry solidification obtains.
A preparation method for the electrochromic device of high flux screening electrochromic material, comprises the following steps:
Step 1: in transparent conductive substrate etching formed m * n matrix arrangement conductive layer, each etching bandwidth identical and insulation, after having etched, clean and dry;
Step 2: etch in step 1 on each conductive layer obtained and spray nano-TiO
2dispersion liquid, sintering, obtains the TiO that thickness is 500 ~ 1200nm
2layer;
Step 3: the etching of a row or column of transparent conductive substrate obtained after step 2 processes brings preparation to print electrode, described in print electrode and to connect with each conductive layer of corresponding a row or column, described in the number that prints electrode be that m or n is individual;
Step 4: the surrounding of each conductive layer after step 3 processes arranges plastic septum, then drips copper salt solution, silver salt solution and quaternary ammonium salt solution to each conductive layer area;
Step 5: top m × n being positioned over respectively each conductive layer after step 4 process to electrode, and drawn by copper-foil conducting electricity;
Step 6: in corresponding the printing electrode and to making alive on the Copper Foil that electrode is drawn, observe the color changeable effect of m × n electrochromic device of each conductive layer, thus realize the high flux screening to electrochromic material and formula.
Preferably, m and n described in above-mentioned steps meets relation: m=n.
Further, in step 3, preparation is when printing electrode: when a line working electrode with same print electrode be connected and draw time, the number printed electrode is that m is individual; When row working electrode with same print electrode be connected and draw time, the number printed electrode is that n is individual.
Wherein, the transparent conductive substrate described in step 1 can be electro-conductive glass, and such as FTO electro-conductive glass (mixes the SnO of fluorine
2transparent conducting glass, SnO
2: F), IZO electro-conductive glass (mixes the In of zinc
2o
3transparent conducting glass, In
2o
3: Zn), AZO electro-conductive glass (mixes the ZnO transparent conductive glass of aluminium, ZnO:Al), GZO electro-conductive glass (mixes the ZnO transparent conductive glass of gallium, ZnO:Ga), SZO electro-conductive glass (mixes the ZnO transparent conductive glass of silicon, ZnO:Si), BZO electro-conductive glass (the ZnO transparent conductive glass of boron-doping, ZnO:B), FZO electro-conductive glass (mixing the ZnO transparent conductive glass of fluorine, ZnO:F), ATO electro-conductive glass (mix the SnO of antimony
2transparent conducting glass, SnO
2: Sb), In
2o
3: Nb (mixes the In of niobium
2o
3transparent conducting glass), ZnO:Sc (mixing the ZnO transparent conductive glass of scandium), SnO
2: Ta (mixes the SnO of thallium
2transparent conducting glass), SnO
2: W (mixes the SnO of tungsten
2transparent conducting glass) etc., also can for scribbling the flexible substrate of transparency conducting layer, such as ITO/PET (polyethylene terephthalate), AZO/PET, AZO/PC (polycarbonate), AZO/PES (polyethersulfone), AZO/PVDF (polyvinylidene fluoride), AZO/TPT (polyvinyl fluoride composite membrane), GZO/PET, GZO/PC, GZO/PEN (Polyethylene Naphthalate), IZO/PET, IZO/PC, FTO/PET, ATO/PES etc.
Further, the detailed process of described step 2 is: compound concentration is 0.001 ~ 0.1g/mL, grain size is the nano-TiO of 5 ~ 500nm
2particle dispersion, each conductive layer adopting ultrasonic spraying method to etch in step 1 to obtain sprays nano-TiO
2particle dispersion, sinters 30min after having sprayed at 500 DEG C, obtains the TiO that thickness is 500 ~ 1200nm
2layer.
Wherein, the thickness printed electrode described in step 3 is equal with the etching depth described in step 1.
Wherein, printing electrode described in step 3 adopts the method for serigraphy to bring in the etching of a row or column and brushes electrocondution slurry and sintering curing obtains.
Wherein, the method of ultrasonic dropping is adopted to drip copper salt solution, silver salt solution and quaternary ammonium salt solution in step 4, the concentration of described copper salt solution is 0.1mol/L, the concentration of described silver salt solution is 0.5mol/L, the concentration of described quaternary ammonium salt solution is 2mol/L, the dripping quantity of described mantoquita and silver salt solution is respectively 0.001 ~ 0.15mL, and the dripping quantity of described quaternary ammonium salt is 0.005 ~ 0.25mL, and the dropping total amount of three kinds of solution is 0.035mL ~ 0.3mL.
