CN103909257A - Nano silver wire in spike structure, conductive paint thereof, preparation and application - Google Patents

Nano silver wire in spike structure, conductive paint thereof, preparation and application Download PDF

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Publication number
CN103909257A
CN103909257A CN201410109348.4A CN201410109348A CN103909257A CN 103909257 A CN103909257 A CN 103909257A CN 201410109348 A CN201410109348 A CN 201410109348A CN 103909257 A CN103909257 A CN 103909257A
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solvent
silver
nano
nano silver
spike structure
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CN103909257B (en
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胡继文
齐键
邹海良
吴丹
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Guoke Guanghua Nanxiong New Materials Research Institute Co ltd
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Guangzhou Chemical Co Ltd of CAS
Nanxiong Material Production Base of Guangzhou Chemical Co Ltd of CAS
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Abstract

The invention belongs to the technical field of nano materials, and discloses a nano silver wire in a spike structure, a conductive paint thereof, preparation and application. The nano silver wire in the spike structure is prepared with by the method including dissolving silver salt, lead agent and metal salt into a solvent, and heating and reacting to obtain a nano silver wire; adding the obtained nano silver wire into the solvent, adding the silver salt and the lead agent, and heating and reacting to obtain the finished nano silver wire. The invention further provided a transparent conductive self-cleaning paint on the basis of the nano silver wire in the spike structure. The nano silver wire in the spike structure is provided with nano /micron multi-layer roughness level formed by combining spherical nano silver and linear nano silver, fluorine-containing compounds are adopted for modifying, epoxy resin serves as a binder, the transparent conductive self-cleaning paint with excellent conductive performances and super double thinning property is obtained and coats on a substrate, the surface of the substrate is provided with excellent conductive performance and a self-cleaning function, and the nano silver wire in the spike structure can be widely applied to the field of electronic appliances.

Description

A kind of spike structure nano silver line and electrically-conducting paint and preparation and application
Technical field
The invention belongs to technical field of nano material, particularly a kind of spike structure nano silver line and electrically-conducting paint and preparation method and application.
Background technology
Transparent conductive film (TCF) is a kind of important photoelectric material, has a wide range of applications in fields such as solar cell, flat-panel screens, light emitting diode and touch-screens.Transparent membrane mainly contains following a few class at present: oxide semiconductor film (TCO), metal film, polymeric membrane, carbon nano-tube film (CNT), graphene film and metal nanometer line film etc.Wherein, the tin indium oxide in oxide semiconductor film (ITO) be current most study, the oxidic transparent conductive film that is most widely used.But because its main component indium belongs to scarce resource and concentrates on a few countries, tin indium oxide, except expensive, is also classified as strategic resource by majority state.And, its bending property of indium tin oxide films and pliability is poor, film matter is crisp, thereby, cost lower, resourceful substitute products better in the urgent need to a kind of performance.
Compared with indium tin oxide films, the transparent conductive film taking macromolecule as backing material not only possesses the photoelectric property identical with it, and also has a lot of distinctive advantages, as: film-forming process is simple, energy alternating bending is folding, pliability is good etc.The flexible liquid crystal display of preparing by flexible substrate been has has been researched and developed and issued to the electronics manufacturer of the U.S., Korea S, Japan and other countries.Along with miniaturization, the multifunction of electronic product, the research of transparent conductive film is just towards large area, high efficiency, flexible, low cost future development.Thereby.Flexible transparent conductive film has very vast potential for future development.
While directly utilizing conducting polymer composite (as polyaniline, polypyrrole) to prepare transparent conductive film, limit its practical application because its conductance is too low.Recently, the research of carbon nano-tube film (CNT), graphene film is also burning hoter, but its preparation technology generally comparatively complicated, equipment requirement is high, high in cost of production drawbacks limit its application.No matter transparent conductive film is for industrial large-sized electronic console, or as hand-held display device (as mobile phone, panel computer, intelligent watch or e-book), its surface is all inevitably by dust or grease contamination, and in most cases clean difficulty, thereby affected to a great extent life-span and the performance of transparent conductive film.
Chinese patent CN101597049B discloses a kind of preparation method of carbon nano-tube film.First prepare carbon nano pipe array as substrate, then with this carbon nano pipe array of plasma etching, finally obtain carbon nano-tube film by this carbon nano pipe array that stretches.Although the carbon nano-tube film that this preparation method obtains has self supporting structure, good electric conductivity and larger transparency; but in the above-mentioned process of preparing carbon nano pipe array; need in the air of 700～900 DEG C, anneal and under protective gas environment, be heated to 500-700 DEG C of such operation; and Cement Composite Treated by Plasma below, preparation procedure complexity, equipment requirement are high, with high costs.
Chinese patent CN103279239A discloses a kind of preparation method of Graphene capacitive touch screen.Although the touch-screen that the method prepares is collapsible, highly sensitive, conductance is high, but its be by two-layer graphene layer and two layers of thin China ink layer altogether four layers be formed by stacking, its thickness is too large, light transmittance is not high, run counter to more and more frivolous this trend of present electronic product simultaneously, and the outermost layer of this touch-screen is graphene layer, be vulnerable to pollute and damage.
Summary of the invention
In order to overcome the shortcoming and deficiency of above-mentioned prior art, primary and foremost purpose of the present invention is to provide a kind of spike structure nano silver line.
Another object of the present invention is to provide a kind of preparation method of above-mentioned spike structure nano silver line.
Still a further object of the present invention is to provide a kind of electrically conducting transparent self-cleaning coating based on above-mentioned spike structure nano silver line.The coating layer thickness of this coating is controlled, and technique is simple, and cost is low, having ensured the substrate transparency and flexible while, has also improved the electric conductivity of substrate, and has given substrate self-cleaning function.
Still a further object of the present invention is to provide the application of above-mentioned electrically conducting transparent self-cleaning coating in electronic apparatus.
Object of the present invention realizes by following proposal:
A kind of spike structure nano silver line, is prepared by following methods:
(1) silver salt, guiding agent, slaine are dissolved in solvent, add thermal response, obtain nano-silver thread;
(2) nano-silver thread preparing is joined in solvent, then add silver salt and guiding agent, add thermal response, obtain spike structure nano silver line.
The mass ratio of step (1) silver salt used, guiding agent, slaine, solvent is: 1:(1.2～1.6): (1.3 × 10 -3～1.9 × 10 -3): (100～200).
The mass ratio of step (2) nano-silver thread used, silver salt, guiding agent, solvent is: 1:(0.03～0.15): 0.06:(250～500).
Described silver salt is silver nitrate, silver perchlorate or silver fluoride.
Described guiding agent is polyethylene glycol, polyoxyethylene, polyvinyl alcohol or PVP.
Described slaine is sodium chloride, sodium bromide, vulcanized sodium, potassium chloride, KBr, potassium hydroxide, iron chloride, frerrous chloride, copper chloride, stannous chloride, platinum chloride, natrium citricum, ascorbic acid or ammonium chloride.
Described solvent is at least one in ethylene glycol, propane diols, glycerine, diglycol, Diethylene Glycol, butanediol, neopentyl glycol and polyethylene glycol.
The thermal rection condition that adds described in step (1) is preferably 160～180 DEG C of reaction 1～2.5h.
The thermal rection condition that adds described in step (2) is preferably at 90～160 DEG C and reacts 1～3h.
Preferably, step prepares after nano-silver thread in (1), centrifugal, and carries out second step reaction after repeatedly removing unreacting reagent with deionized water washing again.
Preferably, step (2) prepares after spike structure nano silver line, centrifugation, and wash to remove unreacting reagent with acetone.
Preferably, the reaction in step (2) is carried out in autoclave.
