CN105130210B - The preparation method of three-dimensional ordered macroporous polyaniline/carbon compound electrochromic membrane - Google Patents
The preparation method of three-dimensional ordered macroporous polyaniline/carbon compound electrochromic membrane Download PDFInfo
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Abstract
The preparation method of three-dimensional ordered macroporous polyaniline/carbon compound electrochromic membrane, it is related to a kind of preparation method of carbon compound electrochromic membrane.The present invention in order to solve existing three-dimensional ordered macroporous structure Polyaniline Electrochromism Thin Film caused by electric conductivity is poor discoloration deficiency technical problem.Method：First, the surface treatment of baseplate material；2nd, the preparation of colloidal solution；3rd, the preparation of colloidal crystal template；4th, carbon covers the preparation of colloidal crystal template；5th, by working electrode, reference electrode and electrode is put into aniline protonic acid aqueous solution, deposited, rinsed, dried, after removing removing template, produce three-dimensional ordered macroporous polyaniline/carbon compound electrochromic membrane；Due to the introducing of carbon in the present invention, the electric conductivity of polyaniline is improved so that the electrochromic property of polyaniline film significantly improves.The invention belongs to the preparation field of electrochomeric films.
Description
Technical field
The present invention relates to a kind of preparation method of carbon compound electrochromic membrane.
Background technology
Electrochromism refers to some optical properties (such as reflectivity, transmitance and thermal emissivity rate) of material in external electrical field
In the presence of occur reversible change phenomenon.As a kind of new function material, electrochromic material optical-electronic energy conversion,
The fields such as light quantity regulation, Infostorage Record, photoswitch, architectural glazings smart windows, large screen display are all widely used
Prospect, with the rapid development of modern microelectronic technology, particularly large scale integrated circuit, Electrochromic device is in the excellent of these fields
Will definitely be more obvious.Electrochromic material generally can be divided into inorganic material and the major class of conducting polymer two.Become compared to inorganic electroluminescence
Color material, conducting polymer have the advantages that abundant color change, easy processing, easy MOLECULE DESIGN and cost are cheap.
Polyaniline is a kind of most commonly used conducting polymer electrochromic material, and its optical quality is good, cyclic reversibility
Height, and aniline monomer is cheap and easily-available.When leading to different voltages, polyaniline can be realized from pale yellow, yellowish green, green, bluish-green to indigo plant
The reversible change of color.However, current Polyaniline Electrochromism Thin Film is nearly all dense film, electrochromic coloration efficiency
It is low, response speed is slow, significantly limit its practical application.Patent CN102978674A, which discloses one kind, has photonic crystal
The preparation method of the Polyaniline Electrochromism Thin Film of structure, due to the presence of orderly pore structure, film illustrates excellent electroluminescent
Discoloration.But the electric conductivity of single polyaniline is poor, the further raising of film electrochromic property is limited.
The content of the invention
The present invention is to solve existing three-dimensional ordered macroporous structure Polyaniline Electrochromism Thin Film because electric conductivity is poor
Caused by discoloration deficiency technical problem, there is provided a kind of three-dimensional ordered macroporous polyaniline/carbon composite electrochromic is thin
The preparation method of film.