The solvent of the copper salt solution described in step 4, silver salt solution and quaternary ammonium salt solution is any one in formamide, dimethyl sulfoxide (DMSO) (DMSO), dimethyl formamide (DMF), dimethyl acetamide (DMAC), hexamethyl phosphoramide.Described quaternary ammonium salt is any one in cetab, tetrabutyl ammonium bromide, tetramethylammonium bromide, teabrom, ammonium bromide, DTAB.Described mantoquita is any one in copper nitrate, cupric chloride, copper sulphate.
Plastic septum described in step 4 is teflon, Polyvinylchloride (PVC) plastic plate, polypropylene (PP) plastic plate, acrylonitrile-butadiene-styrene copolymer (ABS) plastic plate, polycarbonate (PC) plastic plate, polyethylene terephthalate (PET) plastic plate, polyvinylidene fluoride (PVDF) plastic plate etc.
Beneficial effect of the present invention is: electrochromic device provided by the invention can realize the variable color of multiple electrochromic device unit simultaneously, can carry out high flux screening to electrochromic material or formula, accelerates research and development speed, saves cost.
Accompanying drawing explanation
Fig. 1 is that embodiment 1 etches the conductive layer obtained in transparent conductive substrate;
Fig. 2 carries out ultrasonic spraying to conductive layer in transparent conductive substrate in embodiment 1;
Fig. 3 is the transparent conductive substrate in embodiment 1 after sintering;
Fig. 4 scribbles the transparent conductive substrate printed electrode in embodiment 1;
Fig. 5 (a) is the glutinous transparent conductive substrate having plastic septum of embodiment 1; Fig. 5 (b) is for digging the plastic septum of through hole in embodiment 1;
Fig. 6 is the ultrasonic dropping electrolyte solution of embodiment 1 pair of via regions
Fig. 7 (a) encapsulates the device obtained for embodiment 1; Fig. 7 (b) is the glutinous front to electrode having copper-foil conducting electricity of embodiment 1; Fig. 7 (c) is the glutinous back side to electrode having copper-foil conducting electricity;
Fig. 8 (a) is the side view of the transparent conductive substrate after embodiment 1 etching; The transparent conductive substrate that Fig. 8 (b) prints electrode for embodiment 1 scribbles is along the side view in direction of printing electrode; Fig. 8 (c) scribbles the left side view of the transparent conductive substrate that prints electrode for embodiment 1; Fig. 8 (d) has the transparent conductive substrate of plastic septum along the side view in direction of printing electrode for embodiment 1 is glutinous; Fig. 8 (e) is the glutinous left side view having the transparent conductive substrate of plastic septum of embodiment 1; Fig. 8 (f) obtains the side view of device along direction of printing electrode for embodiment 1 encapsulates; Fig. 8 (g) encapsulates the left side view of the device obtained for embodiment 1.
Fig. 9 is that embodiment 2 etches the conductive layer obtained in transparent conductive substrate;
Figure 10 carries out ultrasonic spraying to conductive layer in transparent conductive substrate in embodiment 2;
Figure 11 is the transparent conductive substrate in embodiment 2 after sintering;
Figure 12 scribbles the transparent conductive substrate printed electrode in embodiment 2;
Figure 13 (a) is the glutinous transparent conductive substrate having plastic septum of embodiment 2; Figure 13 (b) is for digging the plastic septum of through hole in embodiment 2;
Figure 14 is the ultrasonic dropping electrolyte solutions of embodiment 2 pairs of via regions
Figure 15 (a) encapsulates the device obtained for embodiment 2; Figure 15 (b) is the glutinous front to electrode having copper-foil conducting electricity of embodiment 2; Figure 15 (c) is the glutinous back side to electrode having copper-foil conducting electricity;
Figure 16 (a) is the side view of the transparent conductive substrate after embodiment 2 etching; The transparent conductive substrate that Figure 16 (b) prints electrode for embodiment 2 scribbles is along the side view in direction of printing electrode; Figure 16 (c) scribbles the left side view of the transparent conductive substrate that prints electrode for embodiment 2; Figure 16 (d) has the transparent conductive substrate of plastic septum along the side view in direction of printing electrode for embodiment 2 is glutinous; Figure 16 (e) is the glutinous left side view having the transparent conductive substrate of plastic septum of embodiment 2; Figure 16 (f) obtains the side view of device along direction of printing electrode for embodiment 2 encapsulates; Figure 16 (g) encapsulates the left side view of the device obtained for embodiment 2.