This spike structure nano silver line has the multi-level roughness of Nano/micron of spherical Nano Silver and wire Nano Silver assembling formation, with respect to traditional nano-silver thread and nanosphere, has better roughness.
Based on an electrically conducting transparent self-cleaning coating for above-mentioned spike structure nano silver line, comprise that primary coat and face are coated with two components, wherein, primary coat is the mixture of epoxy resin and curing agent, face is painted with the solution of above-mentioned spike structure nano silver line.
In described primary coat, the mass ratio of epoxy resin and curing agent is: 1:0.34～1:0.74.
The mass concentration of the solution of described spike structure nano silver line is 0.1～10%.
Preferably, described epoxy resin is polymethylacrylic acid glycidol ether, neopentylglycol diglycidyl ether, benzyl glycidyl ether, polypropylene glycol diglycidyl ether, 1,4-butanediol diglycidyl ether, 1, one in 6-hexanediol diglycidyl ether, E44 type epoxy resin, E51 type epoxy resin, phenol aldehyde type epoxy resin, bisphenol f type epoxy resin, bisphenol A type epoxy resin, poly-adjacent toluene glycidol ether and polyphenylene ethylene oxidic ester, its molecular weight is 1000～100000.
Described curing agent is at least one in triethylamine, tetrabutyl ammonium fluoride, diethylenetriamines, diisopropyl ethyl amine, DMA, octadecyl dimethyl tertiary amine, DADPS, methyl hexahydrophthalic anhydride, oil base dimethyl tertiary amine, 12 tertiary amines, benzyltriethylammoinium chloride, triethanolamine and imidazoles.
The solvent of the solution of described spike structure nano silver line is at least one in methyl alcohol, second alcohol and water.
In order to improve better the two thin performance of coating, can use low-surface-energy material to carry out being applied to again after surface treatment to described spike structure nano silver line and in coating, prepare face and be coated with.
Described surface treatment comprises following concrete steps: spike structure nano silver line, low-surface-energy material are dissolved in solvent, stirring reaction 2～10h at 160～180 DEG C, ultrasonic 10～15min, centrifugal, acetone washing, obtains surface modification spike structure nano silver line.
The mass ratio of spike structure nano silver line used, low-surface-energy material, solvent is: 1:(0.5～10): (200～300).
Preferably, described low-surface-energy material is 3-perfluoro capryl propyl alcohol, perfluor dodecyl mercaptans, 3-perfluoro hexyl propyl alcohol, perfluoro octyl ethanol, the perfluor tert-butyl alcohol, perfluor-2,5-dimethyl-3, at least one in 6-dioxa n-nonanoic acid, 11 fluorine caproic acids, perfluoro caprylic acid, perfluorobutyric acid, perfluoro-heptanoic acid, perfluor decyl mercaptan, perfluor spicy thioalcohol, perfluor dodecyl mercaptans, perfluoro capryl aniline, perfluor nonyl amine and perfluoro octyl sulfonic acid amine.
Described solvent is at least one in ethylene glycol, propane diols, glycerine, diglycol, Diethylene Glycol, butanediol, neopentyl glycol and polyethylene glycol.
Described mixing speed is preferably 300～800rpm/min.
Described centrifugal speed is preferably 6000rpm/min.
A kind of conductive coating, obtains by above-mentioned electrically conducting transparent self-cleaning coating is coated in to substrate surface.
Specifically comprise the following steps: primary coat is coated in to substrate surface, then spraying painting above, heat drying, obtains conductive coating.
Preferably, described heat drying refers to be dried 4～15 hours at 80～150 DEG C.
Preferably, the thickness that described primary coat applies is 0.1～2 μ m.
Base material is preferably tin indium oxide (ITO) film, polyaniline film, film of poly pyrrole, glass or pottery.
Preferably, before base material coated with conductive coating, carry out pretreatment, wherein, the preprocess method of tin indium oxide (ITO) film, polyaniline film, film of poly pyrrole is: use successively ethanol, water washing, and then dry; The preprocess method of glass is: water cleans up, wipe oil; The preprocess method of pottery is: with diluted acid immersion, then use successively ethanol, water washing, final drying.
The electrically conducting transparent self-cleaning coating of preparing in the present invention both can be coated in conductive polymer film surface, also can be coated in other substrate surface.This transparent conductive coating can be used for various electronic devices, and many functions can be provided, and eliminate, and they can be widely used as conductive layer and the electrode of transmission light such as electromagnetic shielding and static.This type of application includes but not limited to that solar cell, flat-panel screens, light emitting diode, touch-screen, radio daughter board, conductive spinning product and fiber, electroluminescent device and electrophoretic display device (EPD) are such as Electronic Paper.
Mechanism of the present invention is:
First the present invention has synthesized a kind of nano-silver thread of spike structure, this nano-silver thread has the multi-level roughness of Nano/micron of spherical Nano Silver and wire Nano Silver assembling formation, with respect to traditional nano-silver thread and nanosphere, there is better roughness, thereby be more conducive to constructing of super-double-hydrophobic surface.Secondly, the present invention can combine ultra-amphosphobic constructed with fluorochemical the electric conductivity of nano silver wire excellence, prepares a kind of transparent conductive coating with self-cleaning function.The present invention is taking epoxy resin as binding agent, and the nano-silver thread at substrate surface bonding one deck via fluorochemical modification, constructs super two open coats with self-cleaning function.Wherein the nano-silver thread of spike structure is given the electric conductivity of substrate surface excellence, and high surface roughness is provided.The fluorochemical of low-surface-energy provides substrate surface self-cleaning function, and epoxy resin has ensured the bonding stability of coating and substrate.
The present invention, with respect to prior art, has following advantage and beneficial effect:
(1) the present invention has synthesized a kind of novel spike structure nano silver line, and surface is coated with Nano silver grain, can provide Nano/micron multi-level surface roughness, thereby can obtain better self-cleaning surface;
(2) in the present invention, adopt the binding agent of epoxy resin as conductive coating, therefore high, the scrubbing resistance of conductive coating stability and the corrosion resistance of preparation, its preparation method is simple, cost is low;
(3) electrically-conducting paint of the present invention is applied to after coating, and light transmission is good, does not affect the original light transmission of substrate;
(4) conductive coating of the present invention, not only gives substrate surface good electric conductivity, also gives substrate surface self-cleaning function;
(5) in the present invention, epoxy component and fluorine component can regulate flexibly according to substrate kind, and coating layer thickness also can free adjustment, therefore practical.
Brief description of the drawings
Fig. 1 is the principle schematic of conductive coating of the present invention.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1: there is the preparation of the transparent conducting coating of self-cleaning function
(1) preparation of nano-silver thread:
Be at 20 DEG C in temperature, silver salt, guiding agent, slaine are dissolved in solvent, preheating, after question response thing dissolves completely, then is warming up to 180 DEG C of isothermal reaction 1h, then washs centrifugal 3 times by deionized water, obtains nano-silver thread.
The mass ratio of silver salt used, guiding agent, slaine, solvent is: 1:1.2:1.3 × 10 -3: 100.
Silver salt is: AgNO 3.
Guiding agent is: polyethylene glycol;
Slaine is: NaCl;
Solvent is: ethylene glycol.
(2) preparation of spike structure nano silver line:
The nano-silver thread preparing is joined to the ultrasonic suspension for preparing in solvent, join in autoclave again, and silver salt and guiding agent are joined in autoclave, at 90 DEG C, react 3h, wash centrifugal 3 times with acetone, obtain spike structure nano silver line.
Wherein the mass ratio of nano-silver thread, silver salt, guiding agent, solvent is: 1:0.03:0.06:250.