The preparation method of three-dimensional ordered macroporous polyaniline/carbon compound electrochromic membrane：
First, the surface treatment of baseplate material：After substrate is ultrasonically treated in acetone, methanol and ultra-pure water respectively, dry；
Wherein ultrasonic power is 60W-100W, and ultrasonic time 10-60min, the substrate is that thickness is coated with golden grid for 0.5mm-2mm
The quartz glass of lattice electrode, the alumina glass for being coated with golden grid electrode are coated with golden grid electrode magnesia glass；
2nd, the preparation of colloidal solution：The silicon dioxide microsphere that sphere diameter is 200nm-500nm is added to deionized water or second
Single dispersing degree ＜ 5% is obtained in alcoholic solution, the colloid emulsion that mass percent concentration is 0.05-0.3%, then through ultrasonic vibration
It is scattered, obtain silica colloid solution；
3rd, the preparation of colloidal crystal template：Substrate after step 1 is handled is put into silica colloid solution,
Make the solvent volatilization in silica colloid solution under the conditions of being 30 DEG C -70 DEG C in temperature, then again at 600 DEG C of -900 DEG C of heat
6-10h is managed, obtains colloidal crystal template；
4th, carbon covers the preparation of colloidal crystal template：The 0.5-1g concentrated sulfuric acid is added in 25ml deionized waters, Ran Houjia
Enter 5-7g sucrose, after sucrose is completely dissolved, in the colloidal crystal template insertion solution that step 3 is obtained, in vacuum, room
2-4h is kept under conditions of temperature, then the colloidal crystal template for having permeated sucrose is taken out from solution, 5-7h is kept at 100 DEG C,
Then continue to keep 5-7h at 160 DEG C, most after reacting 2-4h at 700-900 DEG C in nitrogen atmosphere, obtain carbon coating Colloidal crystals
Body template；
5th, using carbon coating colloidal crystal template as working electrode, using filamentary silver or saturated calomel electrode as reference electrode, nickel sheet
Or platinized platinum is to electrode, each electrode is ultrasonically treated in acetone, wherein ultrasonic power is 60W-100W, ultrasonic time 5-
15min, then clean with distilled water flushing and dry up, by working electrode, reference electrode and that aniline-Bronsted acid is put into electrode is water-soluble
In liquid, electropolymerization is carried out using chronoamperometry, wherein electropolymerization temperature is 20 DEG C -40 DEG C, and it is 0.7- to control sedimentation potential
0.9V, sedimentation time 200-500s, then using ultrapure water, dry, removing template is removed with 1-5% hydrofluoric acid dips
Afterwards, three-dimensional ordered macroporous polyaniline/carbon compound electrochromic membrane is produced；
Concentration of aniline is 0.1-0.5mol/L in aniline-protonic acid aqueous solution described in step 5, and proton acid concentration is
0.1-1mol/L, the Bronsted acid be sulfuric acid, hydrochloric acid, perchloric acid, camphorsulfonic acid with or DBSA.
Due to the introducing of carbon in the present invention, the electric conductivity of polyaniline is improved so that the electrochromism of polyaniline film
It can significantly improve, coloring and fading time substantially shorten, and the increase of spectral modulation amplitude, have higher coloration efficiency.
Brief description of the drawings
Fig. 1 is the scanning electron microscopic picture for testing gained colloidal crystal template in a step 3；
Fig. 2 is the scanning electron microscopic picture for testing a three-dimensional ordered macroporous polyaniline/carbon compound electrochromic membrane of gained；
Fig. 3 is the SEM sections for testing three-dimensional ordered macroporous polyaniline/carbon compound electrochromic membrane that three step 5 obtain
Figure.
Embodiment
Technical solution of the present invention is not limited to act embodiment set forth below, in addition between each embodiment
Any combination.
Embodiment one：The preparation of the three-dimensional ordered macroporous polyaniline of present embodiment/carbon compound electrochromic membrane
Method follows the steps below：
First, the surface treatment of baseplate material：After substrate is ultrasonically treated in acetone, methanol and ultra-pure water respectively, dry；
Wherein ultrasonic power is 60W-100W, and ultrasonic time 10-60min, the substrate is that thickness is coated with golden grid for 0.5mm-2mm
The quartz glass of lattice electrode, the alumina glass for being coated with golden grid electrode or the magnesia glass for being coated with golden grid electrode；
2nd, the preparation of colloidal solution：The silicon dioxide microsphere that sphere diameter is 200nm-500nm is added to deionized water or second
Single dispersing degree ＜ 5% is obtained in alcoholic solution, the colloid emulsion that mass percent concentration is 0.05-0.3%, then through ultrasonic vibration
It is scattered, obtain silica colloid solution；
3rd, the preparation of colloidal crystal template：Substrate after step 1 is handled is put into silica colloid solution,
Make the solvent volatilization in silica colloid solution under the conditions of being 30 DEG C -70 DEG C in temperature, then again at 600 DEG C of -900 DEG C of heat
6-10h is managed, obtains colloidal crystal template；
4th, carbon covers the preparation of colloidal crystal template：The 0.5-1g concentrated sulfuric acid is added in 25ml deionized waters, Ran Houjia
Enter 5-7g sucrose, after sucrose is completely dissolved, in the colloidal crystal template insertion solution that step 3 is obtained, in vacuum, room
2-4h is kept under conditions of temperature, then the colloidal crystal template for having permeated sucrose is taken out from solution, 5-7h is kept at 100 DEG C,
Then continue to keep 5-7h at 160 DEG C, most after reacting 2-4h at 700-900 DEG C in nitrogen atmosphere, obtain carbon coating Colloidal crystals
Body template；
5th, using carbon coating colloidal crystal template as working electrode, using filamentary silver or saturated calomel electrode as reference electrode, nickel sheet
Or platinized platinum is to electrode, each electrode is ultrasonically treated in acetone, wherein ultrasonic power is 60W-100W, ultrasonic time 5-
15min, then clean with distilled water flushing and dry up, by working electrode, reference electrode and that aniline-Bronsted acid is put into electrode is water-soluble
In liquid, electropolymerization is carried out using chronoamperometry, wherein electropolymerization temperature is 20 DEG C -40 DEG C, and it is 0.7- to control sedimentation potential
0.9V, sedimentation time 200-500s, then using ultrapure water, dry, removing template is removed with 1-5% hydrofluoric acid dips
Afterwards, three-dimensional ordered macroporous polyaniline/carbon compound electrochromic membrane is produced；
Concentration of aniline is 0.1-0.5mol/L in aniline-protonic acid aqueous solution described in step 5, and proton acid concentration is
0.1-1mol/L, the Bronsted acid be sulfuric acid, hydrochloric acid, perchloric acid, camphorsulfonic acid with or DBSA.
