CN107201087A - Prussian blue composition for ink, Prussian blue ink film and its preparation method and application - Google Patents
Prussian blue composition for ink, Prussian blue ink film and its preparation method and application Download PDFInfo
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- CN107201087A CN107201087A CN201710257853.7A CN201710257853A CN107201087A CN 107201087 A CN107201087 A CN 107201087A CN 201710257853 A CN201710257853 A CN 201710257853A CN 107201087 A CN107201087 A CN 107201087A
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- Prior art keywords
- prussian blue
- ink
- surfactant
- composition
- water
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- DCYOBGZUOMKFPA-UHFFFAOYSA-N iron(2+);iron(3+);octadecacyanide Chemical compound [Fe+2].[Fe+2].[Fe+2].[Fe+3].[Fe+3].[Fe+3].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] DCYOBGZUOMKFPA-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 239000013225 prussian blue Substances 0.000 title claims abstract description 69
- 229960003351 prussian blue Drugs 0.000 title claims abstract description 69
- 239000000203 mixture Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 239000004094 surface-active agent Substances 0.000 claims abstract description 57
- 238000000034 method Methods 0.000 claims abstract description 36
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical group FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002736 nonionic surfactant Substances 0.000 claims abstract description 21
- 239000003125 aqueous solvent Substances 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 239000011248 coating agent Substances 0.000 claims description 12
- 238000000576 coating method Methods 0.000 claims description 12
- 239000003960 organic solvent Substances 0.000 claims description 11
- 239000000758 substrate Substances 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- 230000003213 activating effect Effects 0.000 claims description 8
- 238000004528 spin coating Methods 0.000 claims description 7
- NECRQCBKTGZNMH-UHFFFAOYSA-N 3,5-dimethylhex-1-yn-3-ol Chemical group CC(C)CC(C)(O)C#C NECRQCBKTGZNMH-UHFFFAOYSA-N 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000007641 inkjet printing Methods 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- LXOFYPKXCSULTL-UHFFFAOYSA-N 2,4,7,9-tetramethyldec-5-yne-4,7-diol Chemical compound CC(C)CC(C)(O)C#CC(C)(O)CC(C)C LXOFYPKXCSULTL-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- 235000011187 glycerol Nutrition 0.000 claims description 3
- 238000007650 screen-printing Methods 0.000 claims description 3
- 238000007046 ethoxylation reaction Methods 0.000 claims description 2
- 230000005611 electricity Effects 0.000 claims 1
- 239000003471 mutagenic agent Substances 0.000 claims 1
- 231100000707 mutagenic chemical Toxicity 0.000 claims 1
- 239000000049 pigment Substances 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 7
- 239000002270 dispersing agent Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- LDQICAMJIICDLF-UHFFFAOYSA-N potassium;iron(2+);iron(3+);hexacyanide Chemical compound [K+].[Fe+2].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] LDQICAMJIICDLF-UHFFFAOYSA-N 0.000 abstract description 4
- RFKJHQXSLBUONF-UHFFFAOYSA-N methyl blue free acid Chemical compound C1=CC(S(=O)(=O)O)=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=NC=2C=CC(=CC=2)S(O)(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S(O)(=O)=O)=CC=2)C=C1 RFKJHQXSLBUONF-UHFFFAOYSA-N 0.000 abstract 1
- 239000000976 ink Substances 0.000 description 86
- 239000010408 film Substances 0.000 description 42
- 239000002904 solvent Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 238000012360 testing method Methods 0.000 description 6
- 238000001914 filtration Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- 229910002547 FeII Inorganic materials 0.000 description 3
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 3
- PRPAGESBURMWTI-UHFFFAOYSA-N [C].[F] Chemical compound [C].[F] PRPAGESBURMWTI-UHFFFAOYSA-N 0.000 description 3
- -1 anion phosphate Chemical class 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 241001062009 Indigofera Species 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical group [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 206010054949 Metaplasia Diseases 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 150000004696 coordination complex Chemical class 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000015689 metaplastic ossification Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241001561902 Chaetodon citrinellus Species 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- 229910016327 MxWO3 Inorganic materials 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000004984 smart glass Substances 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/50—Sympathetic, colour changing or similar inks
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
- C09D11/037—Printing inks characterised by features other than the chemical nature of the binder characterised by the pigment
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/32—Inkjet printing inks characterised by colouring agents
- C09D11/322—Pigment inks
-
- G—PHYSICS
- G02—OPTICS
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2201/00—Polymeric substrate or laminate
- B05D2201/02—Polymeric substrate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2203/00—Other substrates
- B05D2203/30—Other inorganic substrates, e.g. ceramics, silicon
- B05D2203/35—Glass
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2252/00—Sheets
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Nonlinear Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention discloses a kind of Prussian blue composition for ink and Prussian blue ink film and its preparation method and application, the Prussian blue composition for ink contains water-soluble Prussian blue, surfactant and aqueous solvent；The surfactant is fluorocarbon surfactant and/or nonionic surfactant；Relative to 1mL aqueous solvents, water-soluble Prussian blue content is 10 100mg, and the content of surfactant is 3 30mg.The Prussian blue composition for ink of the disclosure replaces Prussian blue pigment using Soluble Prussian blue, the problem of solving poor Prussian blue pigment dissolubility and additional dispersant influence electrochromic effect, improves dispersiveness of the Prussian blue ink in aqueous solvent.The addition of surfactant significantly reduces the surface tension of water system ink simultaneously, promotes ink to form uniform film in base material.It is simple, with short production cycle using the preparation and last handling process of Prussian blue composition for ink preparation ink film, it is advantageously implemented industrialized production.
