CN106298077A - There is the preparation method of the flexible transparent conductive film of super-amphiphobic function - Google Patents
There is the preparation method of the flexible transparent conductive film of super-amphiphobic function Download PDFInfo
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Abstract
The present invention relates to a kind of flexible transparent conductive film preparation method with super-amphiphobic function, feature is that the step included is: is dispersed in by nanometer silver in add-on type transparent silicone rubber solution, adds fluorochemical polyether Nano microsphere, obtains mixing liquid；The mass ratio of nano-silver thread, add-on type transparent silicone rubber solution and fluorochemical polyether Nano microsphere is: 1:20 100:0.1 0.5；Then the mixing liquid in step one is printed in release paper, carries out being heated at 100 150 DEG C solidification 0.5 1 hours, then demoulding, i.e. can obtain the flexible transparent conductive film with super-amphiphobic function.The electric conductivity of its transparent conductive film prepared is the most a lot, has good pliability and chemical resistance, it is achieved that constructing of super-double-hydrophobic surface.
Description
Technical field
The present invention relates to apply the flexible transparent conductive film in the flexible display field at electronic product, particularly to
A kind of preparation method of the flexible transparent conductive film with super-amphiphobic function.
Background technology
In recent years, the development that hand-held electronic product makes rapid progress, giant-screen, fine definition liquid crystal display universal rapidly and
Demand is continuously increased, and provides huge opportunity and development space for transparent conductive film.Transparent conductive film refers to ripple
Long scope between 380 ~ 780 nm the transmitance of visible ray more than 80%, resistivity is less than l0-3 The thin film of Ω .cm, its
High Resolution and Large Size flat-panel screens, solaode, energy-saving infrared reflectance coating, transparency electromagnetic wave shield material, dye sensitization
There are quite varied application prospect and the market space in the electron-optical such as solaode, electrochromic field.
Currently, transparent conductive film is mainly based on the hard transparent conductive material of oxide semiconductor film (TCO)；Oxygen
Changing indium stannum (ITO) is most commonly used transparent conductive film in research and application, but ITO raw material resources are the most rare, also lack
Bending property, pliability are poor and thin film matter is crisp.In recent years, the transparent conductive film with flexible macromolecule as substrate not only possesses
The photoelectric characteristic that ITO is identical, and also there is a lot of distinctive advantage, such as: can bend deformation, the most broken, can roll up, can industrialization
Produce continuously, be conducive to improving efficiency, frivolous portable, facilitate transport etc..Lead at flexible and transparent macromolecule membrane surface-coated height
The conductive filler (such as CNT, Graphene and metal wire etc.) of electricity rate, gives the electric conductivity of its excellence, available flexible and transparent
Conductive film.
This thin film not only possesses good transparency, flexibility, also has excellent conductivity simultaneously, in theory from the point of view of completely
Alternative current just at wide variety of ITO type transparent conductive film.Therefore, at flexible and transparent macromolecule surface with conductive filler
The method building electrically conducting transparent network has become the main development direction of current conductive film, is also the forward position heat of new material research
Point problem.
Flexible transparent conductive film does not require nothing more than satisfactory electrical conductivity, also to have excellent visible light transmissivity.But from physics
Angle is seen, material light transmission and electric conductivity are a pair basic contradictions, available intrinsic conductivity (Direct Current, DC) with
Ratio (the S of photoconductivity (Optic Current, OP)DC/SOP) height the performance of transparent conductive film is described.SDC/SOPMore
Height, shows that the transmitance of thin film is the highest, square resistance is the lowest.It is reported, transparent conductive film prepared by CNT is best
SDC/SOPValue is 25 ~ 35, and S based on GrapheneDC/SOPValue, the most only about 2, but electrically conducting transparent based on nano-silver thread
The S of thin filmDC/SOPValue then can reach 450.Therefore, the flexible transparent conductive film prepared based on nano-silver thread most possibly becomes
For substituting the next-generation of ito thin film, also for realizing the offer such as flexible touch screen, bent light emitting diode (LED) display
The chance realized.
Prepare transparent conductive film currently, with respect to nano-silver thread and application has become study hotspot both domestic and external.Such as day
State-owned a large amount of researchers such as basis, Korea S, the U.S., Germany, Canada are engaged in research the acquisition of technology breakthrough in this field.?
Domestic, Tsing-Hua University, Peking University, South China Science & Engineering University, Jilin University, Shanghai Communications University, Suzhou nanometer institute, country's nanometer
The units such as research center, Guangzhou chemistry institute, Shenzhen Xianjin Technology Academe have also been carried out the research of related fields and have been formed
Respective advantage.Generally speaking, it is currently based on the transparent conductive film of nano-silver thread to there is also following Railway Project and need emphasis
Research and solution, such as: the affinity between (a) nano-silver thread and polyethylene terephthalate (PET) thin film is poor, causes transparent
The wearability of conductive film is bad；Existence contact resistance between (b) nanometer silver and cause conductivity the most relatively low；(c) nanometer silver
Poor dispersion, cause transparency not high enough；D () conductive coating is water funk, mist is short-circuit, or Yi Beishui, oil substances pollute,
The most not chemical attack such as acid and alkali-resistance.Up to the present, also do not have in document report to propose comprehensive result of the above problems.
Therefore, once there is method can solve the problems referred to above and can not only promote the exploitation of Related product, and the theory for association area is ground
Study carefully and there is the biggest novelty.