Silver salt is: AgNO 3.
Guiding agent is: polyethylene glycol.
Solvent is: ethylene glycol.
(3) preparation of fluorine-containing nano-silver thread
Spike structure nano silver line, low-surface-energy material, solvent are joined in reaction bulb, and stirring reaction 10h at 160 DEG C, more ultrasonic 15min, finally wash centrifugal 3 times with acetone, obtains required fluorine-containing nano-silver thread.
Low-surface-energy material is: perfluor dodecyl mercaptans;
Wherein the mass ratio of spike structure nano silver line, low-surface-energy material, solvent is: 1:0.5:200;
Solvent is: ethylene glycol.
(4) there is the preparation of the electrically-conducting paint of self-cleaning function:
Primary coat: epoxy resin is mixed with curing agent;
Face is coated with: the fluorine-containing nano-silver thread solution that mass concentration is 0.1%;
Wherein the mass ratio between epoxy resin and curing agent is: 1:0.34;
Described epoxy resin is: E44 type epoxy resin;
Curing agent is: methyl hexahydrophthalic anhydride;
The solvent that dissolves fluorine-containing nano-silver thread is: methyl alcohol.
(5) there is the preparation of the conductive coating of self-cleaning function:
Primary coat is coated to substrate surface, and its coating layer thickness is 0.1 μ m, then face is coated with and sprays to its surface, then be placed in drying box, at 80 DEG C, is dried 4 hours, can obtain the required conductive coating with self-cleaning function.Principle is shown in Fig. 1.
Wherein base material is: tin indium oxide (ITO) film.
Embodiment 2: there is the preparation of the transparent conducting coating of self-cleaning function
(1) preparation of nano-silver thread:
Be at 20 DEG C in temperature, silver salt, guiding agent, slaine are dissolved in solvent, preheating, after question response thing dissolves completely, then is warming up to 180 DEG C of isothermal reaction 1h, then washs centrifugal 3 times by deionized water, obtains nano-silver thread.
The mass ratio of silver salt used, guiding agent, slaine, solvent is: 1:1.2:1.3 × 10 -3: 100.
Silver salt is: AgNO 3.
Guiding agent is: polyethylene glycol;
Slaine is: NaCl;
Solvent is: ethylene glycol.
(2) preparation of spike structure nano silver line:
The nano-silver thread preparing is joined to the ultrasonic suspension for preparing in solvent, join in autoclave again, and silver salt and guiding agent are joined in autoclave, at 90 DEG C, react 3h, wash centrifugal 3 times with acetone, obtain spike structure nano silver line.
Wherein the mass ratio of nano-silver thread, silver salt, guiding agent, solvent is: 1:0.03:0.06:250.
Silver salt is: AgNO 3.
Guiding agent is: polyethylene glycol.
Solvent is: ethylene glycol.
(3) preparation of fluorine-containing nano-silver thread
Spike structure nano silver line, low-surface-energy material, solvent are joined in reaction bulb, and stirring reaction 10h at 160 DEG C, more ultrasonic 15min, finally wash centrifugal 3 times with acetone, obtains required fluorine-containing nano-silver thread.
Low-surface-energy material is: perfluor dodecyl mercaptans;
Wherein the mass ratio of spike structure nano silver line, low-surface-energy material, solvent is: 1:0.5:200;
Solvent is: ethylene glycol.
(4) there is the preparation of the electrically-conducting paint of self-cleaning function:
Primary coat: epoxy resin is mixed with curing agent;
Face is coated with: the fluorine-containing nano-silver thread solution that mass concentration is 0.1%;
Wherein the mass ratio between epoxy resin and curing agent is: 1:0.34;
Described epoxy resin is: E44 type epoxy resin;
Curing agent is: methyl hexahydrophthalic anhydride;
The solvent that dissolves fluorine-containing nano-silver thread is: methyl alcohol.
(5) there is the preparation of the conductive coating of self-cleaning function:
Primary coat is coated to substrate surface, and its coating layer thickness is 0.1 μ m, then face is coated with and sprays to its surface, then be placed in drying box, at 80 DEG C, is dried 4 hours, can obtain the required conductive coating with self-cleaning function.
Wherein base material is: polyaniline film.
Embodiment 3: there is the preparation of the transparent conducting coating of self-cleaning function
(1) preparation of nano-silver thread:
Be at 20 DEG C in temperature, silver salt, guiding agent, slaine are dissolved in solvent, preheating, after question response thing dissolves completely, then is warming up to 180 DEG C of isothermal reaction 1h, then washs centrifugal 3 times by deionized water, obtains nano-silver thread.
The mass ratio of silver salt used, guiding agent, slaine, solvent is: 1:1.2:1.3 × 10 -3: 100.
Silver salt is: AgNO 3.
Guiding agent is: polyethylene glycol;
Slaine is: NaCl;
Solvent is: ethylene glycol.
(2) preparation of spike structure nano silver line:
The nano-silver thread preparing is joined to the ultrasonic suspension for preparing in solvent, join in autoclave again, and silver salt and guiding agent are joined in autoclave, at 90 DEG C, react 3h, wash centrifugal 3 times with acetone, obtain spike structure nano silver line.
Wherein the mass ratio of nano-silver thread, silver salt, guiding agent, solvent is: 1:0.03:0.06:250.
Silver salt is: AgNO 3.
Guiding agent is: polyethylene glycol.
Solvent is: ethylene glycol.
(3) preparation of fluorine-containing nano-silver thread
Spike structure nano silver line, low-surface-energy material, solvent are joined in reaction bulb, and stirring reaction 10h at 160 DEG C, more ultrasonic 15min, finally wash centrifugal 3 times with acetone, obtains required fluorine-containing nano-silver thread.
Low-surface-energy material is: perfluor dodecyl mercaptans;
Wherein the mass ratio of spike structure nano silver line, low-surface-energy material, solvent is: 1:0.5:200;
Solvent is: ethylene glycol.
(4) there is the preparation of the electrically-conducting paint of self-cleaning function:
Primary coat: epoxy resin is mixed with curing agent;
Face is coated with: the fluorine-containing nano-silver thread solution that mass concentration is 0.1%;
Wherein the mass ratio between epoxy resin and curing agent is: 1:0.34;
Described epoxy resin is: E44 type epoxy resin;
Curing agent is: methyl hexahydrophthalic anhydride;
The solvent that dissolves fluorine-containing nano-silver thread is: methyl alcohol.
(5) there is the preparation of the conductive coating of self-cleaning function:
Primary coat is coated to substrate surface, and its coating layer thickness is 0.1 μ m, then face is coated with and sprays to its surface, then be placed in drying box, at 80 DEG C, is dried 4 hours, can obtain the required conductive coating with self-cleaning function.
Wherein base material is: film of poly pyrrole.
Embodiment 4: there is the preparation of the transparent conducting coating of self-cleaning function
(1) preparation of nano-silver thread:
Be at 20 DEG C in temperature, silver salt, guiding agent, slaine are dissolved in solvent, preheating, after question response thing dissolves completely, then is warming up to 180 DEG C of isothermal reaction 1h, then washs centrifugal 3 times by deionized water, obtains nano-silver thread.
The mass ratio of silver salt used, guiding agent, slaine, solvent is: 1:1.2:1.3 × 10 -3: 100.
Silver salt is: AgNO 3.
Guiding agent is: polyethylene glycol;
Slaine is: Na 2s;
Solvent is: propane diols.
(2) preparation of spike structure nano silver line:
The nano-silver thread preparing is joined to the ultrasonic suspension for preparing in solvent, join in autoclave again, and silver salt and guiding agent are joined in autoclave, at 90 DEG C, react 3h, wash centrifugal 3 times with acetone, obtain spike structure nano silver line.