Embodiment two：Present embodiment is from ultrasonic power in step 1 unlike embodiment one
80W, ultrasonic time 40min.It is other identical with embodiment one.
Embodiment three：Dioxy in step 2 unlike one of present embodiment and embodiment one or two
SiClx microballoon sphere diameter is 300nm.It is other identical with one of embodiment one or two.
Embodiment four：Colloid in step 2 unlike one of present embodiment and embodiment one to three
The mass percent concentration of emulsion is 0.2%.It is other identical with one of embodiment one to three.
Embodiment five：In temperature in step 3 unlike one of present embodiment and embodiment one to four
Spend to make the solvent in silica colloid solution volatilize under the conditions of 50 DEG C.Other phases one of with embodiment one to four
Together.
Embodiment six：Exist again in step 3 unlike one of present embodiment and embodiment one to five
800 DEG C of heat treatment 8h.It is other identical with one of embodiment one to five.
Embodiment seven：It is last in step 4 unlike one of present embodiment and embodiment one to six
In nitrogen atmosphere 3h is reacted at 800 DEG C.It is other identical with one of embodiment one to six.
Embodiment eight：Ultrasound in step 5 unlike one of present embodiment and embodiment one to seven
Power is 90W, ultrasonic time 10min.It is other identical with one of embodiment one to seven.
Embodiment nine：Voltolisation in step 5 unlike one of present embodiment and embodiment one to eight
It is 30 DEG C to close temperature.It is other identical with one of embodiment one to eight.
Embodiment ten：Deposited in step 5 unlike one of present embodiment and embodiment one to nine
Current potential is 0.8V, sedimentation time 400s.It is other identical with one of embodiment one to nine.
Using following experimental verifications effect of the present invention：
Experiment one：
The preparation method of three-dimensional ordered macroporous polyaniline/carbon compound electrochromic membrane follows the steps below：
First, the surface treatment of baseplate material：After substrate is ultrasonically treated in acetone, methanol and ultra-pure water respectively, dry；
Wherein ultrasonic power is 80W, and ultrasonic time 30min, the substrate is the quartzy glass for being coated with golden grid electrode that thickness is 1mm
Glass；
2nd, the preparation of colloidal solution：The silicon dioxide microsphere that sphere diameter is 375nm is added to deionized water or ethanol solution
In obtain single dispersing degree ＜ 5%, mass percent concentration be 0.2% colloid emulsion, then disperse through ultrasonic vibration, obtain two
Silica gel liquid solution；
3rd, the preparation of colloidal crystal template：Substrate after step 1 is handled is put into silica colloid solution,
Make the solvent volatilization in silica colloid solution under the conditions of being 50 DEG C in temperature, be then heat-treated 8h at 750 DEG C again, obtain glue
Body crystal template；
4th, carbon covers the preparation of colloidal crystal template：The 0.7g concentrated sulfuric acid is added in 25ml deionized waters, then added
6g sucrose, after sucrose is completely dissolved, in the colloidal crystal template insertion solution that step 3 is obtained, in vacuum, room temperature
Under the conditions of keep 3h, then the colloidal crystal template for having permeated sucrose is taken out from solution, 5-7h, Ran Hou is kept at 100 DEG C
160 DEG C are continued to keep 6h, most after reacting 3h at 800 DEG C in nitrogen atmosphere, obtain carbon coating colloidal crystal template；
5th, using carbon coating colloidal crystal template as working electrode, using filamentary silver or saturated calomel electrode as reference electrode, nickel sheet
Or platinized platinum is to electrode, and each electrode is ultrasonically treated in acetone, wherein ultrasonic power is 80W, ultrasonic time 10min, then
It is clean with distilled water flushing and dry up, by working electrode, reference electrode and electrode is put into aniline-protonic acid aqueous solution, made
Electropolymerization is carried out with chronoamperometry, wherein electropolymerization temperature is 30 DEG C, and it is 0.8V to control sedimentation potential, and sedimentation time is
350s, then using ultrapure water, dry, after removing removing template with 3% hydrofluoric acid dips, produce three-dimensional ordered macroporous polyphenyl
Amine/carbon compound electrochromic membrane；
Concentration of aniline is 0.2mol/L in aniline-protonic acid aqueous solution described in step 5, and proton acid concentration is 0.5mol/
L, the Bronsted acid are sulfuric acid.