Nature there are many plant leafs and animal feather have super-hydrophobic phenomenon, as Folium Nelumbinis has mud and the spy that do not contaminates
Property (self-cleaning function).If giving a certain material surface " lotus leaf effect ", then this material is derived from cleaning function.Thin relative to super
From the point of view of water surface, the most hydrophobic oleophobic again of super-double-hydrophobic surface, possess anti-fingerprint, waterproof and oilproof, anti-fog freeze proof, acid and alkali-resistance is corrosion-resistant
Function, therefore has more excellent automatically cleaning effect and broader practice prospect.According to triumphant western Irving Baxter (Cassie
Baxter) theoretical, the surface wettability of super-amphiphobic material, mainly surface roughness and surface by material can determine, roughness
The biggest, surface can be the lowest, can realize more preferable ultra-amphosphobic (self-cleaning property).Relatively from the point of view of super hydrophobic surface, super-double-hydrophobic surface
Construction technology increasingly complex and difficult, except large roughness and as far as possible in addition to low-surface-energy need to be tried one's best, also require to be formed coarse
The nanoparticle of degree has certain concaveconvex structure pattern (Re-entrant Structure), it addition, also require low-surface energy substance
In should contain long chain fluorine-containing unit (CnF2n+1(n >=8)) or fluorinated liquid crystal construction unit.Therefore, super-amphiphobic self-cleaning surface is constructed
Being more difficult to, the report of this respect is the most less.It addition, the long chain fluorine-containing material that current application is in super-amphiphobic field, the most right
The material that environment and human body are harmful to.
Super-hydrophobic or the preparation method of super-amphiphobic coating of tradition, can make the pattern of material surface and color are coated with by super-amphiphobic
Layer covers and becomes opaque.In recent years, transparent super-amphiphobic material, the apparent colour that substrate surface will not be changed because of it and shape
Looks, and studied getting more and more.The method constructing transparent hydrophobic or super-double-hydrophobic surface mainly has: plasma etching method, soft
Photoetching method, sol-gal process, phase separation method, nanoparticle and polymer self assembles method etc..Wherein, nanoparticle is poly-with fluorine-containing
Compound self-assembly method is that range of application is the widest and the method for Maximum Value, inorganic mainly by certain size and distribution
Nanoparticle constructs roughness (its particle diameter should be less than visible wavelength, has good dispersion simultaneously), the upper fluoropolymer of grafting
Low-surface-energy drops in thing, realizes transparent super-double-hydrophobic surface with this.Generally speaking, current transparent super-double-hydrophobic surface there is also the most several
Individual problem needs primary study and solution: the roughness on (a) surface and transparency are difficult to take into account simultaneously；B () constructs receiving of roughness
Rice corpuscles difficulty is disperseed, is easily reunited；C the bonding force between () super-amphiphobic coating and base material is weak, mill property is the best；D () preparation technology is multiple
Large-scale production miscellaneous, very difficult.
No matter transparent conductive film uses hand-held electronic display (such as mobile phone, panel computer, electronic reader or notes
This computer) or during the field such as industrial large-sized electronic displays, its surface is the most inevitably polluted by dust or oils and fats, and mostly
It is difficult in the case of number clean up, thus affects service life and the performance of transparent conductive film.If therefore at its surface construction
Layer of transparent super-amphiphobic coating, then can realize the super-amphiphobic automatically cleaning effect of transparent conductive film so that it has the anti-of excellence
Fingerprint, acid rain resistant, resistant to dust, the performance such as wear-resisting.According to statistics, the world market of transparent conductive film is worth in 2015 pre-
Meter reaches 10,000,000,000 dollars, if giving this transparent conductive film self-cleaning performance, then can improve its serviceability further and add
Value, its output value is expected to reach 200 ~ 30,000,000,000 dollars；Therefore, how to give transparent conductive film self-cleaning property, be national warp
Ji and social development need the Key Scientific And Technical Problems urgently solved, there is highly important application prospect and innovative significance.
The present inventor and partner thereof propose in patent 201410093705.2, use the mixed of epoxy resin and firming agent
Compound is as primary coat, and in this, as binding agent topcoating, then bonds one layer at substrate surface and changes via fluorine-containing or silicon-containing compound
The nano-silver thread of property, constructs the conductive coating with self-cleaning function.Although the method can be prepared as having certain automatically cleaning effect
The electrically-conducting paint of fruit, but due in the method, need first with fluorine silicon resin to nano-silver thread modifying surface, it is clear that at silver
Surface carries out chemical modification and nano-silver thread can be made to form the biggest resistance building conductive network when, simultaneously as fluorine
The compatibility between silicon polymer and epoxy resin is not fine, therefore on the one hand can affect the transparency of electrically-conducting paint, thus
Cannot be prepared as transparent conductive film, epoxy resin is also hard and crisp compound simultaneously, therefore cannot realize current flexible saturating
The needs of bright conductive film.Still further aspect, due to the phase between nano-silver thread and the epoxy resin modified through fluorine silicon resin
Capacitive is bad so that this conductive coating is the most weak with the bonding force of base material.Therefore, although this invention realizes on electrically-conducting paint surface
Self-cleaning function.But it can only be confined to some specific fields in the process of application, and cannot apply the most just
Flexible electronics field in fast development.
Furthermore, the present inventor and partner thereof proposed a kind of spike structure in patent 201410109348.4 and received
Rice silver wire, the Nano/micron that this spike structure nano silver wire has spherical nanometer silver and linear nano silver assembling formation is many
Level roughness, utilizes fluorochemical modified, with epoxy resin as binding agent, obtains having superior electrical conductivity energy and super-amphiphobic
The conduction self-cleaning coating of performance, is coated on base material, not only gives the electric conductivity that substrate surface is excellent, also gives substrate table
Face self-cleaning function, can be widely applied to field of electronics.In this patent, utilize the roughness on nano-silver thread surface, enter one
Step improves self-cleaning performance.But it is not high enough still to there are the problems referred to above, such as transparency, flexible bad, conductive coating
The shortcomings such as adhesive property is the best.
Summary of the invention
The primary and foremost purpose of the present invention is to overcome the shortcoming of prior art and deficiency to provide one to have super-amphiphobic function
The preparation method of flexible transparent conductive film, this preparation method the flexible transparent conductive film produced has self-cleaning performance
The advantages such as good, transparency is high, flexible, can meet the demand of user.