Description
Technical field
This disclosure relates to electrochromic material field, in particular it relates to a kind of Prussian blue composition for ink and Prussia
Blue ink film and its preparation method and application.
Background technology
Since finding electrochromism phenomenon from the sixties, this technology with alreading exceed for more than 40 years.Electrochromism is
The material phenomenon that apparent colour changes under extraneous electric field driven, thus can be widely applied to smart window, vehicle dormer window,
The field such as glareproof mirror and display.Electrochromic material includes inorganic material and organic material.Inorganic material is mainly divided
For oxide and metal complex.Wherein metal oxide is topmost is represented as tungsten oxide (WO3), during ion implanting, WO3From
Transparent state is changed into navy blue：
WO3+xe-+xM+→MxWO3
Wherein, M is lithium (Li), sodium (Na) or potassium (K).
It is Prussian blue from depth during ion implanting and most common metal complex is Prussian blue (prussian blue)
Blueness is changed into Transparent color：
Fe4 III(FeII(CN)6)3+4e-+4M+→M4Fe4 II(FeII(CN)6)3
Wherein, M is proton lithium (Li), sodium (Na) or potassium (K) ion.
However, because the dissolubility of prussian blue pigment particles is poor, only forming suspension system in multi-solvents, it is difficult to
Stable solution is formed, its application in liquid phase method prepares electrochromic device film is significantly limit.Currently in order to carrying
High Prussian blue dispersiveness in a solvent, main method is to be combined using suitable dispersant with Prussian blue, increase its
Dispersiveness and stability in liquid phase solvent.But this method compares for the selection of dispersant and the requirement of process for dispersing
It is harsh.
The content of the invention
The purpose of the disclosure is：First aspect can be used for passing through there is provided a kind of Prussian blue composition for ink, the ink
Impact system prepares electrochromic device film；There is provided the ink group that a kind of use disclosure first aspect is provided for second aspect
The method that compound prepares ink film；The third aspect there is provided it is a kind of by disclosure second aspect provided to prepare ink thin
Ink film made by the method for film；Ink or the disclosure that fourth aspect is provided there is provided a kind of disclosure first aspect
Application of the Prussian blue ink film that the third aspect is provided in electrochromic device is prepared.
To achieve these goals, there is provided a kind of Prussian blue composition for ink, said composition for disclosure first aspect
Contain water-soluble Prussian blue, surfactant and aqueous solvent；The surfactant is fluorocarbon surfactant and/or non-
Ionic surface active agent；Relative to aqueous solvent described in 1mL, the Prussian blue content of the water solubility is 10-100mg, described
The content of surfactant is 3-30mg.
Alternatively, the nonionic surfactant is ethoxylated non-ionic surface active agent, and the ethoxylation is non-
Ionic surface active agent be selected from the nonionic surfactant, article number that article number is Dynol 604 be Surfynol 104
Nonionic surfactant, article number be Surfynol 420 nonionic surfactant or article number be Surfynol
At least one of 485 nonionic surfactant；The fluorocarbon surfactant be selected from article number be Zonyl FSJ
The fluorocarbon surface that fluorocarbon surfactant, article number are Zonyl FSE fluorocarbon surfactant, article number is Zonyl FSO
Activating agent or article number are at least one of Capstone (R) FS-64 fluorocarbon surfactant.
