CN106634215A - Nano indium ink for flexible electronic devices as well as preparation method and application of nano indium ink - Google Patents
Nano indium ink for flexible electronic devices as well as preparation method and application of nano indium ink Download PDFInfo
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- 229910052738 indium Inorganic materials 0.000 title claims abstract description 70
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical group CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 36
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical group OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000004094 surface-active agent Substances 0.000 claims abstract description 19
- 229910052751 metal Inorganic materials 0.000 claims abstract description 18
- 239000002184 metal Substances 0.000 claims abstract description 18
- 239000000080 wetting agent Substances 0.000 claims abstract description 14
- 239000000853 adhesive Substances 0.000 claims abstract description 13
- 230000001070 adhesive effect Effects 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 12
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 9
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical group [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000005011 phenolic resin Substances 0.000 claims abstract description 6
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 6
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 5
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical group CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 5
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000008117 stearic acid Substances 0.000 claims abstract description 5
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 4
- PMBXCGGQNSVESQ-UHFFFAOYSA-N 1-Hexanethiol Chemical compound CCCCCCS PMBXCGGQNSVESQ-UHFFFAOYSA-N 0.000 claims description 42
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 27
- 239000002245 particle Substances 0.000 claims description 26
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 19
- -1 alkyl hydrosulfide Chemical compound 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- 239000012279 sodium borohydride Substances 0.000 claims description 12
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 12
- 239000002202 Polyethylene glycol Substances 0.000 claims description 11
- 229920001223 polyethylene glycol Polymers 0.000 claims description 11
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- 150000002170 ethers Chemical class 0.000 claims description 8
- 239000004530 micro-emulsion Substances 0.000 claims description 7
- 239000003960 organic solvent Substances 0.000 claims description 7
- 239000002736 nonionic surfactant Substances 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 5
- 239000004925 Acrylic resin Substances 0.000 claims description 4
- 229920000178 Acrylic resin Polymers 0.000 claims description 4
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 230000001276 controlling effect Effects 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 4
- POULHZVOKOAJMA-UHFFFAOYSA-M dodecanoate Chemical compound CCCCCCCCCCCC([O-])=O POULHZVOKOAJMA-UHFFFAOYSA-M 0.000 claims description 3
- 235000011187 glycerol Nutrition 0.000 claims description 3
- 229940070765 laurate Drugs 0.000 claims description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims 1
- 238000007639 printing Methods 0.000 abstract description 7
- 230000005693 optoelectronics Effects 0.000 abstract description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 abstract 2
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 abstract 1
- 239000005639 Lauric acid Substances 0.000 abstract 1
- 150000001412 amines Chemical class 0.000 abstract 1
- 239000002105 nanoparticle Substances 0.000 abstract 1
- 229940051841 polyoxyethylene ether Drugs 0.000 abstract 1
- 229920000056 polyoxyethylene ether Polymers 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 11
- 239000000839 emulsion Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 229920000620 organic polymer Polymers 0.000 description 7
- 238000000576 coating method Methods 0.000 description 6
- 239000010408 film Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000010409 thin film Substances 0.000 description 6
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 5
- 229920002678 cellulose Polymers 0.000 description 5
- 239000001913 cellulose Substances 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 238000005374 membrane filtration Methods 0.000 description 5
- 239000000523 sample Substances 0.000 description 5
- 238000005245 sintering Methods 0.000 description 4
- 238000007711 solidification Methods 0.000 description 4
- 230000008023 solidification Effects 0.000 description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 description 3
- 150000002472 indium compounds Chemical class 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000002082 metal nanoparticle Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000001771 vacuum deposition Methods 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 235000019082 Osmanthus Nutrition 0.000 description 1
- 241000333181 Osmanthus Species 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 238000010009 beating Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000007641 inkjet printing Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 239000013528 metallic particle Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 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
- C09D11/30—Inkjet printing inks
- C09D11/38—Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes
-
- 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
- C09D11/52—Electrically conductive inks
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
- Conductive Materials (AREA)
Abstract
The invention discloses nano indium ink for flexible electronic devices as well as a preparation method and application of the nano indium ink. The nano indium ink comprises the following components in percent by weight: 40-60% of indium nanoparticles and 40-60% of ink carrier, wherein the ink carrier comprises the following components in percent by weight: 40-70% of a solvent, 10-25% of a surfactant, 1-20% of a wetting agent and 1-15% of an adhesive; the solvent is hexane or ethanol; the surfactant is stearic acid, triethanolamine, lauric acid or polyoxyethylene ether; the wetting agent is diethylene glycol, diethylene glycol butyl ether or glycerol; the adhesive is phenolic resin or fatty amine. The nano indium ink can be widely applied to printers with nozzles with a variety of different sizes, can print fine electronic circuits, and can be used for printing metal electrodes of large-area optoelectronic devices.