Fig. 1 is the SEM figures for the colloidal crystal template that step 3 obtains, it can be seen that template belongs to close-packed hexagonal knot from figure
Structure, defect are considerably less；
Experiment two：
The preparation method of three-dimensional ordered macroporous polyaniline/carbon compound electrochromic membrane follows the steps below：
First, the surface treatment of baseplate material：After substrate is ultrasonically treated in acetone, methanol and ultra-pure water respectively, dry；
Wherein ultrasonic power is 60W, and ultrasonic time 10min, the substrate is the oxidation for being coated with golden grid electrode that thickness is 0.5mm
Lead glass；
2nd, the preparation of colloidal solution：The silicon dioxide microsphere that sphere diameter is 200nm is added to deionized water or ethanol solution
In obtain single dispersing degree ＜ 5%, mass percent concentration be 0.05% colloid emulsion, then disperse through ultrasonic vibration, obtain
Silica colloid solution；
3rd, the preparation of colloidal crystal template：Substrate after step 1 is handled is put into silica colloid solution,
Make the solvent volatilization in silica colloid solution under the conditions of being 30 DEG C in temperature, be then heat-treated 6h at 600 DEG C again, obtain glue
Body crystal template；
4th, carbon covers the preparation of colloidal crystal template：The 0.5g concentrated sulfuric acid is added in 25ml deionized waters, then added
5g sucrose, after sucrose is completely dissolved, in the colloidal crystal template insertion solution that step 3 is obtained, in vacuum, room temperature
Under the conditions of keep 2h, then the colloidal crystal template for having permeated sucrose is taken out from solution, 5-7h, Ran Hou is kept at 100 DEG C
160 DEG C are continued to keep 5h, most after reacting 2h at 700 DEG C in nitrogen atmosphere, obtain carbon coating colloidal crystal template；
5th, using carbon coating colloidal crystal template as working electrode, using filamentary silver or saturated calomel electrode as reference electrode, nickel sheet
Or platinized platinum is to electrode, each electrode is ultrasonically treated in acetone, wherein ultrasonic power is 60W, ultrasonic time 5min, then is used
Distilled water flushing is clean and dries up, and by working electrode, reference electrode and electrode is put into aniline-protonic acid aqueous solution, uses
Chronoamperometry carries out electropolymerization, and wherein electropolymerization temperature is 20 DEG C, and it is 0.7V, sedimentation time 200s to control sedimentation potential,
Then ultrapure water is used, dries, after removing removing template with 1% hydrofluoric acid dips, produces three-dimensional ordered macroporous polyaniline/carbon
Compound electrochromic membrane；
Concentration of aniline is 0.1mol/L in aniline-protonic acid aqueous solution described in step 5, and proton acid concentration is 0.1mol/
L, the Bronsted acid are hydrochloric acid.
Fig. 2 is the SEM figures for three-dimensional ordered macroporous polyaniline/carbon compound electrochromic membrane that step 5 obtains, from figure
It can be seen that polyaniline/carbon compound electrochromic membrane replicates the structure of colloidal crystal template well, obtained three-dimensional has
Sequence macroporous structure order is very good.