Alternatively, the surfactant is fluorocarbon surfactant and nonionic surfactant, the fluorocarbon surface
The weight ratio of activating agent and the nonionic surfactant is 1：(0.01-0.4).
Alternatively, the aqueous solvent is water and/or water-miscible organic solvent；The water-miscible organic solvent is selected from first
At least one of alcohol, ethanol, propyl alcohol, isopropanol, n-butanol, acetone, ethylene glycol or glycerine.
Alternatively, the aqueous solvent is water and water-miscible organic solvent, the volume of the water and water-miscible organic solvent
Than for 1：(0.01-0.5).
Alternatively, the surface tension of the Prussian blue composition for ink is below 30mN/m.
Second aspect includes the disclosure first there is provided a kind of method for preparing Prussian blue ink film, this method
The composition for ink that aspect is provided is coated to substrate after being well mixed, and after heat treatment obtains the Prussian blue ink thin
Film.
Alternatively, the method for the coating includes at least one of blade coating, spin coating, inkjet printing or silk-screen printing.
There is provided made by a kind of method of the preparation ink film provided by disclosure second aspect for the third aspect
Prussian blue ink film；
Composition for ink or disclosure third aspect institute that fourth aspect is provided there is provided a kind of disclosure first aspect
Application of the ink film of offer in electrochromic device is prepared.
The Prussian blue composition for ink of the disclosure replaces Prussian blue pigment using Soluble Prussian blue, solves general
Shandong scholar indigo plant pigment dissolved is poor and the problem of additional dispersant influence electrochromic effect, improves Prussian blue ink in water
Dispersiveness in property solvent.The addition of surfactant significantly reduces the surface tension of water system ink simultaneously, promotes ink
Wetting in low surface tension substrate and sprawl, form uniform Prussian blue ink film.Using the Prussia of the disclosure
The technical process and last handling process that blue ink composition prepares ink film are simple, with short production cycle, are advantageously implemented industry
Metaplasia is produced.
Other feature and advantage of the disclosure will be described in detail in subsequent embodiment part.
Embodiment
Embodiment of this disclosure is described in detail below.It should be appreciated that described herein specific
Embodiment is merely to illustrate and explained the disclosure, is not limited to the disclosure.
Disclosure first aspect there is provided a kind of Prussian blue composition for ink, said composition contain it is water-soluble it is Prussian blue,
Surfactant and aqueous solvent；The surfactant is fluorocarbon surfactant and/or nonionic surfactant；Relatively
In aqueous solvent described in 1mL, the Prussian blue content of the water solubility is 10-100mg, and the content of the surfactant is 3-
30mg。
The Prussian blue composition for ink of the disclosure replaces Prussian blue pigment using Soluble Prussian blue, solves general
Shandong scholar indigo plant pigment dissolved is poor and the problem of additional dispersant influence electrochromic effect, improves Prussian blue ink in water
Dispersiveness in property solvent.The addition of surfactant significantly reduces the surface tension of water system ink simultaneously, promotes ink
Wetting in low surface tension substrate and sprawl, form uniform Prussian blue ink film.Using the Prussia of the disclosure
The technical process and last handling process that blue ink composition prepares ink film are simple, with short production cycle, are advantageously implemented industry
Metaplasia is produced.
In order to further improve the Prussian blue dispersiveness in composition for ink, it is preferable that aqueous relative to described in 1mL
Solvent, the Prussian blue content of the water solubility can be 30-70mg, and the content of the surfactant can be 6-10mg.
According to the disclosure in a first aspect, water-soluble Prussian blue implication is well known to those skilled in the art, molecule
Formula is KFeIIIFeII(CN)6, water solubility is Prussian blue to be easily scattered in water system, can obtain uniform prussian blue nano point
Dispersion liquid.