In order to achieve the above object, the technical scheme is that and be achieved in that, it is that one has super-amphiphobic function
Flexible transparent conductive film preparation method, it is characterised in that comprise the steps:
Step one
Nanometer silver is dispersed in add-on type transparent silicone rubber solution, adds fluorochemical polyether Nano microsphere, obtain mixing liquid；
The mass ratio of nano-silver thread, add-on type transparent silicone rubber solution and fluorochemical polyether Nano microsphere is: 1:20-100:0.1-0.5；
Step 2
Then the mixing liquid in step one is printed in release paper, carries out being heated at 100-150 DEG C solidify 0.5-1 little
Time, then demoulding, i.e. can obtain the flexible transparent conductive film with super-amphiphobic function.
In the technical program, the preparation method of described nano-silver thread is as follows:
Silver salt, guiding agent, slaine are dissolved in solvent, are warming up to 120-160 degree Celsius, after reacting 4-8 hour, Jing Guoli
The heart, then by washing with alcohol, i.e. can get nano-silver thread；Wherein the mass ratio of silver salt, guiding agent, slaine and solvent is 1:0.5-
5:0.001-0.005:20-50；
Wherein said silver salt is silver nitrate, silver perchlorate or Argentous fluoride；
Described guiding agent is Polyethylene Glycol, polyoxyethylene, polyvinyl alcohol or polyvinyl pyrrolidone；
Described slaine be sodium chloride, sodium bromide, sodium sulfide, potassium chloride, potassium bromide, potassium hydroxide, iron chloride, ferrous chloride,
At least one in copper chloride, Cu-lyt., platinum chloride, sodium citrate, ascorbic acid and ammonium chloride；
Described solvent is ethylene glycol, propylene glycol, glycerol, diglycol, Diethylene Glycol, butanediol, neopentyl glycol
With at least one in Polyethylene Glycol.
In the technical program, the preparation method of described add-on type transparent silicone rubber solution is as follows:
Being joined by platinum catalyst in low viscosity vinyl polysiloxane, containing hydrogen silicone oil, MQ resin and inhibitor system, stirring is all
Even i.e. can get organic siliconresin；Wherein low viscosity vinyl polysiloxane, containing hydrogen silicone oil, MQ resin, inhibitor and platinum catalysis
The mass ratio of agent is respectively as follows: 1:0.05-0.1:0.005-0.01:0.0001-0.0002:0.0001-0.0005；
Wherein, described platinum catalyst is the platinum complex of divinyl tetramethyl disiloxane, and described platinum content is 2000-
7000 ppm；
The contents of ethylene of described low viscosity vinyl polysiloxane is 0.2 mol%-2 mol%, and viscosity is 200mPa.S-
The straight chain of 10000mPa.S and side chain and silicone oil；
Described containing hydrogen silicone oil is trimethyl or dimethyl or hydroxy-end capped polymethyl hydrogen siloxane, and in molecule, hydrogen content is 0.5-
1.6%, viscosity is 30-85mPa s；
Described MQ resin is the vinyl MQ silicones that mass content is 0.1-6.5% of molecule medium vinyl, and viscosity is
4000-10000mPa•s；
Described inhibitor is: 3-methyl isophthalic acid-butine-3-alcohol, methylpentynol, 3,5-dimethyl-1-hexin-3-
One in alcohol, 1-acetenyl-1-Hexalin and 3-Phenyl-1-butyn-3-ol.
In the technical program, the preparation method of described fluorochemical polyether Nano microsphere is as follows:
Step one
Silicon dioxide microsphere is joined in solvent B, adds poly (glycidyl methacrylate), be warmed up to 80-150 DEG C,
React 2-6 hour, then be centrifuged, wash to connect to surface a silicon dioxide microsphere having epoxide group；Wherein silicon dioxide microsphere
Particle diameter be 50-500nm, the molecular weight of poly (glycidyl methacrylate) is 5000-20000, silicon dioxide microsphere, solvent
The mass ratio of B and poly (glycidyl methacrylate) is: 1:10-50:1-5；
Step 2
Connecing the surface obtained in step one to prop up has the silicon dioxide microsphere of epoxide group to join in solvent B, adds end mercapto
The Fluoropolyether compound of base, is warmed up to 80-150 DEG C, reacts 2-6 hour, then is centrifuged, and washing to connect to surface to prop up has fluorine-containing gathering
The silicon dioxide microsphere of ether compound, i.e. fluorochemical polyether Nano microsphere；Wherein, surface connects has the silicon dioxide of epoxide group micro-
The mass ratio of ball, solvent B and end sulfydryl Fluoropolyether compound is: 1:10-50:1-5；
Described solvent B is: the one in Ketohexamethylene, oxolane, toluene, dimethylbenzene, butanone and dioxy six alkane.
In the technical program, the synthetic method of described end sulfydryl Fluoropolyether compound is as follows:
Fluorochemical polyether is dissolved in oxolane after adding lithium aluminium hydride reduction reaction 5-10 hour, obtains end and contain hydroxyl
Fluorochemical polyether solution；Adding thiourea and hydrochloric acid in the fluorochemical polyether solution that terminad contains hydroxyl again, the concentration of hydrochloric acid is
37%, react 2-5 hour, add the sodium hydroxide of excess, react 5-10 hour, i.e. can obtain holding the fluorochemical polyether of sulfydryl
Compound；
Wherein the mass ratio of fluorochemical polyether, oxolane, lithium aluminium hydride reduction, thiourea, hydrochloric acid and sodium hydroxide is 1:10-20:
0.001-0.1:3-6:0.1-0.5:1-3；Described fluorochemical polyether is preferably perfluor-2,5,8-trimethyl-3,6,9-trioxa
Lauroyl fluorine (CAS accession number 27639-98-1).