Embodiment
Below in conjunction with embodiment and accompanying drawing, introduction is further done to the present invention:
A kind of electrochromic device of high flux screening electrochromic material, comprise working electrode, titanium dioxide layer, electrolyte layer, to electrode, it is characterized in that, described working electrode is be arranged on substrate, the transparency conducting layer of m * n matrix arrangement, described each transparency conducting layer is disposed with titanium dioxide layer and electrolyte layer, the transparency conducting layer of described a row or column is connected with same printing electrode respectively, described is m × n transparency conducting layer to electrode, individual top electrode being covered respectively to the transparency conducting layer of each band titanium dioxide layer and electrolyte layer of described m × n, working electrode is by extraction of printing electrode, electrode is drawn the Copper Foil on electrode conducting layer each by sticking, the described number printed electrode is m or n.
Further, when a line working electrode with same print electrode be connected and draw time, the number printed electrode is m; When row working electrode with same print electrode be connected and draw time, the number printed electrode is that n is individual.
Further, print electrode described in as electrocondution slurry solidification obtains.
A preparation method for the electrochromic device of high flux screening electrochromic material, comprises the following steps:
Step 1: etching forms the conductive layer of n × n matrix arrangement in transparent conductive substrate, the equal and insulation of each etching bandwidth, after etch, uses deionized water and washes of absolute alcohol 5 ~ 7 times respectively, then oven dry at 70 ~ 150 DEG C in an oven;
Step 2: compound concentration is 0.001 ~ 0.1g/mL, grain size is the nano-TiO of 5 ~ 500nm
2particle dispersion, each conductive layer then adopting ultrasonic spraying method to etch in step 1 to obtain sprays nano-TiO
2particle dispersion, sinters 30min after having sprayed at 500 DEG C, obtains the TiO that thickness is 500 ~ 1200nm
2layer;
Step 3: every a line or each row transparency conducting layer on place 1 piece of plastic septum respectively, described plastic septum opens the square opening that area is less than conductive layer in the top position that each conductive layer is corresponding, then deionized water and ethanol purge 3 ~ 5 times is adopted respectively, and 60 ~ 100 DEG C of dry for standby in an oven;
Step 4: choose n × n area to be greater than in step 3 open the transparent conductive substrate of square opening, deionized water and EtOH Sonicate is adopted to clean 3 ~ 5 times, and 70 ~ 100 DEG C of oven dry in an oven, affix copper-foil conducting electricity in the conductive layer one side of transparent conductive substrate after taking-up and draw as electrode;
Step 5: bring employing screen process press to brush electrocondution slurry a line of the transparent conductive substrate obtained after step 2 processes or a row etching and sintering curing as printing electrode, described printing electrode connects with each conductive layer of corresponding a row or column, the described number printed electrode is n, described in the thickness that prints electrode equal with the etching depth in step 1;
Step 6: the plastic septum step 3 handled well binds in the transparent conductive substrate handled well in step 5, the square opening wherein described in step 3 is positioned over above conductive layer that transparent conductive substrate etches;
Step 7: the copper salt solution preparing 20mL 0.1mol/L respectively, the silver salt solution of 20mL 0.5mol/L, the quaternary ammonium salt solution of 20mL 2mol/L, the method of ultrasonic dropping is adopted to drip the copper salt solution of above-mentioned preparation in each conductive layer area surface that step 6 process obtains, silver salt solution and quaternary ammonium salt solution, wherein the dripping quantity of copper salt solution and silver salt solution is respectively 0.001mL ~ 0.15mL, the dripping quantity of quaternary ammonium salt solution is 0.005mL ~ 0.25mL, the cumulative volume of the above-mentioned three kinds of solution dripped is 0.035mL ~ 0.3mL, then transparent conductive substrate step 4 handled well binds the top of n × n square opening on dividing plate,
Step 8: in corresponding the printing electrode and add voltage on the Copper Foil that electrode is drawn of each conductive layer, observes the color changeable effect of n × n electrochromic device, thus realizes the high flux screening to electrochromic material and formula.