According to the disclosure in a first aspect, surfactant can play Prussian blue composition for ink viscosity and
The effect of surface tension, makes ink have preferably dispersiveness and film forming, disclosure satisfy that the technological requirement of various painting methods,
With the film of the good different-thickness of forming properties.The nonionic surfactant is preferably that ethoxylated non-ionic surface is lived
Property agent, ethoxylated non-ionic surface active agent can be commercial products, for example, selected from article number for Dynol 604 it is non-from
Sub- surfactant, article number are that Surfynol 104 nonionic surfactant, article number are the non-of Surfynol 420
Ionic surface active agent or article number are at least one of Surfynol 485 nonionic surfactant；The fluorine carbon table
Face activating agent can be commercial products, can be that Zonyl FSJ fluorocarbon surfactant, article number are selected from article number
The fluorocarbon surfactant or article number that Zonyl FSE fluorocarbon surfactant, article number is Zonyl FSO are Capstone
(R) at least one of FS-64 fluorocarbon surfactant；Preferably, nonionic surfactant can be to be produced purchased from air
Product company (Air Products) company's trade mark is for Dynol 604 ethoxylated acetylenic glycols surfactant or purchased from air
Products Co., Ltd (Air Products) company's trade mark is Surfynol 104 ethylene oxide polymerization modified surface active's agent, fluorine carbon
The fluo anion phosphate that it is Zonyl FSE purchased from Du Pont (DuPont Company) company's trade mark that surfactant, which can be,
Surfactant or purchased from Du Pont (DuPont Company) company's trade mark be Zonyl FSO fluorine-containing non-ionic polyoxyethylene
Compound Surfactant.
Wherein, surfactant is preferably fluorocarbon surfactant and nonionic surfactant, it is highly preferred that fluorine carbon table
The weight ratio of face activating agent and nonionic surfactant can be 1：(0.01-0.4).In above-mentioned preferred content range,
The composition for ink has more preferable film-formability energy and dispersiveness, and the ink film prepared using the composition for ink is had more
Good electrochromic property.
According to the disclosure in a first aspect, aqueous solvent can be water and/or water-miscible organic solvent；The water solubility has
Machine solvent can be the conventional water-miscible solvent in this area, be preferably selected from methanol, ethanol, propyl alcohol, isopropanol, positive fourth
At least one of alcohol, acetone, ethylene glycol or glycerine.
In order to further improve the dispersiveness of composition for ink, quality of forming film be improved, it is further preferred that aqueous solvent can
Think water and water-miscible organic solvent, the volume ratio of water and water-miscible organic solvent is preferably 1：(0.01-0.5).
According to the disclosure in a first aspect, the surface tension of Prussian blue composition for ink can become interior in a big way
Change, in order to further improve under the dispersiveness and filming performance of ink, preferable case, the surface tension of the ink can be
Below 30mN/m, more preferably 15-25mN/m.
The second aspect of the disclosure is there is provided a kind of method for preparing Prussian blue ink film, and this method includes inciting somebody to action this
The composition for ink that open first aspect is provided is coated to substrate after being well mixed, and after heat treatment obtains the Prussia
Blue ink film.
Wherein, substrate material can be conventional kind, and the substrate can be selected from ITO electro-conductive glass, FTO electro-conductive glass
Or at least one of AZO electro-conductive glass, preferably flexible substrates, flexible substrates are preferably PET-ITO substrates or PEN-ITO
At least one of substrate.The implication of above-mentioned base material is well known to those skilled in the art, and here is omitted.
According to the second aspect of the disclosure, this method can also include：The ink group that disclosure first aspect is provided
Compound is stirred successively after mixing, ultrasonic and filtering.Stirring, ultrasound and filtering are well-known to those skilled in the art, are stirred
Mixing and stirring ultrasound is used for each component in dispersible ink composition, reduces precipitation, and mixing time can be able to be with 0.1-5h, supersonic frequency
20-40kHz, the time can be 1-10min；Filtration treatment is used to filter the sediment fraction in composition for ink, prevents printer
Shower nozzle is blocked and improves printing effect, and its filtering accuracy can be 0.1-0.5 μm.
According to the second aspect of the disclosure, ink film progress heating can be removed into aqueous solvent, heat treatment
Temperature can be 90-150 DEG C, and preferably 100-120 DEG C, heat treatment time can be 5-30min, preferably 10-25min.Should
Method in the particular/special requirement environment such as vacuum drying chamber, nitrogen glove box without removing excess of solvent, it is not required that in infrared lamp
Post-processed with the light conditions such as laser, simplify the preparation process of ink film.
According to the second aspect of the disclosure, the method for the coating can be that composition for ink can be made to form the normal of film
Rule method, preferably at least one of blade coating, spin coating, inkjet printing or silk-screen printing.
When the composition for ink of the disclosure uses knife coating procedure, by the constituent content and blade coating bar that change composition for ink
Part (speed, baseplate temp, blade coating height) can obtain the ink film that thickness is 50-500nm；During using spin coating method, change
The constituent content and spin coating rotating speed of composition for ink can obtain the ink film that thickness is 20-200nm；In order to realize ink film
It is quick be prepared on a large scale, save ink material, the method for the coating is preferably inkjet printing, more preferably lasting ink-jet
Printing, voltage during ink-jet is preferably more than 20V, and the ink film thickness that ink-jet printing process is prepared is generally 0.05-1 μ
M, preferably 0.05-0.2 μm.