The present invention compared with prior art, the invention have the advantages that
1, background technology introduces from the point of view of dielectric silane sol body is assembled into CNT, this patent directly utilizes and receives
The electric conductivity of the transparent conductive film that rice silver wire prepares is the most a lot；
2, this patent uses additional organosilicon be solidified into flexible transparent film, there is good pliability and resistance to chemical attack
Property, self-cleaning performance is good, and transparency is high；
3, this patent uses surface connect and have the Nano microsphere of Fluoropolyether compound to construct the roughness on surface, thus real
Constructing of existing super-double-hydrophobic surface；
When 4, this patent constructing super-amphiphobic material, it is to avoid the most widely used toxicity bigger perfluor material (as
FOEA, PFOA, PFOS etc.), use newly synthesized perfluoropolyether material, this material is environment-protecting asepsis, this patent on the whole
The flexible transparent conductive film with super-amphiphobic function of middle preparation is environmental protection.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment one
(1) preparation of linear nano silver
Silver salt, guiding agent and slaine are dissolved in solvent, are warming up to 120 degrees Celsius, after reacting 4 hours, through centrifugal, then
By washing with alcohol, i.e. can get linear nano silver line；Wherein the mass ratio of silver salt, guiding agent, slaine and solvent is 1:0.5:
0.001:20；
Described silver salt is silver nitrate；Described solvent is ethylene glycol；Described guiding agent is Polyethylene Glycol；Described slaine is chlorination
Sodium；
(2) preparation of add-on type transparent silicone rubber solution
Platinum catalyst is joined in low viscosity vinyl silicone oil, containing hydrogen silicone oil, MQ resin and inhibitor system, stir
I.e. can get organic siliconresin；Wherein low viscosity vinyl silicone oil, containing hydrogen silicone oil, MQ resin, inhibitor and platinum catalyst
Mass ratio is respectively as follows: 1:0.05:0.005:0.0001:0.0001；
Wherein, the contents of ethylene of described low viscosity vinyl polysiloxane is 0.2 mol%, and viscosity is the straight chain silicon of 200mPa.S
Oil；
Described platinum catalyst is the platinum complex of divinyl tetramethyl disiloxane, and described platinum content is 2000ppm；
Described containing hydrogen silicone oil is trimethyl, and in molecule, hydrogen content is 0.5%, and viscosity is 30mPa s；
Described MQ resin is the vinyl MQ silicones of the mass content 0.1% of molecule medium vinyl, and viscosity is 4000mPa s；
Described inhibitor is: 3-methyl isophthalic acid-butine-3-alcohol；
(3) preparation of fluorochemical polyether Nano microsphere
Step one
Silicon dioxide microsphere is joined in solvent B, add poly (glycidyl methacrylate), be warmed up to 80 DEG C, react 2
Hour, then be centrifuged, wash to connect a silicon dioxide microsphere having epoxide group to surface；Wherein the particle diameter of silicon dioxide microsphere is
50nm, the molecular weight of poly (glycidyl methacrylate) is 5000, silicon dioxide microsphere, solvent B and polymethylacrylic acid contracting
The mass ratio of water glyceride is: 1:10:1；
Step 2
Connecing to prop up by surface obtained in step one has the silicon dioxide microsphere of epoxide group to join in solvent B, adds end mercapto
The Fluoropolyether compound of base, is warmed up to 80 DEG C, reacts 2 hours, then is centrifuged, and washing to connect to surface to prop up has fluorochemical polyether chemical combination
The silicon dioxide microsphere of thing, i.e. fluorochemical polyether Nano microsphere；Wherein, surface connects the silicon dioxide microsphere of epoxide group, molten
The mass ratio of agent B and end sulfydryl Fluoropolyether compound is: 1:10:1；Described solvent B is Ketohexamethylene；
(4) preparation of sulfydryl Fluoropolyether compound is held
Fluorochemical polyether is dissolved in oxolane after adding lithium aluminium hydride reduction reaction 5 hours, obtains end and contain hydroxyl
Fluorochemical polyether solution, then terminad contains and adds thiourea and hydrochloric acid in the fluorochemical polyether solution of hydroxyl, concentration of hydrochloric acid is 37%, instead
Answer 2 hours, add the sodium hydroxide of excess, react 5 hours, i.e. can obtain holding the Fluoropolyether compound of sulfydryl；Wherein contain
The mass ratio of perfluoroalkyl polyether, oxolane, lithium aluminium hydride reduction, thiourea, hydrochloric acid and sodium hydroxide is 1:10:0.001:3:0.1:1；Described
Fluorochemical polyether is preferably perfluor-2,5,8-trimethyl-3,6,9-trioxa lauroyl fluorine (CAS accession number 27639-98-1)；
(5) there is the preparation of the flexible transparent conductive film of super-amphiphobic function
Synthesis linear nano silver is dispersed in add-on type transparent silicone rubber solution, adds fluorochemical polyether Nano microsphere, obtain
Mixing liquid, is then printed on mixing liquid in release paper, carries out being heated at 100 DEG C solidification 0.5 hour, then demoulding, i.e.
Can obtain the flexible transparent conductive film with super-amphiphobic function, the flexible transparent conductive film with super-amphiphobic function can be applied
Flexible display field at electronic product；Wherein nano-silver thread, add-on type transparent silicone rubber solution and fluorochemical polyether nanometer are micro-
The mass ratio of ball is: 1:20:0.1.