Wherein the mass ratio of nano-silver thread, silver salt, guiding agent, solvent is: 1:0.03:0.06:250.
Silver salt is: AgNO 3.
Guiding agent is: polyethylene glycol.
Solvent is: propane diols.
(3) preparation of fluorine-containing nano-silver thread
Spike structure nano silver line, low-surface-energy material, solvent are joined in reaction bulb, and stirring reaction 10h at 160 DEG C, more ultrasonic 15min, finally wash centrifugal 3 times with acetone, obtains required fluorine-containing nano-silver thread.
Low-surface-energy material is: the perfluor tert-butyl alcohol;
Wherein the mass ratio of spike structure nano silver line, low-surface-energy material, solvent is: 1:0.5:200;
Solvent is: propane diols.
(4) there is the preparation of the electrically-conducting paint of self-cleaning function:
Primary coat: epoxy resin is mixed with curing agent;
Face is coated with: the fluorine-containing nano-silver thread solution that mass concentration is 0.1%;
Wherein the mass ratio between epoxy resin and curing agent is: 1:0.34;
Described epoxy resin is: phenol aldehyde type epoxy resin;
Curing agent is: diethylenetriamines;
The solvent that dissolves fluorine-containing nano-silver thread is: methyl alcohol.
(5) there is the preparation of the conductive coating of self-cleaning function:
Primary coat is coated to substrate surface, and its coating layer thickness is 0.1 μ m, then face is coated with and sprays to its surface, then be placed in drying box, at 80 DEG C, is dried 4 hours, can obtain the required conductive coating with self-cleaning function.
Wherein base material is: glass.
Embodiment 5: there is the preparation of the transparent conducting coating of self-cleaning function
(1) preparation of nano-silver thread:
Be at 20 DEG C in temperature, silver salt, guiding agent, slaine are dissolved in solvent, preheating, after question response thing dissolves completely, then is warming up to 180 DEG C of isothermal reaction 1h, then washs centrifugal 3 times by deionized water, obtains nano-silver thread.
The mass ratio of silver salt used, guiding agent, slaine, solvent is: 1:1.2:1.3 × 10 -3: 100.
Silver salt is: AgNO 3.
Guiding agent is: polyethylene glycol;
Slaine is: Na 2s;
Solvent is: propane diols.
(2) preparation of spike structure nano silver line:
The nano-silver thread preparing is joined to the ultrasonic suspension for preparing in solvent, join in autoclave again, and silver salt and guiding agent are joined in autoclave, at 90 DEG C, react 3h, wash centrifugal 3 times with acetone, obtain spike structure nano silver line.
Wherein the mass ratio of nano-silver thread, silver salt, guiding agent, solvent is: 1:0.03:0.06:250.
Silver salt is: AgNO 3.
Guiding agent is: polyethylene glycol.
Solvent is: propane diols.
(3) preparation of fluorine-containing nano-silver thread
Spike structure nano silver line, low-surface-energy material, solvent are joined in reaction bulb, and stirring reaction 10h at 160 DEG C, more ultrasonic 15min, finally wash centrifugal 3 times with acetone, obtains required fluorine-containing nano-silver thread.
Low-surface-energy material is: the perfluor tert-butyl alcohol;
Wherein the mass ratio of spike structure nano silver line, low-surface-energy material, solvent is: 1:0.5:200;
Solvent is: propane diols.
(4) there is the preparation of the electrically-conducting paint of self-cleaning function:
Primary coat: epoxy resin is mixed with curing agent;
Face is coated with: the fluorine-containing nano-silver thread solution that mass concentration is 0.1%;
Wherein the mass ratio between epoxy resin and curing agent is: 1:0.34;
Described epoxy resin is: phenol aldehyde type epoxy resin;
Curing agent is: diethylenetriamines;
The solvent that dissolves fluorine-containing nano-silver thread is: methyl alcohol.
(5) there is the preparation of the conductive coating of self-cleaning function:
Primary coat is coated to substrate surface, and its coating layer thickness is 0.1 μ m, then face is coated with and sprays to its surface, then be placed in drying box, at 80 DEG C, is dried 4 hours, can obtain the required conductive coating with self-cleaning function.
Wherein base material is: pottery.
Embodiment 6: there is the preparation of the transparent conducting coating of self-cleaning function
(1) preparation of nano-silver thread:
Be at 70 DEG C in temperature, silver salt, guiding agent, slaine are dissolved in solvent, preheating, after question response thing dissolves completely, then is warming up to 170 DEG C of isothermal reaction 1.5h, then washs centrifugal 3 times by deionized water, obtains nano-silver thread.
The mass ratio of silver salt used, guiding agent, slaine, solvent is: 1:1.4:1.6 × 10 -3: 150.
Silver salt is: AgClO 4.
Guiding agent is: polyvinyl alcohol;
Slaine is: Na 2s;
Solvent is: propane diols.
(2) preparation of spike structure nano silver line:
The nano-silver thread preparing is joined to the ultrasonic suspension for preparing in solvent, join in autoclave again, and silver salt and guiding agent are joined in autoclave, at 130 DEG C, react 2h, wash centrifugal 3 times with acetone, obtain spike structure nano silver line.
Wherein the mass ratio of nano-silver thread, silver salt, guiding agent, solvent is: 1:0.1:0.06:400.
Silver salt is: AgClO 4.
Guiding agent is: polyvinyl alcohol.
Solvent is: propane diols.
(3) preparation of fluorine-containing nano-silver thread
Spike structure nano silver line, low-surface-energy material, solvent are joined in reaction bulb, and stirring reaction 5h at 170 DEG C, more ultrasonic 15min, finally wash centrifugal 3 times with acetone, obtains required fluorine-containing nano-silver thread.
Low-surface-energy material is: the perfluor tert-butyl alcohol;
Wherein the mass ratio of spike structure nano silver line, low-surface-energy material, solvent is: 1:5:250;
Solvent is: propane diols.
(4) there is the preparation of the electrically-conducting paint of self-cleaning function:
Primary coat: epoxy resin is mixed with curing agent;
Face is coated with: the fluorine-containing nano-silver thread solution that mass concentration is 5%;
Wherein the mass ratio between epoxy resin and curing agent is: 1:0.5;
Described epoxy resin is: phenol aldehyde type epoxy resin;
Curing agent is: diethylenetriamines;
The solvent that dissolves fluorine-containing nano-silver thread is: ethanol.
(5) there is the preparation of the conductive coating of self-cleaning function:
Primary coat is coated to substrate surface, and its coating layer thickness is 1 μ m, then face is coated with and sprays to its surface, then be placed in drying box, at 120 DEG C, is dried 8 hours, can obtain the required conductive coating with self-cleaning function.
Wherein base material is: tin indium oxide (ITO) film.
Embodiment 7: there is the preparation of the transparent conducting coating of self-cleaning function
(1) preparation of nano-silver thread:
Be at 70 DEG C in temperature, silver salt, guiding agent, slaine are dissolved in solvent, preheating, after question response thing dissolves completely, then is warming up to 170 DEG C of isothermal reaction 1.5h, then washs centrifugal 3 times by deionized water, obtains nano-silver thread.
The mass ratio of silver salt used, guiding agent, slaine, solvent is: 1:1.4:1.6 × 10 -3: 150.
Silver salt is: AgClO 4.
Guiding agent is: polyvinyl alcohol;
Slaine is: FeCl 3;
Solvent is: glycerine.