Description
Technical field：
The invention belongs to ink-jet printing ink technical field, and in particular to the nanometer indium ink and its preparation for nesa coating
Methods and applications.
Background technology
Microelectronic component based on new organic polymer material（Organic Electronics）Develop generation rapidly
The turn up of one brand-new industry of table.The famous IDTechex companies prediction of Britain, the global sales of new organic electronic device
About 47,000,000,000 dollars/year were up in 2018, by 2028, this numeral will advance by leaps and bounds to about 380,000,000,000 dollars/year.
In the output value distribution of whole industry, there is about 50%-60% to be that, from all kinds of supplementary materials, wherein metal electrode material is constituted about
8%-10% or so.
With the development of computer industry, the communication of man-machine interface into computer technology a focus, touch-screen with
Outstanding man-machine communication way, becomes the most fast technology of Developing.Touch Screen can be made one with machinery compartment with more friendly
Directly mode is linked up, and makes the use more hommization of personal electric product.Wherein, resistance-type and capacitive touch screen need to make
Use nesa coating.The material of nesa coating needs to be provided simultaneously with flexibility, the transparency and electric conductivity.Nesa coating is needed
Touch-screen could be formed after the operations such as etching, printed wire, pressing.
In the process of comprehensive commercialization industrialization, organic electronic also has the technological difficulties that many needs to be broken through, wherein
Including synthesizing and prepare the metal electrode material on organic polymer thin film surface.Semiconductive organic polymer film is required and it
Work function（Work Function）The metal electrode for matching.This kind of metal electrode is mostly with metallic compounds such as Jin Heyin
It is main, it is prepared into by way of vacuum coating on organic polymer thin film surface.But this metal coating technique is generally required
200-300oThe high annealing of C.This temperature range is unaffordable for many organic polymer thin films.It is such
High-temperature technology can cause to be produced on the interface of organic polymer thin film and metal electrode needs many defects, so as to substantially reduce device
Photoelectric transformation efficiency and service life.And, the technology of vacuum coating cannot manufacture big face with printing technology matching
The thin film photocell and flexible electronic device of product and overlarge area.Therefore one class of exploitation is dedicated for all kinds of organic flexible photoelectrons
The thin-film metal electrodes material that device, suitable large area typography is manufactured at normal temperatures and pressures has huge technological value
And economic benefit.
Nanometer indium compound can be dissolved in organic solution, therefore can use normal temperature and pressure technique, by nanometer indium compound
Print and be prepared into transparent conducting film.Based on the good compatibility between nano-metal particle/organic polymer interface, nanometer
Indium compound material can significantly reduce the surface contacted resistance of device, and the material reduced between metal electrode and organic film lacks
Fall into, so as to improve device reliability and photoelectric transformation efficiency.
The content of the invention
The technical problem of solution：Occur in order to solve nesa coating preparation process solidification sintering temperature is too high and gold
The problem of metal nano-particle and matrix compatibility, the invention provides a kind of nanometer indium ink for flexible electronic device and its
Preparation method and application.
Technical scheme：Nanometer indium ink, count by weight percentage, including following component：Nanometer indium particle：40～60%；
Ink carrier：40～60%；The ink carrier includes count by weight percentage following component：Solvent 40～70%, surface is lived
Property agent 10～25%, the % of wetting agent 1～20 and adhesive 1～15%；The solvent is hexane or ethanol；Surfactant is
Stearic acid, triethanolamine, laurate or APEO；Wetting agent is diethylene glycol (DEG), butyl, glycerine；Adhesive
For phenolic resin or acrylic resin.
A diameter of 10 nm ~ 30 nm of above-mentioned nanometer indium particle, and nanometer indium particle is by organic molecule Nang Bao, it is described
Organic molecule is alkyl hydrosulfide.
The preparation method of nanometer indium ink, the preparation process of nanometer indium is：Under magnetic stirring, inidum chloride is dissolved in into hydrochloric acid
In, wherein HCl is 170 ~ 200 with the mass ratio of inidum chloride:1, the mass ratio for adding n-hexane, inidum chloride and n-hexane is 1：
（2.5~ 4）, then will add in above-mentioned solution, wherein four as four polyethyleneglycol bay ethers of nonionic surfactant
The mass ratio of polyethyleneglycol bay ether and inidum chloride is 0.15:1~ 0.25:1, stirring is defined lives containing hydrone, surface
Property agent, organic solvent and In3+Micro emulsion micella micel；Then, hexyl mercaptan stirring, hexyl mercaptan and In are added3+ Molar ratio
For 0.125 ~ 5:1, indium metal is restored the nanometer indium of the hexyl mercaptan Nang Bao for obtaining using excessive sodium borohydride
The mol ratio of grain, sodium borohydride and inidum chloride is 1:1 ~ 2:1.