Embodiment two
(1) preparation of linear nano silver
Silver salt, guiding agent and slaine are dissolved in solvent, are warming up to 160 degrees Celsius, after reacting 8 hours, through centrifugal, then
By washing with alcohol, i.e. can get linear nano silver line；Wherein the mass ratio of silver salt, guiding agent, slaine and solvent is 1:5:
0.005: 50；
Wherein said silver salt is silver perchlorate；Described guiding agent is polyvinyl pyrrolidone；Described slaine is potassium chloride；Institute
Stating solvent is propylene glycol；
(2) preparation of add-on type transparent silicone rubber solution
Being joined by platinum catalyst in low viscosity vinyl polysiloxane, containing hydrogen silicone oil, MQ resin and inhibitor system, stirring is all
Even i.e. can get organic siliconresin；Wherein low viscosity vinyl polysiloxane, containing hydrogen silicone oil, MQ resin, inhibitor and platinum catalysis
The mass ratio of agent is respectively as follows: 1:0.1:0.01:0.0002:0.0005；
Wherein, described platinum catalyst is the platinum complex of divinyl tetramethyl disiloxane, and described platinum content is 7000
ppm；
The contents of ethylene of described low viscosity vinyl polysiloxane is 2 mol%, viscosity be the straight chain of 10000mPa.S and side chain with
And silicone oil；
Described containing hydrogen silicone oil is dimethyl, and in molecule, hydrogen content is 1.6%, and viscosity is 85mPa s；
Described MQ resin is the vinyl MQ silicones of the mass content 6.5% of molecule medium vinyl, and viscosity is 10000mPa
s；
Described inhibitor is in 3-Phenyl-1-butyn-3-ol；
(3) preparation of fluorochemical polyether Nano microsphere
Step one
Silicon dioxide microsphere is joined in solvent B, add poly (glycidyl methacrylate), be warmed up to 150 DEG C, reaction
6 hours, then be centrifuged, wash to connect a silicon dioxide microsphere having epoxide group to surface；The wherein particle diameter of silicon dioxide microsphere
For 500nm, the molecular weight of poly (glycidyl methacrylate) is 20000, silicon dioxide microsphere, solvent B and polymethyl
The mass ratio of acid glycidyl ester is: 1:50:5；
Step 2
Surface step one obtained connects to prop up has the silicon dioxide microsphere of epoxide group to join in solvent B, adds end sulfydryl
Fluoropolyether compound, be warmed up to 150 DEG C, react 6 hours, then be centrifuged, washing to connect to surface has fluorochemical polyether chemical combination
The silicon dioxide microsphere of thing, i.e. fluorochemical polyether Nano microsphere；Wherein, surface connects the silicon dioxide microsphere of epoxide group, molten
The mass ratio of the Fluoropolyether compound of agent B and end sulfydryl is: 1:50:5；Described solvent B is oxolane；
(4) preparation of sulfydryl Fluoropolyether compound is held
Fluorochemical polyether is dissolved in oxolane after adding lithium aluminium hydride reduction reaction 10 hours, obtains end and contain hydroxyl
Fluorochemical polyether solution, then terminad contains and adds thiourea and hydrochloric acid in the fluorochemical polyether solution of hydroxyl, concentration of hydrochloric acid is 37%, instead
Answer 5 hours, add the sodium hydroxide of excess, react 10 hours, i.e. can obtain holding the Fluoropolyether compound of sulfydryl；Wherein contain
The mass ratio of perfluoroalkyl polyether, oxolane, lithium aluminium hydride reduction, thiourea, hydrochloric acid and sodium hydroxide is 1:20:0.1:6:0.5:3；Institute
State fluorochemical polyether and be preferably perfluor-2,5,8-trimethyl-3,6,9-trioxa lauroyl fluorine (CAS accession number 27639-98-1)；
(5) there is the preparation of the flexible transparent conductive film of super-amphiphobic function
Synthesis linear nano silver is dispersed in add-on type transparent silicone rubber solution, adds fluorochemical polyether Nano microsphere, obtain
Mixing liquid, is then printed on mixing liquid in release paper, carries out being heated at 120 DEG C solidification 1 hour, then demoulding,
Obtaining the flexible transparent conductive film with super-amphiphobic function, the flexible transparent conductive film with super-amphiphobic function can be applicable to
The flexible display field of electronic product；Wherein linear nano silver line, add-on type transparent silicone rubber solution and fluorochemical polyether nanometer
The mass ratio of microsphere is: 1:100:0.5.
Embodiment three
(1) preparation of linear nano silver
Silver salt, guiding agent and slaine are dissolved in solvent, are warming up to 140 degrees Celsius, after reacting 6 hours, through centrifugal, then
By washing with alcohol, i.e. can get nano-silver thread；Wherein the mass ratio of silver salt, guiding agent, slaine and solvent is 1:1:0.004:
40；
Wherein said silver salt is Argentous fluoride；Described guiding agent is polyvinyl pyrrolidone；Described slaine is ammonium chloride；Described
Solvent is Polyethylene Glycol；
(2) preparation of add-on type transparent silicone rubber solution
Being joined by platinum catalyst in low viscosity vinyl polysiloxane, containing hydrogen silicone oil, MQ resin and inhibitor system, stirring is all
Even i.e. can get organic siliconresin；Wherein low viscosity vinyl polysiloxane, containing hydrogen silicone oil, MQ resin, inhibitor and platinum catalysis
The mass ratio of agent is respectively as follows: 1:0.08:0.008:0.0001:0.0001；
Wherein, the contents of ethylene of described low viscosity vinyl polysiloxane is 1mol%, and viscosity is the branched chain silicone of 8000mPa.S；
Described containing hydrogen silicone oil is hydroxy-end capped polymethyl hydrogen siloxane, and in molecule, hydrogen content is 1%, and viscosity is 75mPa s；
Described platinum catalyst is the platinum complex of divinyl tetramethyl disiloxane, and described platinum content is 6000 ppm；
Described MQ resin is the vinyl MQ silicones of the mass content 1.5% of molecule medium vinyl, and viscosity is 6000mPa s；
Described inhibitor is 3,5-dimethyl-1-hexin-3-alcohol；
(3) preparation of sulfydryl Fluoropolyether compound is held
Fluorochemical polyether is dissolved in oxolane after adding lithium aluminium hydride reduction reaction 8 hours, obtains end and contain hydroxyl
Fluorochemical polyether.Adding thiourea and hydrochloric acid in the fluorochemical polyether solution that terminad contains hydroxyl again, concentration of hydrochloric acid is 37%, and reaction 4 is little
