CN110129850A - A kind of stepped depositions preparation method of ferrocyanide iron thin film - Google Patents
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Abstract
The present invention relates to a kind of stepped depositions preparation method of ferrocyanide iron thin film, the step of carrying out substep electro-deposition, is: the configuration of precursor solution；Prepare before deposition；Deposition process；Stepped depositions.The present invention provides a kind of electrochemical deposition method applied to ferrocyanide iron thin film, the Prussian blue film that thickness is uniform, surface is smooth, thicker is obtained during the deposition process；It is easy to operate when deposition, expensive experimental facilities is omitted, reduces coating cost.
Description
Technical field
The invention belongs to electrochomeric films technologies of preparing, are related to a kind of stepped depositions preparation side of ferrocyanide iron thin film
Method.
Background technique
Electrochromism (Electrochromic, EC) material be characterized in external voltage drive under, material it is optical
Matter is changed by electrochemical redox reaction.This function makes electrochromic material be applied in many fields, example
Such as smart window, automobile anti-dazzle back vision mirror, high comparison display, the research of devices field have pushed the hair of electrochromism technology
Exhibition.
Electrochromism (EC) material is divided into two major classes: inorganic material and organic material.Organic electrochromic material easily carries out
MOLECULE DESIGN, rich in color and color change are fast, absorbing wavelength range is wide, but its unstable chemcial property, water oxygen and ultraviolet
Resistance is poor, it is cumbersome, at high cost to prepare.Inorganic electrochromic material stable structure, color change is slow, by water in air and oxygen shadow
Sound is smaller, and is hardly influenced by solar ultraviolet, has preferable weatherability, it is people pass that these advantages, which make it extensively,
Note.
Prussian blue (Prussian blue, PB) is a kind of inorganic EC material, he is the compound of mixed valence, general formula
For MI x[MII y(CN)6].For PB, MI, MIIFor the ion (Fe of two kinds of valence states of Fe2+, Fe3+), different redox
Under voltage, PB can be brown (PX) in Prussia, and Prussian green (PG) is Prussian blue (PB), converts between Prussia white (PW), color
In brown, green, it is blue and colourless between changed, it is irreversible state that PX, which is the lower acquisition in PB complete oxidation,
In practical application mainly using PB blue and it is colourless between reversible transition, its main feature is that fast response time, cyclical stability is high, oxygen
The process for changing reduction is as follows:
[FeIIIFeII(CN)6]-(PB)→FeIII[{FeIII(CN)6}2/3{FeII(CN)6}1/3]1/3-(PG)+2/3e-
[FeIIIFeII(CN)6]-(PB)→[FeIIIFeIII(CN)6]0(PX)+e-
[FeIIIFeII(CN)6]-(PB)→[FeIIFeII(CN)6]2-(PW)-e-
There are many kinds of the methods for preparing PB film, such as can to prepare invertibity good Prussian blue thin for spray pyrolysis
Film, referring to " A simple chemical method for deposition of electrochromic Prussian
Blue thin films ", Demiri S, Najdoski M, Velevska J. etc. writes, " Materials Research
Bulletin ", 46 phases in 2011, P.2484.Constant potential electrodeposition process can prepare the uniform prussian blue nano film in surface, ginseng
See " Visible photoelectrochemical sensing platform by situ generated CdS
quantum dots decorated branched-TiO2 nanorods equipped with Prussian blue
Electrochromic display ", Yanhu Wanga, Shenguang Gea etc. writes, " Biosensors and
Bioelectronics ", 89 phases in 2017, P.859.Hydro-thermal method can prepare with the good PB film of substrate adhesiveness, referring to
“Electrochromic properties of hydrothermally grown Prussian blue film and
Device ", Qian J, Ma D, Xu Z etc. writes, " Solar Energy Materials&Solar Cells ", and 2018 177
Phase, P.9.The shortcomings that above-mentioned preparation method is: the PB Film Optics contrast that spray pyrolysis is prepared is not high；Constant voltage deposition
Method and the PB film surface of hydro-thermal method preparation are coarse, in uneven thickness.
Summary of the invention
The object of the present invention is to provide a kind of electrochemical deposition methods applied to electrochromism PB film, solve heavy
As discoloration PB film thickness increases during product, and lead to technical problem in uneven thickness, rough, especially needle
When increasing to 200nm or more, preferably 250nm or more to discoloration PB film thickness, the extreme of thickness is uneven and surface it is thick
It is rough.