There is provided made by a kind of method of the preparation ink film provided by disclosure second aspect for the third aspect
Prussian blue ink film.The Prussian blue ink film of the disclosure can be used for preparing electrochromic device, can also use
In electro-catalysis and energy storage field.
What the ink or the disclosure third aspect that fourth aspect is provided there is provided a kind of disclosure first aspect were provided
Application of the ink film in electrochromic device is prepared.
The disclosure will be further illustrated by embodiment below, but the disclosure is not therefore any way limited.
In following embodiments of the disclosure, water-soluble Prussian blue purchased from Sigma-Aldrich companies, article No. is 03899-25G；Fluorine
Carbon surface active agent is purchased from E.I.Du Pont Company, and the trade mark is Capstone FS-64；Nonionic surfactant is public purchased from air products
(Air Products) company of department, the trade mark is Dynol-604；Remaining reagent is commercial products.
Embodiment 1
The present embodiment is used to illustrate ink of the disclosure and preparation method thereof.
Weigh 300mg fluorocarbon surfactant Capstone FS-64 and 20mg nonionic table respectively by liquid-transfering gun
Face activating agent Dynol-604, and be slowly added to be sufficiently stirred for 2h in the 20mL vials containing 10g deionized waters；Weigh 500mg
Soluble Prussian blue powder, add in above-mentioned solution, be sufficiently stirred for 2h, obtain the Prussian blue combination of inks of the present embodiment
Thing.
Using ITO/PET as matrix, above-mentioned ink is scratched, the Prussian blue ink film of the present embodiment is obtained.
Embodiment 2-7
The composition and content of Prussian blue composition for ink are shown in Table 1, and the step of embodiment 1 is respectively adopted prepares ink
Composition and Prussian blue ink film.
In embodiment 7, using ITO/PET as matrix, above-mentioned composition for ink is coated using spin-coating method, the present embodiment is obtained
Prussian blue ink film.
Comparative example 1
This comparative example is used to illustrate the composition for ink different from the disclosure.
Using the raw material and preparation method of embodiment 1, except that, the composition for ink of this comparative example does not contain surface
Activating agent.
Comparative example 2
Using the raw material and preparation method of embodiment 1, except that, fluorocarbon surfactant and non-ionic surface are lived
Property agent replace with isoreactivity group molar ratio anionic surfactant sodium dodecylbenzene sulfonate (purchased from Shanghai Ling Feng chemistry
Reagent Co., Ltd, lot number is Lot.No.20131106).
Comparative example 3
By 0.65g Prussian blue pigment powders (Aldrich, 99.9%) and 0.13g Disperbyk-2001 (BYK, one
Kind of dispersant containing acrylic), 0.33g Ludox (a kind of inorganic binder) and 11g ethanol mix, and use shaking machine (Red
Devil) disperseed, to obtain the composition of nano-dispersed.
Sheet resistance is cut into 5 × 5cm for 10 Ω/ ito glass2Size, wash simultaneously dry.Then, exist
Prussian blue coating solution 30s described in spin coating under 1000rpm.It is heat-treated at 150 DEG C after 30min, obtains prussian blue coating film.
The thickness of resulting prussian blue coating film is about 340nm.
Testing example 1
The viscosity and surface tension of testing example 1-7 and comparative example 1-3 Prussian blue composition for ink, test result
Table 2 is listed in, wherein ink viscosity is measured by the U.S.'s portable viscosity apparatus of Rheosense microVISC, and surface tension is used
The full-automatic surface tension instruments of BZY-101 are measured by platinum plate method.
The thickness and light transmittance of testing example 1-7 and comparative example 1-3 Prussian blue ink film, test result are listed in
Table 2, wherein film thickness are measured by KLA Tencor D100 step instruments, and the method for testing of light transmittance passes through Japan
Shimadzu UV-3600 spectrophotometers are measured.
Table 1
Table 2
According to the data of table 1, contrasted from embodiment 1-7 and comparative example 1-3, the Prussian blue composition for ink of the disclosure
With more preferable filming performance, the Prussian blue ink film light transmittance of preparation is more preferable.
It is that volume ratio is 1 in the preferred aqueous solvent of the disclosure from the data comparison of embodiment 6 and embodiment 1：
In the case of the water and water-miscible organic solvent of (0.01-0.5), the Prussian blue composition for ink of the disclosure has suitable glue
Degree and surface tension, while the Prussian blue ink film light transmittance prepared is higher.