(2) preparation of spike structure nano silver line:
The nano-silver thread preparing is joined to the ultrasonic suspension for preparing in solvent, join in autoclave again, and silver salt and guiding agent are joined in autoclave, at 130 DEG C, react 2h, wash centrifugal 3 times with acetone, obtain spike structure nano silver line.
Wherein the mass ratio of nano-silver thread, silver salt, guiding agent, solvent is: 1:0.1:0.06:400.
Silver salt is: AgClO 4.
Guiding agent is: polyvinyl alcohol.
Solvent is: glycerine.
(3) preparation of fluorine-containing nano-silver thread
Spike structure nano silver line, low-surface-energy material, solvent are joined in reaction bulb, and stirring reaction 5h at 170 DEG C, more ultrasonic 15min, finally wash centrifugal 3 times with acetone, obtains required fluorine-containing nano-silver thread.
Low-surface-energy material is: 11 fluorine caproic acids;
Wherein the mass ratio of spike structure nano silver line, low-surface-energy material, solvent is: 1:5:250;
Solvent is: glycerine.
(4) there is the preparation of the electrically-conducting paint of self-cleaning function:
Primary coat: epoxy resin is mixed with curing agent;
Face is coated with: the fluorine-containing nano-silver thread solution that mass concentration is 5%;
Wherein the mass ratio between epoxy resin and curing agent is: 1:0.5;
Described epoxy resin is: bisphenol f type epoxy resin;
Curing agent is: triethylamine;
The solvent that dissolves fluorine-containing nano-silver thread is: ethanol.
(5) there is the preparation of the conductive coating of self-cleaning function:
Primary coat is coated to substrate surface, and its coating layer thickness is 1 μ m, then face is coated with and sprays to its surface, then be placed in drying box, at 120 DEG C, is dried 8 hours, can obtain the required conductive coating with self-cleaning function.
Wherein base material is: polyaniline film.
Embodiment 8: there is the preparation of the transparent conducting coating of self-cleaning function
(1) preparation of nano-silver thread:
Be at 70 DEG C in temperature, silver salt, guiding agent, slaine are dissolved in solvent, preheating, after question response thing dissolves completely, then is warming up to 170 DEG C of isothermal reaction 1.5h, then washs centrifugal 3 times by deionized water, obtains nano-silver thread.
The mass ratio of silver salt used, guiding agent, slaine, solvent is: 1:1.4:1.6 × 10 -3: 150.
Silver salt is: AgClO 4.
Guiding agent is: polyvinyl alcohol;
Slaine is: FeCl 3;
Solvent is: glycerine.
(2) preparation of spike structure nano silver line:
The nano-silver thread preparing is joined to the ultrasonic suspension for preparing in solvent, join in autoclave again, and silver salt and guiding agent are joined in autoclave, at 130 DEG C, react 2h, wash centrifugal 3 times with acetone, obtain spike structure nano silver line.
Wherein the mass ratio of nano silver wire, silver salt, guiding agent, solvent is: 1:0.1:0.06:400.
Silver salt is: AgClO 4.
Guiding agent is: polyvinyl alcohol.
Solvent is: glycerine.
(3) preparation of fluorine-containing nano-silver thread
Spike structure nano silver line, low-surface-energy material, solvent are joined in reaction bulb, and stirring reaction 5h at 170 DEG C, more ultrasonic 15min, finally wash centrifugal 3 times with acetone, obtains required fluorine-containing nano-silver thread.
Low-surface-energy material is: 11 fluorine caproic acids;
Wherein the mass ratio of spike structure nano silver line, low-surface-energy material, solvent is: 1:5:250;
Solvent is: glycerine.
(4) there is the preparation of the electrically-conducting paint of self-cleaning function:
Primary coat: epoxy resin is mixed with curing agent;
Face is coated with: the fluorine-containing nano-silver thread solution that mass concentration is 5%;
Wherein the mass ratio between epoxy resin and curing agent is: 1:0.5;
Described epoxy resin is: bisphenol f type epoxy resin;
Curing agent is: triethylamine;
The solvent that dissolves fluorine-containing nano-silver thread is: ethanol.
(5) there is the preparation of the conductive coating of self-cleaning function:
Primary coat is coated to substrate surface, and its coating layer thickness is 1 μ m, then face is coated with and sprays to its surface, then be placed in drying box, at 100 DEG C, is dried 8 hours; Can obtain the required conductive coating with self-cleaning function.
Wherein base material is: film of poly pyrrole.
Embodiment 9: there is the preparation of the transparent conducting coating of self-cleaning function
(1) preparation of nano-silver thread:
Be at 70 DEG C in temperature, silver salt, guiding agent, slaine are dissolved in solvent, preheating, after question response thing dissolves completely, then is warming up to 170 DEG C of isothermal reaction 1.5h, then washs centrifugal 3 times by deionized water, obtains nano-silver thread.
The mass ratio of silver salt used, guiding agent, slaine, solvent is: 1:1.4:1.6 × 10 -3: 150.
Silver salt is: AgClO 4.
Guiding agent is: polyvinyl alcohol;
Slaine is: FeCl 3;
Solvent is: glycerine.
(2) preparation of spike structure nano silver line:
The nano-silver thread preparing is joined to the ultrasonic suspension for preparing in solvent, join in autoclave again, and silver salt and guiding agent are joined in autoclave, at 130 DEG C, react 2h, wash centrifugal 3 times with acetone, obtain spike structure nano silver line.
Wherein the mass ratio of nano silver wire, silver salt, guiding agent, solvent is: 1:0.1:0.06:400.
Silver salt is: AgClO 4.
Guiding agent is: polyvinyl alcohol.
Solvent is: glycerine.
(3) preparation of fluorine-containing nano-silver thread
Spike structure nano silver line, low-surface-energy material, solvent are joined in reaction bulb, and stirring reaction 5h at 170 DEG C, more ultrasonic 15min, finally wash centrifugal 3 times with acetone, obtains required fluorine-containing nano-silver thread.
Low-surface-energy material is: 11 fluorine caproic acids;
Wherein the mass ratio of spike structure nano silver line, low-surface-energy material, solvent is: 1:5:250;
Solvent is: glycerine.
(4) there is the preparation of the electrically-conducting paint of self-cleaning function:
Primary coat: epoxy resin is mixed with curing agent;
Face is coated with: the fluorine-containing nano-silver thread solution that mass concentration is 5%;
Wherein the mass ratio between epoxy resin and curing agent is: 1:0.5;
Described epoxy resin is: bisphenol f type epoxy resin;
Curing agent is: triethylamine;
The solvent that dissolves fluorine-containing nano-silver thread is: ethanol.
(5) there is the preparation of the conductive coating of self-cleaning function:
Primary coat is coated to substrate surface, and its coating layer thickness is 1 μ m, then face is coated with and sprays to its surface, then be placed in drying box, at 120 DEG C, is dried 8 hours, can obtain the required conductive coating with self-cleaning function.
Wherein base material is: glass.
Embodiment 10: there is the preparation of the transparent conducting coating of self-cleaning function
(1) preparation of nano-silver thread:
Be at 70 DEG C in temperature, silver salt, guiding agent, slaine are dissolved in solvent, preheating, after question response thing dissolves completely, then is warming up to 170 DEG C of isothermal reaction 1.5h, then washs centrifugal 3 times by deionized water, obtains nano-silver thread.
The mass ratio of silver salt used, guiding agent, slaine, solvent is: 1:1.4:1.6 × 10 -3: 150.
Silver salt is: AgClO 4.
Guiding agent is: polyvinyl alcohol;
Slaine is: CuCl 2;
Solvent is: butanediol.