The electrochromic device of high flux screening electrochromic material of the present invention can realize the screening to electrochromic material and formula, mainly by controlling kind and the volume of the solution of ultrasonic dropping, thus realizes the screening to material and concentration.Described electrochromic device can utilize multi-path power supply to apply voltage to wherein each electrochromic device unit simultaneously.
Embodiment 1
A preparation method for the electrochromic device of high flux screening electrochromic material, comprises the following steps:
Step one: the FTO electro-conductive glass being 10cm × 10cm by size is by the conductive layer being etched into 2 × 2 square formations shown in Fig. 1, the width of each etching band is 5mm, and ensure etching tape insulation, utilize deionized water, absolute ethyl alcohol to clean 5 times respectively respectively, and dry at 80 DEG C;
Step 2: take titania that 0.1g grain size is 20nm respectively, 0.6mL terpinol, 0.03g ethyl cellulose, 0.01g lauric acid, 30mL absolute ethyl alcohol to add in ball grinder after ball milling 50min, obtain the nano-TiO that 20mL concentration is 0.005g/mL
2particle dispersion, sprays nano-TiO by adopting shown in Fig. 2 on ultrasonic spraying process each conductive layer described in step one
2particle dispersion, sinters 30min by this FTO electro-conductive glass after spraying terminates, obtains the TiO that thickness is 600nm at 500 DEG C
2layer;
Step 3: be 9cm × 2.5cm by 2 block sizes, thickness is 0.5mm teflon dividing plate digs out through hole by shown in Fig. 5 (b), hole size is 2cm × 2cm, baking oven is put into after again the dividing plate handled well being utilized respectively deionized water, washes of absolute alcohol 3 times, dry at 80 DEG C, for subsequent use;
Step 4: choose the FTO electro-conductive glass that 4 block sizes are 2.5cm × 2.8cm, be immersed in deionized water and absolute ethyl alcohol respectively, supersonic cleaning machine is utilized to clean 3 times, dry at 80 DEG C, press shown in Fig. 7 (b) He (c) after taking out, affix at its conductive layer the copper-foil conducting electricity that width is 3mm;
Step 5: adopt screen process press to arrange according to the FTO electro-conductive glass two after Fig. 4 institute is shown in step 2 process and etch band and brush conductive silver paste and 200 DEG C of solidifications, described each conductive layer arranged with corresponding that prints electrode connects, the width printed electrode is 3mm, and thickness is identical with the degree of depth etched in step one;
Step 6: the teflon dividing plate that step 3 is obtained by the conductive layer binding the FTO electro-conductive glass after step 5 process shown in Fig. 5 (a) respectively, on dividing plate open the top that hole is positioned at conductive layer;
Step 7: take 260mg cupric chloride, 1.7g silver nitrate, 12.896g tetrabutyl ammonium bromide respectively, is dissolved in respectively in 20mL DMSO solution, is mixed with solution;
Step 8: the through hole edge of the FTO electro-conductive glass upper spacer obtained in step 6 affixes double faced adhesive tape, utilize ultrasonic dropping respectively to the three kinds of solution prepared in implantation step seven in each through hole, the amount that silver salt solution and copper salt solution inject is respectively 0.005mL, the injection rate IR of quaternary ammonium salt solution is 0.1mL, then the FTO electro-conductive glass that step 4 obtains is covered, conductive layer is also compacting downwards, and drawn by copper-foil conducting electricity, successively above-mentioned identical operation is taked to other through hole again, in corresponding the printing electrode and copper-foil conducting electricity adds suitable voltage of each Conductive layer portions after completing, observe its electrochromic effect to carry out the screening of material and formula.
The device that the present embodiment prepares well can realize the high flux screening to electro-deposition electrochromic material, once can realize the screening of 4 different formulations.And after having tested, after dismounting cleaning is carried out to associated components, also can reuse.