The preferred embodiment of the disclosure described in detail above, still, the disclosure are not limited in above-mentioned embodiment
Detail, in the range of the technology design of the disclosure, a variety of simple variants can be carried out with technical scheme of this disclosure, this
A little simple variants belong to the protection domain of the disclosure.
It is further to note that each particular technique feature described in above-mentioned embodiment, in not lance
In the case of shield, it can be combined by any suitable means.In order to avoid unnecessary repetition, the disclosure to it is various can
The combination of energy no longer separately illustrates.
In addition, can also be combined between a variety of embodiments of the disclosure, as long as it is without prejudice to originally
Disclosed thought, it should equally be considered as disclosure disclosure of that.
Claims (10)
1. a kind of Prussian blue composition for ink, it is characterised in that：Said composition contains water-soluble Prussian blue, surfactant
And aqueous solvent；The surfactant is fluorocarbon surfactant and/or nonionic surfactant；
Relative to aqueous solvent described in 1mL, the Prussian blue content of the water solubility is 10-100mg, the surfactant
Content is 3-30mg.
2. composition according to claim 1, it is characterised in that：The nonionic surfactant be ethoxylation it is non-from
Sub- surfactant, the ethoxylated non-ionic surface active agent is selected from the non-ionic surface that article number is Dynol 604
The nonionic table that activating agent, article number are Surfynol 104 nonionic surfactant, article number is Surfynol 420
Face activating agent or article number are at least one of Surfynol 485 nonionic surfactant；The fluoro-carbon surface active
Agent be selected from the fluorocarbon surfactant that article number is Zonyl FSJ, the fluorocarbon surfactant that article number is Zonyl FSE,
During the fluorocarbon surfactant or article number that article number is Zonyl FSO are Capstone (R) FS-64 fluorocarbon surfactant
At least one.
3. composition according to claim 1, it is characterised in that：The surfactant is fluorocarbon surfactant and non-
The weight ratio of ionic surface active agent, the fluorocarbon surfactant and the nonionic surfactant is 1：(0.01-
0.4)。
4. composition according to claim 1, it is characterised in that：The aqueous solvent is water and/or water-soluble organic molten
Agent；The water-miscible organic solvent is in methanol, ethanol, propyl alcohol, isopropanol, n-butanol, acetone, ethylene glycol or glycerine
At least one.
5. composition according to claim 1, it is characterised in that：The aqueous solvent be water and water-miscible organic solvent,
The volume ratio of the water and water-miscible organic solvent is 1：(0.01-0.5).
6. composition according to claim 1, it is characterised in that：The surface tension of the Prussian blue composition for ink is
Below 30mN/m.
7. a kind of method for preparing Prussian blue ink film, it is characterised in that：This method includes will be any in claim 1-6
Composition described in one is coated to substrate after being well mixed, and after heat treatment obtains the Prussian blue ink film.
8. method according to claim 7, it is characterised in that：The method of the coating includes blade coating, spin coating, inkjet printing
At least one of or silk-screen printing.
9. the Prussian blue ink film that the method according to claim 7 or 8 is prepared.
10. the Prussian blue ink film described in composition or claim 9 in claim 1-6 described in any one is in electricity
Application in mutagens color device.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4498739A (en) * | 1981-05-26 | 1985-02-12 | Seiko Instruments & Electronics Ltd. | Electrochromic display devices using iron(III) hexacyanoferrate(II) salt |
| CN101389720A (en) * | 2006-02-27 | 2009-03-18 | 株式会社理光 | Inkjet recording device and inkjet recording method |
| CN101395244A (en) * | 2006-03-06 | 2009-03-25 | Skc株式会社 | Preparation of Prussian Blue Coating Films for Electrochromic Devices |
-
2017
- 2017-04-19 CN CN201710257853.7A patent/CN107201087A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4498739A (en) * | 1981-05-26 | 1985-02-12 | Seiko Instruments & Electronics Ltd. | Electrochromic display devices using iron(III) hexacyanoferrate(II) salt |
| CN101389720A (en) * | 2006-02-27 | 2009-03-18 | 株式会社理光 | Inkjet recording device and inkjet recording method |
| CN101395244A (en) * | 2006-03-06 | 2009-03-25 | Skc株式会社 | Preparation of Prussian Blue Coating Films for Electrochromic Devices |
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Application publication date: 20170926 |