Experiment three：
The preparation method of three-dimensional ordered macroporous polyaniline/carbon compound electrochromic membrane follows the steps below：
First, the surface treatment of baseplate material：After substrate is ultrasonically treated in acetone, methanol and ultra-pure water respectively, dry；
Wherein ultrasonic power is 100W, and ultrasonic time 60min, the substrate is the oxidation for being coated with golden grid electrode that thickness is 2mm
Magnesium glass；
2nd, the preparation of colloidal solution：The silicon dioxide microsphere that sphere diameter is 500nm is added to deionized water or ethanol solution
In obtain single dispersing degree ＜ 5%, mass percent concentration be 00.3% colloid emulsion, then disperse through ultrasonic vibration, obtain
Silica colloid solution；
3rd, the preparation of colloidal crystal template：Substrate after step 1 is handled is put into silica colloid solution,
Make the solvent volatilization in silica colloid solution under the conditions of being 30 DEG C -70 DEG C in temperature, then again at 600 DEG C of -900 DEG C of heat
6-10h is managed, obtains colloidal crystal template；
4th, carbon covers the preparation of colloidal crystal template：The 1g concentrated sulfuric acid is added in 25ml deionized waters, then adds 7g
Sucrose, after sucrose is completely dissolved, in the colloidal crystal template insertion solution that step 3 is obtained, in the bar of vacuum, room temperature
4h is kept under part, then the colloidal crystal template for having permeated sucrose is taken out from solution, 7h is kept at 100 DEG C, then at 160 DEG C
Continue to keep 7h, most after reacting 4h at 900 DEG C in nitrogen atmosphere, obtain carbon coating colloidal crystal template；
5th, using carbon coating colloidal crystal template as working electrode, using filamentary silver or saturated calomel electrode as reference electrode, nickel sheet
Or platinized platinum is to electrode, and each electrode is ultrasonically treated in acetone, wherein ultrasonic power is 100W, ultrasonic time 15min, then
It is clean with distilled water flushing and dry up, by working electrode, reference electrode and electrode is put into aniline-protonic acid aqueous solution, made
Electropolymerization is carried out with chronoamperometry, wherein electropolymerization temperature is 40 DEG C, and it is 0.9V to control sedimentation potential, and sedimentation time is
500s, then using ultrapure water, dry, after removing removing template with 5% hydrofluoric acid dips, produce three-dimensional ordered macroporous polyphenyl
Amine/carbon compound electrochromic membrane；
Concentration of aniline is 0.5mol/L in aniline-protonic acid aqueous solution described in step 5, and proton acid concentration is 1mol/L,
The Bronsted acid is DBSA.
Fig. 3 is the SEM sectional views for three-dimensional ordered macroporous polyaniline/carbon compound electrochromic membrane that step 5 obtains, from
It can be clearly seen that the μ m-thick of polyaniline/carbon compound electrochromic membrane about 10 on figure, order is preferable.
Claims (10)
1. the preparation method of three-dimensional ordered macroporous polyaniline/carbon compound electrochromic membrane, it is characterised in that three-dimensional ordered macroporous
The preparation method of polyaniline/carbon compound electrochromic membrane follows the steps below：
First, the surface treatment of baseplate material：After substrate is ultrasonically treated in acetone, methanol and ultra-pure water respectively, dry；Wherein
Ultrasonic power is 60W-100W, and ultrasonic time 10-60min, the substrate is that thickness is coated with golden grid electricity for 0.5mm-2mm
The quartz glass of pole, the alumina glass for being coated with golden grid electrode or the magnesia glass for being coated with golden grid electrode；
2nd, the preparation of colloidal solution：The silicon dioxide microsphere that sphere diameter is 200nm-500nm is added to deionized water or ethanol is molten
Single dispersing degree ＜ 5% is obtained in liquid, the colloid emulsion that mass percent concentration is 0.05-0.3%, then through ultrasonic vibration point
Dissipate, obtain silica colloid solution；
3rd, the preparation of colloidal crystal template：Substrate after step 1 is handled is put into silica colloid solution, in temperature
Spend to make the solvent in silica colloid solution volatilize under the conditions of 30 DEG C -70 DEG C, then again in 600 DEG C of -900 DEG C of heat treatment 6-
10h, obtain colloidal crystal template；
4th, carbon covers the preparation of colloidal crystal template：The 0.5-1g concentrated sulfuric acid is added in 25ml deionized waters, then adds 5-
7g sucrose, after sucrose is completely dissolved, in the colloidal crystal template insertion solution that step 3 is obtained, in vacuum, room temperature
Under the conditions of keep 2-4h, then the colloidal crystal template for having permeated sucrose is taken out from solution, keeps 5-7h at 100 DEG C, then
Continue to keep 5-7h at 160 DEG C, most after reacting 2-4h at 700-900 DEG C in nitrogen atmosphere, obtain carbon coating colloidal crystal mould
Plate；
5th, using carbon coating colloidal crystal template as working electrode, using filamentary silver or saturated calomel electrode as reference electrode, nickel sheet or platinum
Piece is to electrode, and each electrode is ultrasonically treated in acetone, and wherein ultrasonic power is 60W-100W, ultrasonic time 5-15min,
It is clean with distilled water flushing again and dry up, by working electrode, reference electrode and electrode is put into aniline-protonic acid aqueous solution,
Electropolymerization is carried out using chronoamperometry, wherein electropolymerization temperature is 20 DEG C -40 DEG C, and it is 0.7-0.9V to control sedimentation potential, is sunk
The product time is 200-500s, then using ultrapure water, dries, after removing removing template with 1-5% hydrofluoric acid dips, produces three
Tie up ordered big hole polyaniline/carbon compound electrochromic membrane；
Concentration of aniline is 0.1-0.5mol/L in aniline-protonic acid aqueous solution described in step 5, and proton acid concentration is 0.1-
1mol/L, the Bronsted acid are sulfuric acid, hydrochloric acid, perchloric acid, camphorsulfonic acid or DBSA.