Embodiment 2
A preparation method for the electrochromic device of high flux screening electrochromic material, comprises the following steps:
Step one: the FTO electro-conductive glass being 10cm × 10cm by size is by the conductive layer being etched into 4 × 4 square formation arrangements shown in Fig. 9, the width of each etching band is 5mm, and ensure etching tape insulation, utilize deionized water, absolute ethyl alcohol to clean 5 times respectively respectively, and dry at 80 DEG C;
Step 2: take titania that 0.1g grain size is 20nm respectively, 0.6mL terpinol, 0.03g ethyl cellulose, 0.01g lauric acid, 30mL absolute ethyl alcohol add ball milling 50min in ball grinder, obtain the nano-TiO that 20mL concentration is 0.005g/mL
2particle dispersion, and spray nano-TiO by utilizing shown in Figure 10 on the method for ultrasonic spraying each conductive layer described in step one
2particle dispersion, sinters 30min after spraying terminates, obtains the TiO that thickness is 800nm at 500 DEG C
2layer;
Step 3: be 9cm × 1.5cm by 4 block sizes, thickness digs out through hole by shown in Figure 13 (b) for 0.5mm teflon dividing plate, hole size is 1.2cm × 1.2cm, again the dividing plate handled well is utilized deionized water, washes of absolute alcohol 3 times respectively, and dry at 80 DEG C, for subsequent use;
Step 4: choose the FTO electro-conductive glass that 16 block sizes are 1.5cm × 1.8cm, be immersed in deionized water and absolute ethyl alcohol respectively, ultrasonic cleaning 3 times, dry at 80 DEG C, according to shown in Figure 15 (b) He (c) after taking-up, affix at its conductive layer the copper-foil conducting electricity that width is 3mm;
Step 5: adopt screen process press to arrange according to the FTO electro-conductive glass four after Figure 12 institute is shown in step 2 process and etch band and brush conductive silver paste and 200 DEG C of solidifications, described each conductive layer arranged with corresponding that prints electrode connects, the width printed electrode is 3mm, and thickness is consistent with the degree of depth etched in step one;
Step 6: by the teflon dividing plate obtained in step 3 by the conductive layer binding the FTO electro-conductive glass after step 5 process shown in Figure 13 (a) respectively, on dividing plate open the top that hole is positioned at conductive layer;
Step 7: take 260mg cupric chloride, 1.7g silver nitrate, 12.896g tetrabutyl ammonium bromide respectively, be dissolved in respectively in the DMSO solution of 20mL, be mixed with solution;
Step 8: the through hole edge of the FTO electro-conductive glass upper spacer obtained in step 6 affixes double faced adhesive tape, adopt the method for ultrasonic dropping respectively to three kinds of solution of preparation in implantation step seven in each through hole, the amount that silver salt solution and copper salt solution inject is respectively 0.1mL, the injection rate IR of quaternary ammonium salt solution is 0.25mL, then the FTO electro-conductive glass that step 4 obtains is covered, conductive layer is also compacting downwards, and drawn by copper-foil conducting electricity, successively above-mentioned identical operation is taked to other through hole again, in corresponding the printing electrode and copper-foil conducting electricity adds suitable voltage of each Conductive layer portions after completing, observe its electrochromic effect to carry out the screening of material.
The device that the present embodiment prepares well can complete the high flux screening to electro-deposition electrochromic material, once can realize the screening of 16 different formulations simultaneously, and after having tested, after dismounting cleaning is carried out to associated components, can also reuse.
Embodiment 3
A preparation method for the electrochromic device of high flux screening electrochromic material, comprises the following steps:
Step one: be the square formation that the FTO electro-conductive glass of 10cm × 10cm is etched into 6 × 6 by size, the width of each etching band is 5mm, and ensure the insulation of etching band portion, put into baking oven after utilizing deionized water, absolute ethyl alcohol to clean 5 times respectively respectively, dry at 80 DEG C;
Step 2: the grain size taking 0.1g is respectively the titania of 20nm, 0.6mL terpinol, 0.03g ethyl cellulose, 0.01g lauric acid, 30mL absolute ethyl alcohol to add in ball grinder after ball milling 50min, obtains the nano-TiO that 20mL concentration is 0.005g/mL
2particle dispersion, then adopts on ultrasonic spraying process each conductive layer described in step one and sprays nano-TiO
2particle dispersion, sinters 30min after spraying terminates, obtains the TiO that thickness is 800nm at 500 DEG C
2layer;
Step 3: be 9cm × 1cm by 6 block sizes, thickness is that the teflon dividing plate of 0.5mm digs out through hole according to embodiment 1 rule, hole size is 0.7cm × 0.7cm, baking oven is put into after again the dividing plate handled well being utilized respectively deionized water, washes of absolute alcohol 3 times, dry at 80 DEG C, for subsequent use;
Step 4: choose the FTO electro-conductive glass that 36 block sizes are 1cm × 1.3cm, be immersed in respectively in deionized water and absolute ethyl alcohol, utilize supersonic cleaning machine to clean 3 times, dries, affixes the copper-foil conducting electricity that width is 3mm after taking-up at its conductive layer at 80 DEG C;
Step 5: adopt the FTO electro-conductive glass six of screen process press after step 2 process to arrange etching band and brush conductive silver paste and 200 DEG C of solidifications, described each conductive layer arranged with corresponding that prints electrode connects, the width printed electrode is 3mm, and thickness is identical with the degree of depth etched in step one;
Step 6: teflon dividing plate step 3 obtained binds on the conductive layer of the FTO electro-conductive glass after step 5 process respectively, on dividing plate open the top that hole is positioned at conductive layer;
Step 7: take 260mg cupric chloride, the silver nitrate of 1.7g, 12.896g tetrabutyl ammonium bromide respectively, be dissolved in respectively in 20mL DMSO solution, be mixed with solution.