The technical scheme is that a kind of stepped depositions preparation method of ferrocyanide iron thin film, the potassium ferricyanide
Film thickness is in 200nm or more, and especially in 250nm or more, the step of carrying out electro-deposition is as follows:
The preparation of step 1, precursor solution: by a certain amount of potassium ferricyanide powder and ferric trichloride powder be dissolved in from
Precursor solution is formed in sub- water, wherein potassium ferricyanide concentration be 0.005~0.5mol/L, ferric trichloride concentration be 0.005~
0.5mol/L, and hydrochloric acid is added, the concentration of hydrochloric acid be added is 0.002~0.9mol/L；Capable of effectively dropping for hydrochloric acid is added
It sinks the size of poly- particle in low solution, prevents ferrocyanide iron particle rapid polymerization from precipitating；
Prepare before step 2, deposition: precursor solution being placed in electrolytic cell, the substrate of transparency conducting layer will be coated with, to electricity
Pole and reference electrode are immersed in precursor solution, and the substrate for being coated with transparency conducting layer is working electrode, are coated with transparency conducting layer
Substrate and the cathode of electrolysis power connect, the anode of electrode and electrolysis power is connected, described is that be coated with ITO saturating to electrode
Electrode, platinum electrode, platinum electrode, foil electrode, stainless steel electrode or the graphite electrode of bright conductive layer, using filamentary silver or platinum filament as
Reference electrode, reference electrode are placed on working electrode and between electrodes；
Step 3, stepped depositions process: it is carried out in the substrate for being coated with transparency conducting layer and to DC voltage is applied between electrode
Multiple electro-deposition, one single deposition time are no more than 10s, and the DC voltage is no more than -1V, and number is to reach target thickness
Only.
Further, rear every time to take out transparent conductive substrate in the step 3, it is rinsed with deionized water, until cleaning table
The precursor solution of face remnants, then put naturally dry in air.
Further, the DC voltage is -0.01V~-1V.
Further, the transparency conducting layer being coated in the substrate of transparency conducting layer is ITO material or FTO material.
Further, potassium ferricyanide concentration is 0.005~0.5mol/L in the precursor solution of step 1.
Further, ferric trichloride concentration is 0.005~0.5mol/L in the precursor solution of step 1.
Further, the concentration of hydrochloric acid is 0.005~0.5mol/L in step 1.
Further, the one single deposition time is 1s~5s.It preferably, is 1s.
Further, the ratio between frequency of depositing and sedimentation time are not less than 1.5 number/seconds.
The invention has the advantages that providing a kind of electrochemical deposition method applied to electrochromism PB film, depositing
The PB film that thickness is uniform, surface is smooth, thickness is thicker is obtained in journey；It is easy to operate when deposition, expensive experiment is omitted and sets
It is standby, reduce coating cost.
Specific embodiment
The present invention is described in further details below.A kind of stepped depositions preparation method of ferrocyanide iron thin film,
The step of carrying out electro-deposition is as follows:
Embodiment 1
1, the preparation of precursor solution: in deionized water by a certain amount of potassium ferricyanide, the dissolution of ferric trichloride powder,
Middle potassium ferricyanide concentration is 0.005~0.5mol/L, ferric trichloride concentration is 0.005~0.5mol/L, and hydrochloric acid, salt is then added
The concentration of acid is 0.005~0.5mol/L；
2, prepare before deposition: precursor solution be placed in electrolytic cell, the substrate of transparency conducting layer will be coated with, to electrode and
Reference electrode is immersed in precursor solution, and the cathode of the substrate and power supply that are coated with transparency conducting layer connects, to electrode and power supply
Anode connection, it is described to electrode be transparent conductive layer, platinum electrode, platinum electrode, foil electrode, stainless steel electrode or
Graphite electrode is put between two electrodes using filamentary silver or platinum filament as reference electrode；
3, be distributed deposition process: under room temperature, the substrate for being coated with transparency conducting layer and to application -0.01V between electrode~-
The DC voltage of 1V carries out electro-deposition, and sedimentation time is 1s~10s；Take out transparent conductive substrate after every deposition is primary, spend from
Sub- water rinses, and until the precursor solution of clean surface residual, then puts naturally dry in air, then proceedes to before putting it into
It drives in liquid solution, repeats 3, to increase film thickness, number of repetition is until reaching target thickness.