Time, add the sodium hydroxide of excess, react 8 hours, i.e. can obtain holding the Fluoropolyether compound of sulfydryl；The most fluorine-containing poly-
The mass ratio of ether, oxolane, lithium aluminium hydride reduction, thiourea, hydrochloric acid and sodium hydroxide is 1:16:0.06:4:0.35:2；Described contains
Perfluoroalkyl polyether is preferably perfluor-2,5,8-trimethyl-3,6,9-trioxa lauroyl fluorine (CAS accession number 27639-98-1)；
(4) preparation of fluorochemical polyether Nano microsphere
Step one
Silicon dioxide microsphere is joined in solvent B, add poly (glycidyl methacrylate), be warmed up to 120 DEG C, reaction
3 hours, then be centrifuged, wash to connect a silicon dioxide microsphere having epoxide group to surface.The wherein particle diameter of silicon dioxide microsphere
For 100nm, the molecular weight of poly (glycidyl methacrylate) is 10000, silicon dioxide microsphere, solvent B and polymethyl
The mass ratio of acid glycidyl ester is: 1:20:2；
Step 2
Connecing to prop up by surface obtained in step one has the silicon dioxide microsphere of epoxide group to join in solvent B, adds end
The Fluoropolyether compound of sulfydryl, is warmed up to 120 DEG C, reacts 4 hours, then is centrifuged, and washing to connect to surface to prop up has fluorochemical polyether
The silicon dioxide microsphere of compound, i.e. fluorochemical polyether Nano microsphere；Wherein, surface connects has the silicon dioxide of epoxide group micro-
The mass ratio of ball, solvent B and end sulfydryl Fluoropolyether compound is: 1:40:3；Described solvent B is toluene；
(5) there is the preparation of the flexible transparent conductive film of super-amphiphobic function
Synthesis linear nano silver is dispersed in add-on type transparent silicone rubber solution, adds fluorochemical polyether Nano microsphere, obtain
Mixing liquid, is then printed on mixing liquid in release paper, carries out being heated at 150 DEG C solidification 0.6 hour, then demoulding, i.e.
Can obtain the flexible transparent conductive film with super-amphiphobic function, the flexible transparent conductive film with super-amphiphobic function can be applied
Flexible display field at electronic product；Wherein nano-silver thread, add-on type transparent silicone rubber solution and fluorochemical polyether nanometer are micro-
The mass ratio of ball is: 1:80:0.3.
Embodiment four
(1) preparation of linear nano silver
Silver salt, guiding agent and slaine are dissolved in solvent, are warming up to 120 degrees Celsius, after reacting 5 hours, through centrifugal, then
By washing with alcohol, i.e. can get linear nano silver line；Wherein the mass ratio of silver salt, guiding agent, slaine and solvent is 1:2:
0.003:30；
Wherein said silver salt is silver nitrate；Described guiding agent is polyvinyl pyrrolidone；Described slaine is sodium sulfide；Described
Solvent is neopentyl glycol；
(2) preparation of add-on type transparent silicone rubber solution
Being joined by platinum catalyst in low viscosity vinyl polysiloxane, containing hydrogen silicone oil, MQ resin and inhibitor system, stirring is all
Even i.e. can get organic siliconresin；Wherein low viscosity vinyl polysiloxane, containing hydrogen silicone oil, MQ resin, inhibitor and platinum catalysis
The mass ratio of agent is respectively as follows: 1:0.1:0.01:0.0002:0.0002；
Wherein, the contents of ethylene of described low viscosity vinyl polysiloxane is 1.2 mol%, and viscosity is the branched silicon of 5000mPa.S
Oil；
Described containing hydrogen silicone oil is trimethyl or dimethyl or hydroxy-end capped polymethyl hydrogen siloxane, and in molecule, hydrogen content is
1.2%, viscosity is 45mPa s；
Described MQ resin is the vinyl MQ silicones of the mass content 3.5% of molecule medium vinyl, and viscosity is 5000mPa s；
Described inhibitor is 3-methyl isophthalic acid-butine-3-alcohol；
Described platinum catalyst is the platinum complex of divinyl tetramethyl disiloxane, and described platinum content is 3000 ppm；
(3) preparation of fluorochemical polyether Nano microsphere
Step one
Silicon dioxide microsphere is joined in solvent B, add poly (glycidyl methacrylate), be warmed up to 110 DEG C, reaction
3 hours, then be centrifuged, wash to connect a silicon dioxide microsphere having epoxide group to surface；The wherein particle diameter of silicon dioxide microsphere
For 100nm, the molecular weight of poly (glycidyl methacrylate) is 10000, silicon dioxide microsphere, solvent B and polymethyl
The mass ratio of acid glycidyl ester is: 1:40:3；
Step 2
Connecing to prop up by surface obtained in step one has the silicon dioxide microsphere of epoxide group to join in solvent B, adds end
The Fluoropolyether compound of sulfydryl, is warmed up to 100 DEG C, reacts 3 hours, then is centrifuged, and washing to connect to surface to prop up has fluorochemical polyether
The silicon dioxide microsphere of compound, i.e. fluorochemical polyether Nano microsphere；Wherein, surface connects has the silicon dioxide of epoxide group micro-
The mass ratio of ball, solvent B and end sulfydryl Fluoropolyether compound is: 1:30:2；Described solvent B is dioxy six alkane；
(4) preparation of sulfydryl Fluoropolyether compound is held
Fluorochemical polyether is dissolved in oxolane after adding lithium aluminium hydride reduction reaction 6 hours, obtains end and contain hydroxyl
Fluorochemical polyether solution, then terminad contains and adds thiourea and hydrochloric acid in the fluorochemical polyether solution of hydroxyl, concentration of hydrochloric acid is 37%, instead
Answer 4 hours, add the sodium hydroxide of excess, react 7 hours, i.e. can obtain holding the Fluoropolyether compound of sulfydryl；Wherein contain
The mass ratio of perfluoroalkyl polyether, oxolane, lithium aluminium hydride reduction, thiourea, hydrochloric acid and sodium hydroxide is 1:15:0.009:4:0.3:2；Described
Fluorochemical polyether be preferably perfluor-2,5,8-trimethyl-3,6,9-trioxa lauroyl fluorine (CAS accession number 27639-98-1)；
(5) there is the preparation of the flexible transparent conductive film of super-amphiphobic function
Synthesis linear nano silver is dispersed in add-on type transparent silicone rubber solution, adds fluorochemical polyether Nano microsphere, obtain
Mixing liquid, is then printed on mixing liquid in release paper, carries out being heated at 110 DEG C solidification 0.8 hour, then demoulding, i.e.