Step 8: the through hole edge of the FTO electro-conductive glass upper spacer obtained in step 6 affixes double faced adhesive tape, utilize ultrasonic dropping respectively to the three kinds of solution prepared in implantation step seven in each through hole, the amount that silver salt solution and copper salt solution inject is respectively 0.05mL, the injection rate IR of quaternary ammonium salt solution is 0.1, then the FTO electro-conductive glass that step 4 obtains is covered, conductive layer is also compacting downwards, and drawn by copper-foil conducting electricity, successively above-mentioned identical operation is taked to other through hole again, in corresponding the printing electrode and copper-foil conducting electricity adds suitable voltage of each Conductive layer portions after completing, observe its electrochromic effect to carry out the screening of material and formula.
The device that the present embodiment prepares can well complete to be done the high flux screening of electro-deposition electrochromic material, once can realize the screening of 36 different formulations.And after having tested, after dismounting cleaning is carried out to associated components, can also reuse.
Embodiment 4
A preparation method for the electrochromic device of high flux screening electrochromic material, comprises the following steps:
Step one: be the conductive layer that the AZO electro-conductive glass of 10cm × 10cm is etched into the square formation arrangement of 4 × 4 by size, the width of each etching band is 5mm, and ensure etching tape insulation, utilize deionized water, absolute ethyl alcohol to clean 5 times respectively respectively, and dry at 80 DEG C;
Step 2: the grain size taking 0.1g is respectively the titania of 20nm, 0.6mL terpinol, 0.03g ethyl cellulose, 0.01g lauric acid, 30mL absolute ethyl alcohol to add in ball grinder after ball milling 50min, obtains the nano-TiO that 20mL concentration is 0.005g/mL
2particle dispersion, adopts on ultrasonic spraying process each conductive layer described in step one and sprays nano-TiO
2particle dispersion, sinters 30min after spraying terminates, obtains the TiO that thickness is 1000nm at 500 DEG C
2layer;
Step 3: be 9cm × 1.5cm by 4 block sizes, thickness is that 0.5mm teflon dividing plate digs out through hole according to embodiment 1 rule, and hole size is 1.2cm × 1.2cm, then the dividing plate handled well is utilized deionized water, washes of absolute alcohol 3 times respectively, dry at 80 DEG C, for subsequent use;
Step 4: choose the AZO electro-conductive glass that 16 block sizes are 1.5cm × 1.8cm, be immersed in respectively in deionized water and absolute ethyl alcohol, utilize supersonic cleaning machine to clean 3 times, dries, affixes the copper-foil conducting electricity that width is 3mm after taking-up at its conductive layer at 80 DEG C;
Step 5: adopt the AZO electro-conductive glass four lines etching band of screen process press after step 2 process to brush conductive silver paste and 200 DEG C of solidifications, described printing electrode connects with each conductive layer of corresponding a line, the width printed electrode is 3mm, and thickness is identical with the degree of depth that step one etches;
Step 6: teflon dividing plate step 3 obtained binds on the conductive layer of the AZO electro-conductive glass after step 5 process respectively, on dividing plate open the top that hole is positioned at conductive layer;
Step 7: take 260mg cupric chloride, the silver nitrate of 1.7g, 12.896g tetrabutyl ammonium bromide respectively, be dissolved in respectively in the DMSO solution of 20mL, be mixed with solution.