(2) preparation of spike structure nano silver line:
The nano-silver thread preparing is joined to the ultrasonic suspension for preparing in solvent, join in autoclave again, and silver salt and guiding agent are joined in autoclave, at 130 DEG C, react 2h, wash centrifugal 3 times with acetone, obtain spike structure nano silver line.
Wherein the mass ratio of nano silver wire, silver salt, guiding agent, solvent is: 1:0.1:0.06:400.
Silver salt is: AgClO 4.
Guiding agent is: polyvinyl alcohol.
Solvent is: butanediol.
(3) preparation of fluorine-containing nano-silver thread
Spike structure nano silver line, low-surface-energy material, solvent are joined in reaction bulb, and stirring reaction 5h at 170 DEG C, more ultrasonic 15min, finally wash centrifugal 3 times with acetone, obtains required fluorine-containing nano-silver thread.
Low-surface-energy material is: perfluoro capryl aniline;
Wherein the mass ratio of spike structure nano silver line, low-surface-energy material, solvent is: 1:5:250;
Solvent is: butanediol.
(4) there is the preparation of the electrically-conducting paint of self-cleaning function:
Primary coat: epoxy resin is mixed with curing agent;
Face is coated with: the fluorine-containing nano-silver thread solution that mass concentration is 5%;
Wherein the mass ratio between epoxy resin and curing agent is: 1:0.5;
Described epoxy resin is: bisphenol A type epoxy resin;
Curing agent is: DADPS;
The solvent that dissolves fluorine-containing nano-silver thread is: ethanol.
(5) there is the preparation of the conductive coating of self-cleaning function:
Primary coat is coated to substrate surface, and its coating layer thickness is 1 μ m, then face is coated with and sprays to its surface, then be placed in drying box, at 120 DEG C, is dried 8 hours, can obtain the required conductive coating with self-cleaning function.
Wherein base material is: pottery.
Embodiment 11: there is the preparation of the transparent conducting coating of self-cleaning function
(1) preparation of nano-silver thread:
Be at 120 DEG C in temperature, silver salt, guiding agent, slaine are dissolved in solvent, preheating, after question response thing dissolves completely, then is warming up to 160 DEG C of isothermal reaction 2.5h, then washs centrifugal 3 times by deionized water, obtains nano-silver thread.
The mass ratio of silver salt used, guiding agent, slaine, solvent is: 1:1.6:1.9 × 10 -3: 200.
Silver salt is: AgF.
Guiding agent is: PVP;
Slaine is: CuCl 2;
Solvent is: butanediol.
(2) preparation of spike structure nano silver line:
The nano-silver thread preparing is joined to the ultrasonic suspension for preparing in solvent, join in autoclave again, and silver salt and guiding agent are joined in autoclave, at 160 DEG C, react 1h, wash centrifugal 3 times with acetone, obtain spike structure nano silver line.
Wherein the mass ratio of nano silver wire, silver salt, guiding agent, solvent is: 1:0.15:0.06:500.
Silver salt is: AgF.
Guiding agent is: PVP.
Solvent is: butanediol.
(3) preparation of fluorine-containing nano-silver thread
Spike structure nano silver line, low-surface-energy material, solvent are joined in reaction bulb, and stirring reaction 2h at 180 DEG C, more ultrasonic 15min, finally wash centrifugal 3 times with acetone, obtains required fluorine-containing nano-silver thread.
Low-surface-energy material is: perfluoro capryl aniline;
Wherein the mass ratio of spike structure nano silver line, low-surface-energy material, solvent is: 1:10:300;
Solvent is: butanediol.
(4) there is the preparation of the electrically-conducting paint of self-cleaning function:
Primary coat: epoxy resin is mixed with curing agent;
Face is coated with: the fluorine-containing nano-silver thread solution that mass concentration is 10%;
Wherein the mass ratio between epoxy resin and curing agent is: 1:0.74;
Described epoxy resin is: bisphenol A type epoxy resin;
Curing agent is: DADPS;
The solvent that dissolves fluorine-containing nano-silver thread is: water.
(5) there is the preparation of the conductive coating of self-cleaning function:
Primary coat is coated to substrate surface, and its coating layer thickness is 2 μ m, then face is coated with and sprays to its surface, then be placed in drying box, at 150 DEG C, is dried 15 hours, can obtain the required conductive coating with self-cleaning function.
Wherein base material is: tin indium oxide (ITO) film.
Embodiment 12: there is the preparation of the transparent conducting coating of self-cleaning function
(1) preparation of nano-silver thread:
Be at 120 DEG C in temperature, silver salt, guiding agent, slaine are dissolved in solvent, preheating, after question response thing dissolves completely, then is warming up to 160 DEG C of isothermal reaction 2.5h, then washs centrifugal 3 times by deionized water, obtains nano-silver thread.
The mass ratio of silver salt used, guiding agent, slaine, solvent is: 1:1.6:1.9 × 10 -3: 200.
Silver salt is: AgF.
Guiding agent is: PVP;
Slaine is: CuCl 2;
Solvent is: butanediol.
(2) preparation of spike structure nano silver line:
The nano-silver thread preparing is joined to the ultrasonic suspension for preparing in solvent, join in autoclave again, and silver salt and guiding agent are joined in autoclave, at 160 DEG C, react 1h, wash centrifugal 3 times with acetone, obtain spike structure nano silver line.
Wherein the mass ratio of nano silver wire, silver salt, guiding agent, solvent is: 1:0.15:0.06:500.
Silver salt is: AgF.
Guiding agent is: PVP.
Solvent is: butanediol.
(3) preparation of fluorine-containing nano-silver thread
Spike structure nano silver line, low-surface-energy material, solvent are joined in reaction bulb, and stirring reaction 2h at 180 DEG C, more ultrasonic 15min, finally wash centrifugal 3 times with acetone, obtains required fluorine-containing nano-silver thread.
Low-surface-energy material is: perfluoro capryl aniline;
Wherein the mass ratio of spike structure nano silver line, low-surface-energy material, solvent is: 1:10:300;
Solvent is: butanediol.
(4) there is the preparation of the electrically-conducting paint of self-cleaning function:
Primary coat: epoxy resin is mixed with curing agent;
Face is coated with: the fluorine-containing nano-silver thread solution that mass concentration is 10%;
Wherein the mass ratio between epoxy resin and curing agent is: 1:0.74;
Described epoxy resin is: bisphenol A type epoxy resin;
Curing agent is: DADPS;
The solvent that dissolves fluorine-containing nano-silver thread is: water.
(5) there is the preparation of the conductive coating of self-cleaning function:
Primary coat is coated to substrate surface, and its coating layer thickness is 2 μ m, then face is coated with and sprays to its surface, then be placed in drying box, at 150 DEG C, is dried 15 hours, can obtain the required conductive coating with self-cleaning function.
Wherein base material is: polyaniline film.
Embodiment 13: there is the preparation of the transparent conducting coating of self-cleaning function
(1) preparation of nano-silver thread:
Be at 120 DEG C in temperature, silver salt, guiding agent, slaine are dissolved in solvent, preheating, after question response thing dissolves completely, then is warming up to 160 DEG C of isothermal reaction 2.5h, then washs centrifugal 3 times by deionized water, obtains nano-silver thread.
The mass ratio of silver salt used, guiding agent, slaine, solvent is: 1:1.6:1.9 × 10 -3: 200.
Silver salt is: AgF.
Guiding agent is: PVP;
Slaine is: natrium citricum;
Solvent is: neopentyl glycol.
(2) preparation of spike structure nano silver line:
The nano-silver thread preparing is joined to the ultrasonic suspension for preparing in solvent, join in autoclave again, and silver salt and guiding agent are joined in autoclave, at 160 DEG C, react 1h, wash centrifugal 3 times with acetone, obtain spike structure nano silver line.