Embodiment 2
In deionized water, then appropriate hydrochloric acid is added dropwise in a certain amount of potassium ferricyanide, the dissolution of ferric trichloride powder, is configured to
The potassium ferricyanide containing 0.025mol/L, 0.025mol/L ferric trichloride, 0.025mol/L hydrochloric acid precursor solution.Taking platinized platinum is work
Make electrode, filamentary silver is reference electrode, is coated with the substrate of transparency conducting layer as working electrode, is immersed in precursor solution together
In, the constant deposition voltage of application -0.01V, time 1s is deposited twice, is taken out transparent conductive substrate after depositing for the first time, put
It is rinsed in pond, until the precursor solution of clean surface residual, then puts naturally dry in air, then proceed to be put
Enter in precursor solution, obtains the PB film of 250~350nm.
Embodiment 3
In deionized water, then appropriate hydrochloric acid is added dropwise in a certain amount of potassium ferricyanide, the dissolution of ferric trichloride powder, is configured to
The potassium ferricyanide containing 0.025mol/L, 0.025mol/L ferric trichloride, 0.025mol/L hydrochloric acid precursor solution.Taking platinized platinum is work
Make electrode, filamentary silver is reference electrode, is coated with the substrate of transparency conducting layer as working electrode, is immersed in precursor solution together
In, the constant deposition voltage of application -0.01V, time 1s deposits primary rear taking-up transparent conductive substrate, is placed on pond Zhong Chong
It washes, the precursor solution until cleaning surface residual then puts naturally dry in air, then proceedes to put it into presoma molten
In liquid, repeated deposition 2 times, the PB film of 500~600nm is obtained.
Embodiment 4
In deionized water, then appropriate hydrochloric acid is added dropwise in a certain amount of potassium ferricyanide, the dissolution of ferric trichloride powder, is configured to
The potassium ferricyanide containing 0.025mol/L, 0.025mol/L ferric trichloride, 0.025mol/L hydrochloric acid precursor solution.Taking platinized platinum is work
Make electrode, filamentary silver is reference electrode, is coated with the substrate of transparency conducting layer as working electrode, is immersed in precursor solution together
In, the constant deposition voltage of application -0.01V, time 1s deposits primary rear taking-up transparent conductive substrate, is placed on pond Zhong Chong
It washes, the precursor solution until cleaning surface residual then puts naturally dry in air, then proceedes to put it into presoma molten
In liquid, repeated deposition 3 times, the PB film of 600~700nm is obtained.
Embodiment 5
In deionized water, then appropriate hydrochloric acid is added dropwise in a certain amount of potassium ferricyanide, the dissolution of ferric trichloride powder, is configured to
The potassium ferricyanide containing 0.025mol/L, 0.025mol/L ferric trichloride, 0.025mol/L hydrochloric acid precursor solution.Taking platinized platinum is work
Make electrode, filamentary silver is reference electrode, is coated with the substrate of transparency conducting layer as working electrode, is immersed in precursor solution together
In, the constant deposition voltage of application -0.01V, time 5s deposits primary rear taking-up transparent conductive substrate, is placed on pond Zhong Chong
It washes, until the precursor solution of clean surface residual, then puts naturally dry in air, obtain the PB film of 400~500nm.
Embodiment 6
In deionized water, then appropriate hydrochloric acid is added dropwise in a certain amount of potassium ferricyanide, the dissolution of ferric trichloride powder, is configured to
The potassium ferricyanide containing 0.0125mol/L, 0.0125mol/L ferric trichloride, 0.0125mol/L hydrochloric acid precursor solution.Take platinized platinum
For working electrode, filamentary silver is reference electrode, is coated with the substrate of transparency conducting layer as working electrode, it is molten to be immersed in presoma together
In liquid, the constant deposition voltage of application -0.01V, time 1s deposits primary rear taking-up transparent conductive substrate, is placed in pond
It rinses, until the precursor solution of clean surface residual, then puts naturally dry in air, then proceed to put it into presoma
In solution, repeated deposition 2 times, the PB film of 200nm is obtained.
Embodiment 7
In deionized water, then appropriate hydrochloric acid is added dropwise in a certain amount of potassium ferricyanide, the dissolution of ferric trichloride powder, is configured to
The potassium ferricyanide containing 0.0125mol/L, 0.0125mol/L ferric trichloride, 0.0125mol/L hydrochloric acid precursor solution.Take platinized platinum
For working electrode, filamentary silver is reference electrode, is coated with the substrate of transparency conducting layer as working electrode, it is molten to be immersed in presoma together
In liquid, the constant deposition voltage of application -0.01V, time 1s deposits primary rear taking-up transparent conductive substrate, is placed in pond
It rinses, until the precursor solution of clean surface residual, then puts naturally dry in air, then proceed to put it into presoma
In solution, repeated deposition 3 times, the PB film of 200~270nm is obtained.