Can obtain the flexible transparent conductive film with super-amphiphobic function, the flexible transparent conductive film with super-amphiphobic function can be applied
Flexible display field at electronic product；Wherein nano-silver thread, add-on type transparent silicone rubber solution and fluorochemical polyether nanometer are micro-
The mass ratio of ball is: 1:80:0.4.
Embodiment five
(1) preparation of linear nano silver
Silver salt, guiding agent and slaine are dissolved in solvent, are warming up to 140 degrees Celsius, after reacting 5 hours, through centrifugal, then
By washing with alcohol, i.e. can get nano-silver thread；Wherein the mass ratio of silver salt, guiding agent, slaine and solvent is 1:3:0.002:
25；
Wherein said silver salt is silver nitrate；Described guiding agent is polyvinyl pyrrolidone；Described slaine is sodium chloride；Described
Solvent is butanediol；
(2) preparation of add-on type transparent silicone rubber solution
Being joined by platinum catalyst in low viscosity vinyl polysiloxane, containing hydrogen silicone oil, MQ resin and inhibitor system, stirring is all
Even i.e. can get organic siliconresin；Wherein low viscosity vinyl polysiloxane, containing hydrogen silicone oil, MQ resin, inhibitor and platinum catalysis
The mass ratio of agent is respectively as follows: 1:0.07:0.009:0.0001:0.0003；
Wherein, the contents of ethylene of described low viscosity vinyl polysiloxane is 1.5 mol%, and viscosity is the straight chain silicon of 500mPa.S
Oil；
Described containing hydrogen silicone oil is trimethyl or dimethyl or hydroxy-end capped polymethyl hydrogen siloxane, and in molecule, hydrogen content is 1%,
Viscosity is 45mPa s；
Described MQ resin is the vinyl MQ silicones of the mass content 1.5% of molecule medium vinyl, and viscosity is 5000mPa s.
Described inhibitor is 3,5-dimethyl-1-hexin-3-alcohol；
Described platinum catalyst is the platinum complex of divinyl tetramethyl disiloxane, and described platinum content is 6000 ppm；
(3) preparation of fluorochemical polyether Nano microsphere
Step one
Silicon dioxide microsphere is joined in solvent B, add poly (glycidyl methacrylate), be warmed up to 100 DEG C, reaction
3 hours, then be centrifuged, wash to connect a silicon dioxide microsphere having epoxide group to surface；The wherein particle diameter of silicon dioxide microsphere
For 100nm, the molecular weight of poly (glycidyl methacrylate) is 10000, silicon dioxide microsphere, solvent B and polymethyl
The mass ratio of acid glycidyl ester is: 1:20:2；
Step 2
Connecing to prop up by surface obtained in step one has the silicon dioxide microsphere of epoxide group to join in solvent B, adds end
The Fluoropolyether compound of sulfydryl, is warmed up to 90 DEG C, reacts 3 hours, then is centrifuged, and washing to connect to surface to prop up has fluorochemical polyether
The silicon dioxide microsphere of compound, i.e. fluorochemical polyether Nano microsphere；Wherein, surface connect have a silicon dioxide microsphere for epoxide group,
The mass ratio of solvent B and end sulfydryl Fluoropolyether compound is: 1:20:2；Described solvent B is dimethylbenzene；
(4) preparation of sulfydryl Fluoropolyether compound is held
Fluorochemical polyether is dissolved in oxolane after adding lithium aluminium hydride reduction reaction 6 hours, obtains end and contain hydroxyl
Fluorochemical polyether, then terminad contains and adds thiourea and hydrochloric acid in the fluorochemical polyether solution of hydroxyl, concentration of hydrochloric acid is 37%, and reaction 3 is little
Time, add the sodium hydroxide of excess, react 6 hours, i.e. can obtain holding the Fluoropolyether compound of sulfydryl；The most fluorine-containing poly-
The mass ratio of ether, oxolane, lithium aluminium hydride reduction, thiourea, hydrochloric acid and sodium hydroxide is 1:20:0.001:6:0.5:1；Described
Fluorochemical polyether is preferably perfluor-2,5,8-trimethyl-3,6,9-trioxa lauroyl fluorine (CAS accession number 27639-98-1)；
(5) there is the preparation of the flexible transparent conductive film of super-amphiphobic function
Synthesis linear nano silver is dispersed in add-on type transparent silicone rubber solution, adds fluorochemical polyether Nano microsphere, obtain
Mixing liquid, is then printed on mixing liquid in release paper, carries out being heated at 150 DEG C solidification 1 hour, then demoulding,
Obtaining the flexible transparent conductive film with super-amphiphobic function, the flexible transparent conductive film with super-amphiphobic function can be applicable to
The flexible display field of electronic product；Wherein nano-silver thread, add-on type transparent silicone rubber solution and fluorochemical polyether Nano microsphere
Mass ratio be: 1:100:0.1.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by above-described embodiment
Limit, the change made under other any spirit without departing from the present invention and principle, modify, substitute, combine, simplify,
All should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (5)
1. a flexible transparent conductive film preparation method with super-amphiphobic function, it is characterised in that comprise the steps:
Step one
Nanometer silver is dispersed in add-on type transparent silicone rubber solution, adds fluorochemical polyether Nano microsphere, obtain mixing liquid；
The mass ratio of nano-silver thread, add-on type transparent silicone rubber solution and fluorochemical polyether Nano microsphere is: 1:20-100:0.1-0.5；
Step 2
Then the mixing liquid in step one is printed in release paper, carries out being heated at 100-150 DEG C solidify 0.5-1 little
Time, then demoulding, i.e. can obtain the flexible transparent conductive film with super-amphiphobic function.