Wherein the mass ratio of nano silver wire, silver salt, guiding agent, solvent is: 1:0.15:0.06:500.
Silver salt is: AgF.
Guiding agent is: PVP.
Solvent is: neopentyl glycol.
(3) preparation of fluorine-containing nano-silver thread
Spike structure nano silver line, low-surface-energy material, solvent are joined in reaction bulb, and stirring reaction 2h at 180 DEG C, more ultrasonic 15min, finally wash centrifugal 3 times with acetone, obtains required fluorine-containing nano-silver thread.
Low-surface-energy material is: perfluoro octyl sulfonic acid amine;
Wherein the mass ratio of spike structure nano silver line, low-surface-energy material, solvent is: 1:10:300;
Solvent is: neopentyl glycol.
(4) there is the preparation of the electrically-conducting paint of self-cleaning function:
Primary coat: epoxy resin is mixed with curing agent;
Face is coated with: the fluorine-containing nano-silver thread solution that mass concentration is 10%;
Wherein the mass ratio between epoxy resin and curing agent is: 1:0.74;
Described epoxy resin is: polyphenylene ethylene oxidic ester;
Curing agent is: 12 tertiary amines;
The solvent that dissolves fluorine-containing nano-silver thread is: water.
(5) there is the preparation of the conductive coating of self-cleaning function:
Primary coat is coated to substrate surface, and its coating layer thickness is 2 μ m, then face is coated with and sprays to its surface, then be placed in drying box, at 150 DEG C, is dried 15 hours, can obtain the required conductive coating with self-cleaning function.
Wherein base material is: film of poly pyrrole.
Embodiment 14: there is the preparation of the transparent conducting coating of self-cleaning function
(1) preparation of nano-silver thread:
Be at 120 DEG C in temperature, silver salt, guiding agent, slaine are dissolved in solvent, preheating, after question response thing dissolves completely, then is warming up to 160 DEG C of isothermal reaction 2.5h, then washs centrifugal 3 times by deionized water, obtains nano-silver thread.
The mass ratio of silver salt used, guiding agent, slaine, solvent is: 1:1.6:1.9 × 10 -3: 200.
Silver salt is: AgF.
Guiding agent is: PVP;
Slaine is: natrium citricum;
Solvent is: neopentyl glycol.
(2) preparation of spike structure nano silver line:
The nano-silver thread preparing is joined to the ultrasonic suspension for preparing in solvent, join in autoclave again, and silver salt and guiding agent are joined in autoclave, at 160 DEG C, react 1h, wash centrifugal 3 times with acetone, obtain spike structure nano silver line.
Wherein the mass ratio of nano silver wire, silver salt, guiding agent, solvent is: 1:0.15:0.06:500.
Silver salt is: AgF.
Guiding agent is: PVP.
Solvent is: neopentyl glycol.
(3) preparation of fluorine-containing nano-silver thread
Spike structure nano silver line, low-surface-energy material, solvent are joined in reaction bulb, and stirring reaction 2h at 180 DEG C, more ultrasonic 15min, finally wash centrifugal 3 times with acetone, obtains required fluorine-containing nano-silver thread.
Low-surface-energy material is: perfluoro octyl sulfonic acid amine;
Wherein the mass ratio of spike structure nano silver line, low-surface-energy material, solvent is: 1:10:300;
Solvent is: neopentyl glycol.
(4) there is the preparation of the electrically-conducting paint of self-cleaning function:
Primary coat: epoxy resin is mixed with curing agent;
Face is coated with: the fluorine-containing nano-silver thread solution that mass concentration is 10%;
Wherein the mass ratio between epoxy resin and curing agent is: 1:0.74;
Described epoxy resin is: polyphenylene ethylene oxidic ester;
Curing agent is: 12 tertiary amines;
The solvent that dissolves fluorine-containing nano-silver thread is: water.
(5) there is the preparation of the conductive coating of self-cleaning function:
Primary coat is coated to substrate surface, and its coating layer thickness is 2 μ m, then face is coated with and sprays to its surface, then be placed in drying box, at 150 DEG C, is dried 15 hours, can obtain the required conductive coating with self-cleaning function.
Wherein base material is: glass.
Embodiment 15: there is the preparation of the transparent conducting coating of self-cleaning function
(1) preparation of nano-silver thread:
Be at 120 DEG C in temperature, silver salt, guiding agent, slaine are dissolved in solvent, preheating, after question response thing dissolves completely, then is warming up to 160 DEG C of isothermal reaction 2.5h, then washs centrifugal 3 times by deionized water, obtains nano-silver thread.
The mass ratio of silver salt used, guiding agent, slaine, solvent is: 1:1.6:1.9 × 10 -3: 200.
Silver salt is: AgF.
Guiding agent is: PVP;
Slaine is: natrium citricum;
Solvent is: neopentyl glycol.
(2) preparation of spike structure nano silver line:
The nano-silver thread preparing is joined to the ultrasonic suspension for preparing in solvent, join in autoclave again, and silver salt and guiding agent are joined in autoclave, at 160 DEG C, react 1h, wash centrifugal 3 times with acetone, obtain spike structure nano silver line.
Wherein the mass ratio of nano silver wire, silver salt, guiding agent, solvent is: 1:0.15:0.06:500.
Silver salt is: AgF.
Guiding agent is: PVP.
Solvent is: neopentyl glycol.
(3) preparation of fluorine-containing nano-silver thread
Spike structure nano silver line, low-surface-energy material, solvent are joined in reaction bulb, and stirring reaction 2h at 180 DEG C, more ultrasonic 15min, finally wash centrifugal 3 times with acetone, obtains required fluorine-containing nano-silver thread.
Low-surface-energy material is: perfluoro octyl sulfonic acid amine;
Wherein the mass ratio of spike structure nano silver line, low-surface-energy material, solvent is: 1:10:300;
Solvent is: neopentyl glycol.
(4) there is the preparation of the electrically-conducting paint of self-cleaning function:
Primary coat: epoxy resin is mixed with curing agent;
Face is coated with: the fluorine-containing nano-silver thread solution that mass concentration is 10%;
Wherein the mass ratio between epoxy resin and curing agent is: 1:0.74;
Described epoxy resin is: polyphenylene ethylene oxidic ester;
Curing agent is: 12 tertiary amines;
The solvent that dissolves fluorine-containing nano-silver thread is: water.
(5) there is the preparation of the conductive coating of self-cleaning function:
Primary coat is coated to substrate surface, and its coating layer thickness is 2 μ m, then face is coated with and sprays to its surface, then be placed in drying box, at 150 DEG C, is dried 15 hours, can obtain the required conductive coating with self-cleaning function.
Wherein base material is: pottery.
Embodiment 16: there is the performance measurement of the transparent conducting coating of self-cleaning function
The conductive coating of the self-cleaning function that embodiment 1～15 is prepared carries out the tests such as resistance, light transmittance, water contact angle, oily contact angle and roll angle, the results are shown in Table 1.
Wherein, contact angle and roll angle are all to measure at 25 DEG C, and water contact angle is measured by deionized water, and drop amount is 6 μ L, and oily contact angle is measured with edible oil, and drop amount is 8 μ L, and roll angle is measured by deionized water, and drop amount is 5 μ L.
As shown in Table 1, the conductive coating that the present invention prepares has good hydrophobicity and oleophobic property, has good automatically cleaning ability; Light transmittance is high, and the transparency is good; Sheet resistance is low, has good electric conductivity.