Embodiment 8
In deionized water, then appropriate hydrochloric acid is added dropwise in a certain amount of potassium ferricyanide, the dissolution of ferric trichloride powder, is configured to
The potassium ferricyanide containing 0.0125mol/L, 0.0125mol/L ferric trichloride, 0.0125mol/L hydrochloric acid precursor solution.Take platinized platinum
For working electrode, filamentary silver is reference electrode, is coated with the substrate of transparency conducting layer as working electrode, it is molten to be immersed in presoma together
In liquid, the constant deposition voltage of application -0.01V, time 1s deposits primary rear taking-up transparent conductive substrate, is placed in pond
It rinses, until the precursor solution of clean surface residual, then puts naturally dry in air, then proceed to put it into presoma
In solution, repeated deposition 4 times, the PB film of 270~350nm is obtained.
Embodiment 9
In deionized water, then appropriate hydrochloric acid is added dropwise in a certain amount of potassium ferricyanide, the dissolution of ferric trichloride powder, is configured to
The potassium ferricyanide containing 0.0125mol/L, 0.0125mol/L ferric trichloride, 0.0125mol/L hydrochloric acid precursor solution.Take platinized platinum
For working electrode, filamentary silver is reference electrode, is coated with the substrate of transparency conducting layer as working electrode, it is molten to be immersed in presoma together
In liquid, the constant deposition voltage of application -0.01V, time 1s deposits primary rear taking-up transparent conductive substrate, is placed in pond
It rinses, until the precursor solution of clean surface residual, then puts naturally dry in air, then proceed to put it into presoma
In solution, repeated deposition 5 times, the PB film of 500~650nm is obtained.
Embodiment 10
In deionized water, then appropriate hydrochloric acid is added dropwise in a certain amount of potassium ferricyanide, the dissolution of ferric trichloride powder, is configured to
The potassium ferricyanide containing 0.0125mol/L, 0.0125mol/L ferric trichloride, 0.0125mol/L hydrochloric acid precursor solution.Take platinized platinum
For working electrode, filamentary silver is reference electrode, is coated with the substrate of transparency conducting layer as working electrode, it is molten to be immersed in presoma together
In liquid, the constant deposition voltage of application -0.01V, time 1s deposits primary rear taking-up transparent conductive substrate, is placed in pond
It rinses, until the precursor solution of clean surface residual, then puts naturally dry in air, then proceed to put it into presoma
In solution, repeated deposition 6 times, the PB film of 580~650nm is obtained.
In deionized water, then appropriate hydrochloric acid is added dropwise in a certain amount of potassium ferricyanide, the dissolution of ferric trichloride powder, is configured to
Containing the potassium ferricyanide, ferric trichloride, hydrochloric acid precursor solution.Taking platinized platinum is working electrode, and filamentary silver is reference electrode, is coated with ITO
The substrate of transparency conducting layer is immersed in precursor solution together as working electrode, and design parameter is as follows
Claims (10)
1. a kind of stepped depositions preparation method of ferrocyanide iron thin film, the potassium ferricyanide film thickness in 200nm or more, into
The step of row electro-deposition, is as follows:
The preparation of step 1, precursor solution: before potassium ferricyanide powder and the dissolution of ferric trichloride powder are formed in deionized water
Liquid solution is driven, wherein potassium ferricyanide concentration is 0.005~0.5mol/L, and ferric trichloride concentration is 0.005~0.5mol/L, and
Hydrochloric acid is added, the concentration of hydrochloric acid be added is 0.002~0.9mol/L；
Prepare before step 2, deposition: precursor solution be placed in electrolytic cell, the substrate of transparency conducting layer will be coated with, to electrode and
Reference electrode is immersed in precursor solution, and the substrate for being coated with transparency conducting layer is working electrode, is coated with the base of transparency conducting layer
The connection of the cathode of plate and electrolysis power connects the anode of electrode and electrolysis power, and described is to be coated with transparent to lead to electrode
Electrode, platinum electrode, platinum electrode, foil electrode, stainless steel electrode or the graphite electrode of electric layer, using filamentary silver or platinum filament as reference
Electrode, reference electrode are placed on working electrode and between electrodes；
Step 3, stepped depositions process: it is carried out repeatedly in the substrate for being coated with transparency conducting layer and to DC voltage is applied between electrode
Electro-deposition, one single deposition time are no more than 10s, and the DC voltage is no more than -1V, and number is until reaching target thickness.
