CN107197543A - A kind of preparation method of the low dimensional nano-sized carbon electric heating film of Nano Silver surface modification - Google Patents
A kind of preparation method of the low dimensional nano-sized carbon electric heating film of Nano Silver surface modification Download PDFInfo
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- CN107197543A CN107197543A CN201710398023.6A CN201710398023A CN107197543A CN 107197543 A CN107197543 A CN 107197543A CN 201710398023 A CN201710398023 A CN 201710398023A CN 107197543 A CN107197543 A CN 107197543A
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- nano
- low dimensional
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- carbon material
- dimensional nano
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
- H05B3/34—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater flexible, e.g. heating nets or webs
Abstract
The invention discloses a kind of low dimensional nano-sized carbon electric heating film preparation method of Nano Silver surface modification, the method comprising the steps of:A) using surface replacement or/and chemical reduction method in low dimensional nano-carbon material surface modification or covering or parcel nano-Ag particles;B) the low dimensional nano-carbon material of the surface finish nano Argent grain of gained is mixed with the binding agent of low-temperature sintering silver paste;C) graphical carbon Ag films are directly prepared on flexible cryogenic substrate by silk-screen printing technique, after low-temperature sintering under 130 180 DEG C of aerobic conditions 30 90 minutes, the low dimensional nano-sized carbon electric heating film of the Nano Silver surface modification are obtained.Present invention utilizes carbon nanomaterial, contribution of the carbon to film heating function is maintained, silver-colored this kind of high heat-conductivity conducting metal material is wrapped up by the surface of carbon, under the driving of identical voltage, heating effect can be strengthened, the transmission of temperature is realized, the temperature uniformity of film is improved.Cost of the present invention is low, technique simple, be easy to industrialized production.
Description
Technical field
The present invention relates to electrical-heating film material and flexible electronics field, specifically a kind of nanometer silver surface is repaiied
The preparation method of the low dimensional nano-sized carbon electric heating film of decorations.
Background technology
Electric heating film abbreviation Electric radiant Heating Film, its operation principle is that in the presence of electric field, the carbon molecules group in heater produces
Violent friction and shock occurs between " Brownian movement ", carbon molecules, the heat energy of generation is in the form of far infrared radiation and convection current
The conversion ratio of externally transmission, its electric energy and heat energy is up to more than 98%.The effect of carbon molecules is brought rapidly up Electric radiant Heating Film surface.Electricity
Why hotting mask can play a part of to space is brought rapidly up, in that the input of its 100% electric energy is efficiently converted to
Far infrared radiation energy and 33% convection current heat energy more than 66%.Electric radiant Heating Film is divided into high temperature, low temperature electric heating film.High-temperature electric heating membrane is general
For electronic apparatus, military affairs etc., the Electric radiant Heating Film of nowadays science and technology production.Low temperature electric heating film is can generate heat after a kind of energization translucent
Polyester film, by conductive special ink, metal current-carrying bar be processed, hot pressing is made between insulation polyester film.During work
Using Electric radiant Heating Film as heater, heat is sent into space in the form of radiation, its resultant effect is better than traditional heating mode.Therefore its turn
Efficiency high is changed, except sub-fraction loss(2%), the overwhelming majority(98%)It is converted to heat energy.
Because Electric radiant Heating Film is pure resistor element circuit, electric conversion efficiency depends primarily on the resistance of film.Electricity of the prior art
Hotting mask mainly employs the carbon or carbon membrane of conductive energy, because the resistance of film is big, on the one hand causes electric conversion efficiency to damage
Lose larger;On the other hand the heating uniformity of film can be made poor.Existing new technology proposes the composite guide in carbon material in recent years
Body or semi-conducting material, strengthen the heating-up temperature and uniformity of Electric radiant Heating Film.Such as CN106131984A propose by nano silver wire with
Graphene oxide is compound to be prepared for thin film heater, and with simple carbon film ratio, the heating-up temperature and uniformity of such product are more preferably.
But, on the one hand the film is the physical surface contact by will be realized between nano-silver thread and graphene oxide for spin coating and illumination
Type is combined, and mutual gap is big, and has contact impedance, limits temperature rise ability;The material of another aspect graphene oxide in itself lacks
The electric conductivity for limiting film is fallen into, therefore heating properties are not optimal.CN 105916222A propose to use graphene and semiconductor
Material combines and is prepared for infrared ray heating film, improves energy-saving efficiency.The semi-conducting material film carried in this method, on the one hand
The technique realization using evaporation is needed, complex process and technique consume energy big;Another aspect preparation temperature height is unsuitable for preparing flexibility
The preparation of Electric radiant Heating Film.
In recent years, as flexible electronic increasingly increases compliant conductive heat conduction film requirements, the requirement to flexible electrothermal membrane
Also more and more higher.Advantage and development bottleneck based on above New Electrothermal Film, can be by preparing nanocarbon-metal composite wood
Material is applied to Electric radiant Heating Film, the effective heating property and uniformity for improving Electric radiant Heating Film.
The content of the invention
The purpose of the present invention is directed to above-mentioned technical problem, and the present invention is received using the carbon in nano-carbon material particularly low dimensional
Mitron and grapheme material surface parcel high-conductivity metal material silver, by the way that cost is low, technique is simple, be easy to industrialized production
Technique, it is proposed that it is a kind of prepare flexibility can be effectively applied to the slurry and preparation method of electrical-heating film.