The size of nanometer indium is by alkyl hydrosulfide and In3+ Molar ratio regulating and controlling, as alkyl hydrosulfide and In3+ Mole
Ratio is 0.125 ~ 5:When 1, the size of nanometer indium is received between 10 ~ 30nm and as alkyl hydrosulfide consumption increases
The size of rice indium particle is gradually reduced.
Above-mentioned nanometer indium ink is applied in flexible electronic device is prepared.
Beneficial effect：The present invention solves solidification sintering temperature is too high and metal nanoparticle and matrix compatibility are asked
Topic.Nanometer indium particle is the nanometer indium particle of mercaptan Nang Bao, and the use of mercaptan can increase between metallic particles and base material
Compatibility, also can use as the dispersant of ink system.Additionally, by regulation and control alkyl hydrosulfide and In3+ Molar ratio changing
Become the size of nanometer indium so that the ink can be widely applied to the printer of various different size nozzles, can both print fine
Electronic circuit, can be used for again large area opto-electronic device metal electrode printing prepare in.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the present invention.（a）For transmission electron microscope（TEM）The conductive ink of the present invention of displaying is at 90 DEG C
The structure on sintering conductive indium film surface after 2 hours；（b）For transmission electron microscope（TEM）The conductive ink of the present invention of displaying is in 80 DEG C of burnings
The structure on knot conductive indium film surface after 2 hours.
Specific embodiment
Above example technology design only to illustrate the invention and feature, its object is to allow the person skilled in the art be
Will appreciate that present disclosure and implement according to this, can not be limited the scope of the invention with this.It is all smart according to the present invention
Equivalent transformation or modification that refreshing essence is done, all should be included within the scope of the present invention.
Embodiment 1：
The inidum chloride solid of 5.0 g is weighed, in being dissolved in the hydrochloric acid of the 0.06M of 12.5 mL, the n-hexane of 25.0 mL is added, is formed
Mixed solution, is stirring evenly and then adding into the four polyethyleneglycol bay ethers of 1.0 mL as nonionic surfactant.Stirring shape
Into containing hydrone, surfactant, organic solvent and In3+Micro emulsion micella micel.Add hexyl mercaptan（Hexyl mercaptan and
In3+ Molar ratio be 5:1）, add 1.25 g sodium borohydride indium metal is restored, obtain organic molecule Nang Bao's
Nanometer indium particle.
The nanometer indium particle for weighing 1.5 g organic molecule Nang Bao is dissolved in the hexane of 2.0 mL, adds the ethanol of 0.23 g tri-
Amine adds 0.4 g diethylene glycol (DEG)s as wetting agent as surfactant, adds the phenolic resin of 0.3 g as adhesive, stirring
30 min, using 0.45 μm of cellulose mixture membrane filtration emulsion printable ink is obtained.
Indium determines that its fusing point is lower than metals such as silver, gold due to self property, and the fusing point of nanometer indium is lower, nanometer indium
The solidification temperature of ink typically at 80 ~ 100 DEG C, far below the solidification temperature of conductive silver ink.The indium ink of the present invention is through beating
Print, the h of heat-agglomerating 2 in 90 DEG C of baking ovens naturally cools to room temperature and forms uniform conductive film.Connect in substrate material surface
Continuous and uniform distribution shows and the preferable compatibility of base material.By regulating and controlling alkyl hydrosulfide and In3+ Molar ratio come
Change the size of nanometer indium, as hexyl mercaptan and In3+ Molar ratio be 5:When 1, the indium particle size control for obtaining is left in 10nm
It is right（A in Fig. 1）.It is 0.3 m Ω/ that Jing four probe methods measure sheet resistance.
Embodiment 2：
The inidum chloride solid of about 4.0 g is weighed, in being dissolved in the hydrochloric acid of the 0.06M of 10.0 mL, magnetic agitation is subsequently adding 20
The n-hexane of mL, forms mixed solution, and the four polyethyleneglycol bay ethers of 0.8 mL are added as nonionic after stirring a few minutes
Surfactant.Stirring is defined containing hydrone, surfactant, organic solvent and In3+Micro emulsion micella micel.Add
Hexyl mercaptan（Hexyl mercaptan and In3+ Molar ratio be 1:8）, add 1.0 g sodium borohydride indium metal is restored, obtain
The nanometer indium particle of organic molecule Nang Bao.