2. a kind of stepped depositions preparation method of ferrocyanide iron thin film as described in claim 1, it is characterised in that: the iron
Potassium cyanide film thickness is in 250nm or more.
3. a kind of stepped depositions preparation method of ferrocyanide iron thin film as described in claim 1, it is characterised in that: the step
It is rear every time to take out transparent conductive substrate in rapid 3, it is rinsed with deionized water, until the precursor solution of clean surface residual, then is put
Naturally dry in air.
4. a kind of stepped depositions preparation method of ferrocyanide iron thin film as described in claim 1, it is characterised in that: described straight
Galvanic electricity pressure is -0.01V~-1V.
5. a kind of stepped depositions preparation method of ferrocyanide iron thin film as described in claim 1, it is characterised in that: the plating
Having the transparency conducting layer in the substrate of transparency conducting layer is ITO material or FTO material.
6. a kind of stepped depositions preparation method of ferrocyanide iron thin film as described in claim 1, it is characterised in that: step 1
Precursor solution in potassium ferricyanide concentration be 0.005~0.5mol/L.
7. a kind of stepped depositions preparation method of ferrocyanide iron thin film as described in claim 1, it is characterised in that: step 1
Precursor solution in ferric trichloride concentration be 0.005~0.5mol/L.
8. a kind of stepped depositions preparation method of ferrocyanide iron thin film as described in claim 1, it is characterised in that: step 1
The concentration of middle hydrochloric acid is 0.005~0.5mol/L.
9. a kind of stepped depositions preparation method of ferrocyanide iron thin film as described in claim 1, it is characterised in that: deposition time
The ratio between several and sedimentation time is not less than 1.5 number/seconds.
10. a kind of stepped depositions preparation method of ferrocyanide iron thin film as described in claim 1, it is characterised in that: single
Sedimentation time is 1s~5s.It preferably, is 1s.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110947387A (en) * | 2019-11-25 | 2020-04-03 | 中国工程物理研究院材料研究所 | Preparation method and application of nickel-iron double metal hydroxide nano film material |
| CN113777856A (en) * | 2021-08-24 | 2021-12-10 | 同济大学 | Method for regulating and controlling non-linear absorption performance of Prussian blue film and Prussian blue film |
| CN113867065A (en) * | 2021-11-15 | 2021-12-31 | 西北工业大学 | Preparation method of prussian blue electrochromic film |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0068634A1 (en) * | 1981-05-26 | 1983-01-05 | SEIKO INSTRUMENTS & ELECTRONICS LTD. | A process of making iron (III) hexacyanoferrate (II) and to iron (III) hexacyanoferrate (II) made thereby |
| US4818352A (en) * | 1985-06-04 | 1989-04-04 | Central Glass Company, Limited | Electrodeposition of functional film on electrode plate relatively high in surface resistivity |
-
2019
- 2019-04-29 CN CN201910355440.1A patent/CN110129850B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0068634A1 (en) * | 1981-05-26 | 1983-01-05 | SEIKO INSTRUMENTS & ELECTRONICS LTD. | A process of making iron (III) hexacyanoferrate (II) and to iron (III) hexacyanoferrate (II) made thereby |
| US4818352A (en) * | 1985-06-04 | 1989-04-04 | Central Glass Company, Limited | Electrodeposition of functional film on electrode plate relatively high in surface resistivity |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110947387A (en) * | 2019-11-25 | 2020-04-03 | 中国工程物理研究院材料研究所 | Preparation method and application of nickel-iron double metal hydroxide nano film material |
| CN110947387B (en) * | 2019-11-25 | 2022-07-01 | 中国工程物理研究院材料研究所 | Preparation method and application of nickel-iron double metal hydroxide nano film material |
| CN113777856A (en) * | 2021-08-24 | 2021-12-10 | 同济大学 | Method for regulating and controlling non-linear absorption performance of Prussian blue film and Prussian blue film |
| CN113777856B (en) * | 2021-08-24 | 2023-08-29 | 同济大学 | Method for regulating nonlinear absorption performance of Prussian blue film and Prussian blue film |
| CN113867065A (en) * | 2021-11-15 | 2021-12-31 | 西北工业大学 | Preparation method of prussian blue electrochromic film |
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