Step 8: the through hole edge of the AZO electro-conductive glass upper spacer obtained in step 6 affixes double faced adhesive tape, utilize ultrasonic dropping respectively to the three kinds of solution prepared in implantation step seven in each through hole, the amount that silver salt solution and copper salt solution inject is respectively 0.12mL, the injection rate IR of quaternary ammonium salt solution is 0.2mL, then the AZO electro-conductive glass that step 4 obtains is covered, conductive layer is also compacting downwards, and drawn by copper-foil conducting electricity, successively above-mentioned identical operation is taked to other through hole again, in corresponding the printing electrode and copper-foil conducting electricity adds suitable voltage of each Conductive layer portions after completing, observe its electrochromic effect to carry out the screening of material and formula.
The device that the present embodiment prepares well can complete the work of the high flux screening to electro-deposition electrochromic material, once can realize the screening of 16 different formulations.And after having tested, after dismounting cleaning is carried out to associated components, can also reuse.
Embodiment 5
A preparation method for the electrochromic device of high flux screening electrochromic material, comprises the following steps:
Step one: be the conductive layer that the FTO electro-conductive glass of 10cm × 10cm is etched into 4 × 4 square formations arrangements by size, the width of each etching band is 5mm, and ensure etching tape insulation, utilize deionized water, absolute ethyl alcohol to clean 5 times respectively respectively, and dry at 80 DEG C;
Step 2: the grain size taking 0.1g is respectively the titania of 20nm, 0.6mL terpinol, 0.03g ethyl cellulose, 0.01g lauric acid, 30mL absolute ethyl alcohol to add in ball grinder after ball milling 50min, obtains the nano-TiO that 20mL concentration is 0.005g/mL
2particle dispersion, adopts on ultrasonic spraying process each conductive layer described in step one and sprays nano-TiO
2particle dispersion, sinters 30min after spraying terminates, obtains the TiO that thickness is 1200nm at 500 DEG C
2layer;
Step 3: be 9cm × 1.5cm by 4 block sizes, thickness is that 0.5mm teflon dividing plate digs out through hole according to embodiment 1 rule, hole size is 1.2cm × 1.2cm, baking oven is put into after again the dividing plate handled well being utilized respectively deionized water, washes of absolute alcohol 3 times, dry at 80 DEG C, for subsequent use;
Step 4: choose the FTO electro-conductive glass that 16 block sizes are 1.5cm × 1.8cm, be immersed in respectively in deionized water and absolute ethyl alcohol, utilize supersonic cleaning machine to clean 3 times, dries, affixes the copper-foil conducting electricity that width is 3mm after taking-up at its conductive layer at 80 DEG C;
Step 5: adopt the FTO electro-conductive glass four of screen process press after step 2 process to arrange etching band and brush conductive silver paste and 200 DEG C of solidifications, described each conductive layer arranged with corresponding that prints electrode connects, the width printed electrode is 3mm, and thickness is identical with the degree of depth etched in step one;
Step 6: teflon dividing plate step 3 obtained binds on the conductive layer of the FTO electro-conductive glass after step 5 process respectively, on dividing plate open the top that hole is positioned at conductive layer;
Step 7: take 260mg cupric chloride, 1.7g silver nitrate, 12.896g tetrabutyl ammonium bromide respectively, be dissolved in respectively in the DMF solution of 20mL, be mixed with solution;
Step 8: the through hole edge of the FTO electro-conductive glass upper spacer obtained in step 6 affixes double faced adhesive tape, utilize ultrasonic dropping respectively to the three kinds of solution prepared in implantation step seven in each through hole, the amount that silver salt solution and copper salt solution inject is respectively 0.08mL, the injection rate IR of quaternary ammonium salt solution is 0.1mL, then the FTO electro-conductive glass that step 4 obtains is covered, conductive layer is also compacting downwards, and drawn by copper-foil conducting electricity, successively above-mentioned identical operation is taked to other through hole again, in corresponding the printing electrode and copper-foil conducting electricity adds suitable voltage of each Conductive layer portions after completing, observe its electrochromic effect to carry out the screening of material and formula.
The device that the present embodiment prepares well can realize the work of the high flux screening to electro-deposition electrochromic material, once can realize the screening of 16 different formulations.And after having tested, after dismounting cleaning is carried out to associated components, can also reuse.