Weigh 2.0 g nanometer indium particles to be dissolved in the hexane of 3 mL, add 0.3 g stearic acid as surfactant, plus
Enter 0.4 g glycerine as wetting agent, add the acrylic resin of 0.32 g as adhesive, stir 30 min, use 0.45
μm cellulose mixture membrane filtration emulsion obtain printable ink.
Jing after printing, the heat-agglomerating 2h in 80 DEG C of baking ovens naturally cools to room temperature to this ink.Sintered products are using sweeping
Retouch electron microscopic observation to learn：After sintering, indium particle joins together on glass carrier surface；By regulating and controlling alkyl hydrosulfide and In3+ 's
Molar ratio changing the size of nanometer indium, as hexyl mercaptan and In3+ Molar ratio be 1:When 8, the indium particle size control for obtaining
System is at 30nm or so (b in Fig. 1).It is 0.4 m Ω/ that Jing four probe methods measure sheet resistance.
Embodiment 3
Under magnetic stirring, inidum chloride is dissolved in hydrochloric acid, wherein HCl is 170 with the mass ratio of inidum chloride:1, add just oneself
The mass ratio of alkane, inidum chloride and n-hexane is 1：2.5, then using as four polyethyleneglycol bays of nonionic surfactant
Ether is added in solution, wherein the mass ratio of four polyethyleneglycol bay ethers and inidum chloride is 0.15:1, stirring is defined containing water
Molecule, surfactant, organic solvent and In3+Micro emulsion micella micel；Then, hexyl mercaptan stirring, hexyl mercaptan and In are added3 + Molar ratio be 0.125:1, indium metal is restored the nanometer of the mercaptan Nang Bao for obtaining using excessive sodium borohydride
The mol ratio of indium particle, sodium borohydride and inidum chloride is 1:1.
The nanometer indium particle of hexyl mercaptan Nang Bao is dissolved in solvent, is added and is stirred after surfactant, wetting agent and adhesive
Mix and uniformly obtain emulsion, using 0.45 μm of cellulose mixture membrane filtration emulsion the ink of conduction is obtained.Nanometer indium particle
（Mass percent）：40%；Ink carrier（Mass percent）：60%；Following (the mass percent of the composition of ink carrier）：Ethanol
（Solvent, 70%）, stearic acid（Surfactant, 25%）, butyl（Wetting agent, 1%）, acrylic resin（Adhesive,
4%）.Jing after printing, the heat-agglomerating 2h in 80 DEG C of baking ovens naturally cools to room temperature to this ink.Jing four probe methods measure surface
Resistance is 0.45 m Ω/.
Embodiment 4
Under magnetic stirring, inidum chloride is dissolved in hydrochloric acid, wherein HCl is 190 with the mass ratio of inidum chloride:1, add just oneself
The mass ratio of alkane, inidum chloride and n-hexane is 1:3.3, then using as the four polyethyleneglycol moons of nonionic surfactant
Osmanthus ether is added in solution, wherein the mass ratio of four polyethyleneglycol bay ethers and inidum chloride is 0.2:1, stirring define containing
Hydrone, surfactant, organic solvent and In3+Micro emulsion micella micel；Then, add hexyl mercaptan stirring, hexyl mercaptan and
In3+ Molar ratio be 2:1, indium metal is restored the nanometer indium of the mercaptan Nang Bao for obtaining using excessive sodium borohydride
The mol ratio of particle, sodium borohydride and inidum chloride is 1.5:1.
The nanometer indium particle of hexyl mercaptan Nang Bao is dissolved in solvent, is added and is stirred after surfactant, wetting agent and adhesive
Mix and uniformly obtain emulsion, using 0.45 μm of cellulose mixture membrane filtration emulsion the ink of conduction is obtained.Nanometer indium particle
（Mass percent）：50%；Ink carrier（Mass percent）：50%.Wherein, following (the quality percentage of the composition of ink carrier
Than）：Ethanol（Solvent, 60%）, triethanolamine（Surfactant, 15%）, diethylene glycol (DEG)（Wetting agent, 15%）, phenolic resin（It is gluing
Agent, 10%）.Jing after printing, the heat-agglomerating 2h in 80 DEG C of baking ovens naturally cools to room temperature to this ink.Jing four probe methods are measured
Sheet resistance is 0.47 m Ω/.