The preparation method of the flexible transparent conductive film with super-amphiphobic function the most according to claim 1, its feature exists
As follows in the preparation method of described nano-silver thread:
Silver salt, guiding agent, slaine are dissolved in solvent, are warming up to 120-160 degree Celsius, after reacting 4-8 hour, Jing Guoli
The heart, then by washing with alcohol, i.e. can get nano-silver thread；Wherein the mass ratio of silver salt, guiding agent, slaine and solvent is 1:0.5-
5:0.001-0.005:20-50；
Wherein said silver salt is silver nitrate, silver perchlorate or Argentous fluoride；
Described guiding agent is Polyethylene Glycol, polyoxyethylene, polyvinyl alcohol or polyvinyl pyrrolidone；
Described slaine be sodium chloride, sodium bromide, sodium sulfide, potassium chloride, potassium bromide, potassium hydroxide, iron chloride, ferrous chloride,
At least one in copper chloride, Cu-lyt., platinum chloride, sodium citrate, ascorbic acid and ammonium chloride；
Described solvent is ethylene glycol, propylene glycol, glycerol, diglycol, Diethylene Glycol, butanediol, neopentyl glycol
With at least one in Polyethylene Glycol.
The preparation method of the flexible transparent conductive film with super-amphiphobic function the most according to claim 1, its feature exists
As follows in the preparation method of described add-on type transparent silicone rubber solution:
Being joined by platinum catalyst in low viscosity vinyl polysiloxane, containing hydrogen silicone oil, MQ resin and inhibitor system, stirring is all
Even i.e. can get organic siliconresin；Wherein low viscosity vinyl polysiloxane, containing hydrogen silicone oil, MQ resin, inhibitor and platinum catalysis
The mass ratio of agent is respectively as follows: 1:0.05-0.1:0.005-0.01:0.0001-0.0002:0.0001-0.0005；
Wherein, described platinum catalyst is the platinum complex of divinyl tetramethyl disiloxane, and described platinum content is 2000-
7000 ppm；
The contents of ethylene of described low viscosity vinyl polysiloxane is 0.2 mol%-2 mol%, and viscosity is 200mPa.S-
The straight chain of 10000mPa.S and side chain and silicone oil；
Described containing hydrogen silicone oil is trimethyl or dimethyl or hydroxy-end capped polymethyl hydrogen siloxane, and in molecule, hydrogen content is 0.5-
1.6%, viscosity is 30-85mPa s；
Described MQ resin is the vinyl MQ silicones that mass content is 0.1-6.5% of molecule medium vinyl, and viscosity is
4000-10000mPa•s；
Described inhibitor is: 3-methyl isophthalic acid-butine-3-alcohol, methylpentynol, 3,5-dimethyl-1-hexin-3-
One in alcohol, 1-acetenyl-1-Hexalin and 3-Phenyl-1-butyn-3-ol.
The preparation method of the flexible transparent conductive film with super-amphiphobic function the most according to claim 1, its feature exists
As follows in the preparation method of described fluorochemical polyether Nano microsphere:
Step one
Silicon dioxide microsphere is joined in solvent B, adds poly (glycidyl methacrylate), be warmed up to 80-150 DEG C,
React 2-6 hour, then be centrifuged, wash to connect to surface a silicon dioxide microsphere having epoxide group；Wherein silicon dioxide microsphere
Particle diameter be 50-500nm, the molecular weight of poly (glycidyl methacrylate) is 5000-20000, silicon dioxide microsphere, solvent
The mass ratio of B and poly (glycidyl methacrylate) is: 1:10-50:1-5；
Step 2
Connecing the surface obtained in step one to prop up has the silicon dioxide microsphere of epoxide group to join in solvent B, adds end mercapto
The Fluoropolyether compound of base, is warmed up to 80-150 DEG C, reacts 2-6 hour, then is centrifuged, and washing to connect to surface to prop up has fluorine-containing gathering
The silicon dioxide microsphere of ether compound, i.e. fluorochemical polyether Nano microsphere；Wherein, surface connects has the silicon dioxide of epoxide group micro-
The mass ratio of ball, solvent B and end sulfydryl Fluoropolyether compound is: 1:10-50:1-5；
Described solvent B is: the one in Ketohexamethylene, oxolane, toluene, dimethylbenzene, butanone and dioxy six alkane.
The preparation method of the flexible transparent conductive film with super-amphiphobic function the most according to claim 4, its feature exists
As follows in the synthetic method of described end sulfydryl Fluoropolyether compound:
Fluorochemical polyether is dissolved in oxolane after adding lithium aluminium hydride reduction reaction 5-10 hour, obtains end and contain hydroxyl
Fluorochemical polyether solution；Adding thiourea and hydrochloric acid in the fluorochemical polyether solution that terminad contains hydroxyl again, the concentration of hydrochloric acid is
37%, react 2-5 hour, add the sodium hydroxide of excess, react 5-10 hour, i.e. can obtain holding the fluorochemical polyether of sulfydryl
Compound；
Wherein the mass ratio of fluorochemical polyether, oxolane, lithium aluminium hydride reduction, thiourea, hydrochloric acid and sodium hydroxide is 1:10-20:
0.001-0.1:3-6:0.1-0.5:1-3；Described fluorochemical polyether is preferably perfluor-2,5,8-trimethyl-3,6,9-trioxa
Lauroyl fluorine (CAS accession number 27639-98-1).
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