2. the preparation method of three-dimensional ordered macroporous polyaniline/carbon compound electrochromic membrane according to claim 1, its feature
In step 1 ultrasonic power be 80W, ultrasonic time 40min.
3. the preparation method of three-dimensional ordered macroporous polyaniline/carbon compound electrochromic membrane according to claim 1, its feature
In step 2 silicon dioxide microsphere sphere diameter be 300nm.
4. the preparation method of three-dimensional ordered macroporous polyaniline/carbon compound electrochromic membrane according to claim 1, its feature
It is 0.2% in the mass percent concentration of the colloid emulsion in step 2.
5. the preparation method of three-dimensional ordered macroporous polyaniline/carbon compound electrochromic membrane according to claim 1, its feature
Solvent volatilization in silica colloid solution is made under the conditions of being 50 DEG C in temperature in step 3.
6. the preparation method of three-dimensional ordered macroporous polyaniline/carbon compound electrochromic membrane according to claim 1, its feature
In step 3 8h is being heat-treated at 800 DEG C.
7. the preparation method of three-dimensional ordered macroporous polyaniline/carbon compound electrochromic membrane according to claim 1, its feature
In step 4 most after in nitrogen atmosphere 800 DEG C react 3h.
8. the preparation method of three-dimensional ordered macroporous polyaniline/carbon compound electrochromic membrane according to claim 1, its feature
In step 5 ultrasonic power be 90W, ultrasonic time 10min.
9. the preparation method of three-dimensional ordered macroporous polyaniline/carbon compound electrochromic membrane according to claim 1, its feature
In step 5 electropolymerization temperature be 30 DEG C.
10. the preparation method of three-dimensional ordered macroporous polyaniline/carbon compound electrochromic membrane according to claim 1, it is special
Sign in step 5 sedimentation potential be 0.8V, sedimentation time 400s.
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| US5399450A (en) * | 1989-04-28 | 1995-03-21 | Seiko Epson Corporation | Method of preparation of a color filter by electrolytic deposition of a polymer material on a previously deposited pigment |
| CN102592749A (en) * | 2012-03-08 | 2012-07-18 | 哈尔滨工业大学 | Method of surface self-assembly of graphene/polyimide transparent electric conduction film |
| CN102978674A (en) * | 2012-11-19 | 2013-03-20 | 哈尔滨工业大学 | Preparation method of electrochromic film having photonic crystal structure |
| CN103066283A (en) * | 2013-01-15 | 2013-04-24 | 上海大学 | Method for preparing lithium manganese phosphate material with three-dimensional ordered macroporous structure |
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2015
- 2015-07-13 CN CN201510409030.2A patent/CN105130210B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5399450A (en) * | 1989-04-28 | 1995-03-21 | Seiko Epson Corporation | Method of preparation of a color filter by electrolytic deposition of a polymer material on a previously deposited pigment |
| CN102592749A (en) * | 2012-03-08 | 2012-07-18 | 哈尔滨工业大学 | Method of surface self-assembly of graphene/polyimide transparent electric conduction film |
| CN102978674A (en) * | 2012-11-19 | 2013-03-20 | 哈尔滨工业大学 | Preparation method of electrochromic film having photonic crystal structure |
| CN103066283A (en) * | 2013-01-15 | 2013-04-24 | 上海大学 | Method for preparing lithium manganese phosphate material with three-dimensional ordered macroporous structure |
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