Embodiment 5
Under magnetic stirring, inidum chloride is dissolved in hydrochloric acid, wherein HCl is 200 with the mass ratio of inidum chloride:1, add just oneself
The mass ratio of alkane, inidum chloride and n-hexane is 1：4, then using as four polyethyleneglycol bay ethers of nonionic surfactant
In adding solution, wherein the mass ratio of four polyethyleneglycol bay ethers and inidum chloride is 0.25:1, stirring is defined containing moisture
Son, surfactant, organic solvent and In3+Micro emulsion micella micel；Then, hexyl mercaptan stirring, hexyl mercaptan and In are added3+
Molar ratio be 5:1, indium metal is restored the nanometer indium of the mercaptan Nang Bao for obtaining using excessive sodium borohydride
The mol ratio of grain, sodium borohydride and inidum chloride is 2:1.
The nanometer indium particle of hexyl mercaptan Nang Bao is dissolved in solvent, is added and is stirred after surfactant, wetting agent and adhesive
Mix and uniformly obtain emulsion, using 0.45 μm of cellulose mixture membrane filtration emulsion the ink of conduction is obtained.Nanometer indium particle
（Mass percent）：60%；Ink carrier（Mass percent）：40%.Wherein, following (the quality percentage of the composition of ink carrier
Than）：Hexane（Solvent, 40%）, laurate（Surfactant, 25%）, butyl work（Wetting agent, 20%）, phenolic resin
（Adhesive, 15%）.Jing after printing, the heat-agglomerating 2h in 80 DEG C of baking ovens naturally cools to room temperature to this ink.Jing four probe methods
It is 0.35 m Ω/ to measure sheet resistance.
Claims (7)
1. nanometer indium ink, it is characterised in that count by weight percentage, including following component：Nanometer indium particle：40～60%；
Ink carrier：40～60%；The ink carrier includes count by weight percentage following component：Solvent 40～70%, surface is lived
Property agent 10～25%, the % of wetting agent 1～20 and adhesive 1～15%；The solvent is hexane or ethanol；Surfactant is
Stearic acid, triethanolamine, laurate or APEO；Wetting agent is diethylene glycol (DEG), butyl, glycerine；Adhesive
For phenolic resin or acrylic resin.
2. according to claim 1 nanometer of indium ink, it is characterised in that a diameter of 10 nm of the nanometer indium particle ~
30 nm。
3. according to claim 1 nanometer of indium ink, it is characterised in that the nanometer indium particle is by organic molecule Nang Bao.
4. according to claim 3 nanometer of indium ink, it is characterised in that described organic molecule is alkyl hydrosulfide.
5. according to the preparation method of the arbitrary nanometer indium ink of claim 1 ~ 4, it is characterised in that the preparation process of nanometer indium
For：Under magnetic stirring, inidum chloride is dissolved in hydrochloric acid, wherein HCl is 170 ~ 200 with the mass ratio of inidum chloride:1, add
The mass ratio of n-hexane, inidum chloride and n-hexane is 1：（2.5~ 4）, then using as the four of nonionic surfactant poly- second
Glycol list bay ether is added in above-mentioned solution, wherein the mass ratio of four polyethyleneglycol bay ethers and inidum chloride is 0.15:1~
0.25:1, stirring is defined containing hydrone, surfactant, organic solvent and In3+Micro emulsion micella micel；Then, plus
Enter hexyl mercaptan stirring, hexyl mercaptan and In3+ Molar ratio be 0.125 ~ 5:1, using excessive sodium borohydride by indium metal
The mol ratio for restoring the nanometer indium particle of the hexyl mercaptan Nang Bao for obtaining, sodium borohydride and inidum chloride is 1:1 ~ 2:1.
6. the preparation method of according to claim 5 nanometer of indium ink, it is characterised in that the size of nanometer indium passes through alkyl
Mercaptan and In3+ Molar ratio regulating and controlling；As alkyl hydrosulfide and In3+ Molar ratio be 0.125 ~ 5:When 1, nanometer indium
Size between 10 ~ 30nm and as alkyl hydrosulfide consumption increases, the size of nanometer indium particle is gradually reduced.
7. the arbitrary nanometer indium ink of claim 1 ~ 4 is applied in flexible electronic device is prepared.
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| CN201611094498.8A CN106634215A (en) | 2016-12-01 | 2016-12-01 | Nano indium ink for flexible electronic devices as well as preparation method and application of nano indium ink |
| PCT/CN2016/109956 WO2018098853A1 (en) | 2016-12-01 | 2016-12-14 | Nano-indium ink for flexible electronic devices, preparation method therefor and application thereof |
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