Table 1 has the performance indications of the conductive coating of self-cleaning function
? Average resistance (Ω/) Light transmittance (%) Water contact angle (°) Oil contact angle (°) Roll angle (°)
Embodiment 1 37 85 149 138 10
Embodiment 2 40 87 150 140 8
Embodiment 3 39 84 151 138 8
Embodiment 4 42 85 147 140 9
Embodiment 5 44 — 152 139 7
Embodiment 6 31 82 155 142 4
Embodiment 7 32 78 152 141 5
Embodiment 8 27 83 150 138 7
Embodiment 9 28 80 156 141 4
Embodiment 10 31 — 153 143 5
Embodiment 11 23 75 163 150 3
Embodiment 12 17 79 158 151 4
Embodiment 13 22 81 162 153 2
Embodiment 14 20 77 160 151 3
Embodiment 15 18 — 164 149 4
Note: in upper table, average resistance is measured by four point probe tester, and light transmittance is measured by light transmittance tester, embodiment 4, embodiment 10 and embodiment 15, due to base material select be pottery, itself is completely light tight, so cannot measure the light transmittance of coating, represents by "-".
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under Spirit Essence of the present invention and principle, substitutes, combination, simplify; all should be equivalent substitute mode, within being included in protection scope of the present invention.

Claims (10)

1. a spike structure nano silver line, is characterized in that being prepared by following methods:
(1) silver salt, guiding agent, slaine are dissolved in solvent, add thermal response, obtain nano-silver thread;
(2) nano-silver thread preparing is joined in solvent, then add silver salt and guiding agent, add thermal response, obtain spike structure nano silver line.
2. spike structure nano silver line according to claim 1, is characterized in that: the mass ratio of step (1) silver salt used, guiding agent, slaine, solvent is 1:(1.2～1.6): (1.3 × 10 -3～1.9 × 10 -3): (100～200); The mass ratio of step (2) nano-silver thread used, silver salt, guiding agent, solvent is: 1:(0.03～0.15): 0.06:(250～500).
3. spike structure nano silver line according to claim 1, is characterized in that: described silver salt is silver nitrate, silver perchlorate or silver fluoride; Described guiding agent is polyethylene glycol, polyoxyethylene, polyvinyl alcohol or PVP; Described slaine is sodium chloride, sodium bromide, vulcanized sodium, potassium chloride, KBr, potassium hydroxide, iron chloride, frerrous chloride, copper chloride, stannous chloride, platinum chloride, natrium citricum, ascorbic acid or ammonium chloride; Described solvent is at least one in ethylene glycol, propane diols, glycerine, diglycol, Diethylene Glycol, butanediol, neopentyl glycol and polyethylene glycol.
4. spike structure nano silver line according to claim 1, is characterized in that: the thermal rection condition that adds described in step (1) is 160～180 DEG C of reaction 1～2.5h; The thermal rection condition that adds described in step (2) is to react 1～3h at 90～160 DEG C.
5. the electrically conducting transparent self-cleaning coating based on spike structure nano silver line described in claim 1, it is characterized in that: comprise that primary coat and face are coated with two components, wherein, primary coat is the mixture of epoxy resin and curing agent, and face is painted with the solution of spike structure nano silver line claimed in claim 1.
6. electrically conducting transparent self-cleaning coating according to claim 5, is characterized in that: in described primary coat, the mass ratio of epoxy resin and curing agent is 1:0.34～1:0.74; The mass concentration of the solution of described spike structure nano silver line is 0.1～10%.
7. electrically conducting transparent self-cleaning coating according to claim 5, it is characterized in that: described epoxy resin is polymethylacrylic acid glycidol ether, neopentylglycol diglycidyl ether, benzyl glycidyl ether, polypropylene glycol diglycidyl ether, 1, 4-butanediol diglycidyl ether, 1, 6-hexanediol diglycidyl ether, E44 type epoxy resin, E51 type epoxy resin, phenol aldehyde type epoxy resin, bisphenol f type epoxy resin, bisphenol A type epoxy resin, one in poly-adjacent toluene glycidol ether and polyphenylene ethylene oxidic ester, its molecular weight is 1000～100000, described curing agent is at least one in triethylamine, tetrabutyl ammonium fluoride, diethylenetriamines, diisopropyl ethyl amine, DMA, octadecyl dimethyl tertiary amine, DADPS, methyl hexahydrophthalic anhydride, oil base dimethyl tertiary amine, 12 tertiary amines, benzyltriethylammoinium chloride, triethanolamine and imidazoles, the solvent of the solution of described spike structure nano silver line is at least one in methyl alcohol, second alcohol and water.
8. electrically conducting transparent self-cleaning coating according to claim 5, it is characterized in that: described spike structure nano silver line is through the processing of low-surface-energy material surface, described surface treatment comprises following concrete steps: spike structure nano silver line, low-surface-energy material are dissolved in solvent, stirring reaction 2～10h at 160～180 DEG C, ultrasonic 10～15min, centrifugal, acetone washing, obtain surface modification spike structure nano silver line;
The mass ratio of spike structure nano silver line used, low-surface-energy material, solvent is 1:(0.5～10): (200～300);
Described low-surface-energy material is 3-perfluoro capryl propyl alcohol, perfluor dodecyl mercaptans, 3-perfluoro hexyl propyl alcohol, perfluoro octyl ethanol, the perfluor tert-butyl alcohol, perfluor-2,5-dimethyl-3, at least one in 6-dioxa n-nonanoic acid, 11 fluorine caproic acids, perfluoro caprylic acid, perfluorobutyric acid, perfluoro-heptanoic acid, perfluor decyl mercaptan, perfluor spicy thioalcohol, perfluor dodecyl mercaptans, perfluoro capryl aniline, perfluor nonyl amine and perfluoro octyl sulfonic acid amine.
9. a conductive coating, is characterized in that obtaining by the electrically conducting transparent self-cleaning coating described in claim 5 is coated in to substrate surface.
10. the application in electronic apparatus according to the electrically conducting transparent self-cleaning coating described in claim 5～8 any one.
CN201410109348.4A 2014-03-21 2014-03-21 A kind of spike structure nano silver line and electrically-conducting paint thereof and preparation and application Expired - Fee Related CN103909257B (en)

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EP3118265A1 (en) * 2015-07-14 2017-01-18 Henkel AG & Co. KGaA Conductive transparent coating
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US10564780B2 (en) 2015-08-21 2020-02-18 3M Innovative Properties Company Transparent conductors including metal traces and methods of making same
CN106448804A (en) * 2016-09-28 2017-02-22 顺德职业技术学院 Preparation method of flexible transparent conductive thin film having self-cleaning function
CN106448804B (en) * 2016-09-28 2017-10-31 顺德职业技术学院 The preparation method of flexible transparent conductive film with self-cleaning function
CN107159882A (en) * 2017-04-24 2017-09-15 中国科学院合肥物质科学研究院 Gold and silver core-shell nano thorn and its production and use
CN107159882B (en) * 2017-04-24 2019-06-11 中国科学院合肥物质科学研究院 Jin-silver core-shell nano thorn and its preparation method and application
CN106938341A (en) * 2017-05-19 2017-07-11 西北大学 A kind of method that utilization polyalcohol is mixed with smaller diameter nano silver wire
CN106938341B (en) * 2017-05-19 2019-09-24 西北大学 A method of smaller diameter silver nanowires is mixed with using polyalcohol
US10822517B2 (en) 2018-11-28 2020-11-03 Industrial Technology Research Institute Resin composition and cured resin composition
CN113903502A (en) * 2019-11-14 2022-01-07 宸盛光电有限公司 Conductive structure with self-assembly protective layer and self-assembly coating composition
CN113061363A (en) * 2021-04-19 2021-07-02 北京纳米能源与***研究所 Marking paint, single-electrode friction nano generator and touch detection system

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