Claims (10)
1. the electrochromic device of a high flux screening electrochromic material, comprise the electrochromic device unit that substrate arranges with the m * n matrix be arranged on substrate, described electrochromic device unit is followed successively by the working electrode be arranged on substrate, titanium dioxide layer, electrolyte layer and to electrode from the bottom up, the working electrode of described a row or column is connected with same printing electrode and draws as working electrode, described in the number that prints electrode be m or n.
2. the electrochromic device of high flux screening electrochromic material according to claim 1, is characterized in that, described is m × n transparency conducting layer to electrode.
3. the electrochromic device of high flux screening electrochromic material according to claim 1, is characterized in that, described electrolytic solution is the mixed liquor of copper salt solution, silver salt solution and quaternary ammonium salt solution.
4. the electrochromic device of high flux screening electrochromic material according to claim 1, is characterized in that, described in print electrode for electrocondution slurry solidification obtain.
5. a preparation method for the electrochromic device of high flux screening electrochromic material, comprises the following steps:
Step 1: in transparent conductive substrate etching formed m * n matrix arrangement conductive layer, each etching bandwidth identical and insulation, after having etched, clean and dry;
Step 2: etch in step 1 on each conductive layer obtained and spray nano-TiO
2dispersion liquid, sintering, obtains the TiO that thickness is 500 ~ 1200nm
2layer;
Step 3: the etching of a row or column of transparent conductive substrate obtained after step 2 processes brings preparation to print electrode, described in print electrode and to connect with each conductive layer of corresponding a row or column, described in the number that prints electrode be that m or n is individual;
Step 4: the surrounding of each conductive layer after step 3 processes arranges plastic septum, then drips copper salt solution, silver salt solution and quaternary ammonium salt solution to each conductive layer area;
Step 5: top m × n being positioned over respectively each conductive layer after step 4 process to electrode, and drawn by copper-foil conducting electricity;
Step 6: in corresponding the printing electrode and to making alive on the Copper Foil that electrode is drawn, observe the color changeable effect of m × n electrochromic device of each conductive layer, thus realize the high flux screening to electrochromic material and formula.
6. the preparation method of the electrochromic device of high flux screening electrochromic material according to claim 5, is characterized in that, described m and n meets relation: m=n.
7. the preparation method of the electrochromic device of high flux screening electrochromic material according to claim 5, it is characterized in that, the transparent conductive substrate described in step 1 is FTO electro-conductive glass, IZO electro-conductive glass, AZO electro-conductive glass, GZO electro-conductive glass, SZO electro-conductive glass, BZO electro-conductive glass, FZO electro-conductive glass, ATO electro-conductive glass, mix the In of niobium
2o
3transparent conducting glass, mix the ZnO transparent conductive glass of scandium, mix the SnO of thallium
2transparent conducting glass, mix the SnO of tungsten
2transparent conducting glass.
8. the preparation method of the electrochromic device of high flux screening electrochromic material according to claim 5, it is characterized in that, the transparent conductive substrate described in step 1 is ITO/PET, AZO/PET, AZO/PC, AZO/PES, AZO/PVDF, AZO/TPT, GZO/PET, GZO/PC, GZO/PEN, IZO/PET, IZO/PC, FTO/PET, ATO/PES.
9. the preparation method of the electrochromic device of high flux screening electrochromic material according to claim 5, it is characterized in that, the method of ultrasonic dropping is adopted to drip copper salt solution in step 4, silver salt solution and quaternary ammonium salt solution, the concentration of described copper salt solution is 0.1mol/L, the concentration of described silver salt solution is 0.5mol/L, the concentration of described quaternary ammonium salt solution is 2mol/L, the dripping quantity of described mantoquita and silver salt solution is respectively 0.001 ~ 0.15mL, the dripping quantity of described quaternary ammonium salt is 0.005 ~ 0.25mL, the dropping total amount of three kinds of solution is 0.035mL ~ 0.3mL.
10. the preparation method of the electrochromic device of high flux screening electrochromic material according to claim 5, it is characterized in that, the solvent of the copper salt solution described in step 4, silver salt solution and quaternary ammonium salt solution is any one in formamide, dimethyl sulfoxide (DMSO) (DMSO), dimethyl formamide (DMF), dimethyl acetamide (DMAC), hexamethyl phosphoramide.
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