To achieve the above object, the present invention is adopted the following technical scheme that:
A kind of low dimensional nano-sized carbon electric heating film preparation method of Nano Silver surface modification, feature is that this method is included in detail below
Step:
Step 1:Received using surface replacement or/and chemical reduction method in low dimensional nano-carbon material surface modification or covering or parcel
Rice Argent grain, obtains the low dimensional nano-carbon material of surface finish nano Argent grain;Wherein low dimensional nano-carbon material is carbon nanometer
Pipe/fiber, grapheme material;
Step 2:It is prepared by Nano Silver@nano carbon composite materials
Pass through the low dimensional nano-carbon material and low temperature of the surface finish nano Argent grain of ball milling or stirring or roll-in method by obtained by
The binding agent mixing of silver paste is sintered, mixed proportion accounts for 6-35% for the low dimensional nano-carbon material of surface finish nano Argent grain;
Gross mass percentage compositions of the AgNPs in low-temperature sintering silver paste binding agent is 25-50%..
Step 3:Graphical carbon Ag films are directly prepared on flexible cryogenic substrate by silk-screen printing technique, through 130-
Low-temperature sintering obtains the low dimensional nano-sized carbon electrical heating of the Nano Silver surface modification after 30-90 minutes under 180 DEG C of aerobic conditions
Film;Wherein:
It is described low dimensional nano-carbon material surface modification or covering or parcel nano-Ag particles, specifically include:
1)Nano-carbon material is cleaned, first with 20-60mM HCl deionized water solutions immersion low dimensional nano-carbon material, by super
Sound is cleaned 30 minutes, standby after 80-100 DEG C of drying;
2)The surface treatment of low dimensional nano-carbon material:
(a)The coating material for choosing certain mass is mixed with watery hydrochloric acid, as sensitizing solution, is added in sensitizing solution cleaned
Low dimensional nano-carbon material, after standing 6-10 hours under the conditions of room temperature after stirring 5-10 minutes, obtains sediment;Wherein, it is described
Sensitizer is stannous chloride(SnCl2), butter of tin (SnCl4) or stannous sulfate(SnSO4);Low dimensional nano-carbon material with it is quick
The mass ratio of agent is 6 ~ 20:3, watery hydrochloric acid concentration 5-10%;(b)Or from surfactant and low dimensional nano-carbon material
Mix in deionized water, wherein, the surfactant is cetyl trimethylammonium bromide CTAB or polyacrylic acid
Sodium PAA;The mass ratio of surfactant and low dimensional nano-carbon material is 5 ~ 8:10;
(c)Or by low dimensional nano-carbon material and dimethyl sulfoxide and ethylene glycol atom or group transfer reaction and polyelectrolyte hydroxyl
Base practices esterification with α-bromine isobutyl acylbromide or α-chlorpromazine chloride, completes the non-covalent modification of carbon nano tube surface;
3)Low dimensional nano-carbon material after surface treated is cleaned 3 times with deionized water, Nanocarbon-Y is obtained and suspends
Liquid;Wherein, Y is the modification cation in different modifying material;
4)Silver nitrate is added in Nanocarbon-Y suspension so that Y and AgNO3Mass ratio be 1-1.5, and
Nanocarbon and AgNO3Mass ratio be 0.8-1.5, add reducing agent, solution stirred into 10-30min, made by electrostatic
With or coordination, obtain AgNPs@Nanocarbon sediments;Wherein described reducing agent is glucose, chitosan, PVP, lemon
One kind in lemon acid sodium;
5)The AgNPs Nanocarbon sediments of acquisition are cleaned after 3 times with deionized water, through 80-100 DEG C of drying, table are obtained
Face is modified or covering or the low dimensional nano-carbon material for wrapping up nano-Ag particles.
Compared with prior art, the present invention has following remarkable advantage:
1st, the nano-Ag particles of high conduction performance have been wrapped up in nanometer carbon surface, the contact impedance between carbon material can be reduced,
So as to improve electric conductivity;Meanwhile, Argent grain, which can fill up the space in film between solid, can also further improve film
Monolithic conductive performance.
2nd, carbon nanomaterial surface parcel be nano-scale Argent grain, can the melting below 180 DEG C of low temperature, can be with
Be applied to flexible transparent substrate prepared including PET material etc. flexibility Electric radiant Heating Film, in the case of without high-temperature process with
Substrate also has preferable adhesive force.
3rd, present invention utilizes carbon nanomaterial, contribution of the carbon to film heating function is maintained, is wrapped by the surface of carbon
Silver-colored this kind of high heat-conductivity conducting metal material is wrapped up in, under the driving of identical voltage, heating effect can be strengthened, the transmission of temperature is realized,
Improve the temperature uniformity of film.
Brief description of the drawings
Fig. 1, Fig. 2 are the CNT transmission electron microscope photo figure of different silver-colored parcel amounts;Wherein, Fig. 1 is what a small amount of Ag was wrapped up
CNTs;Fig. 2 is the CNTs that thickness Ag is wrapped up;
Fig. 3 is present invention gained AgNPs@CNTs electric heating film diagrammatic cross-sections.
Embodiment
Embodiment 1
Nano-carbon material is cleaned, first with the HCl deionized water solution immersion nano-carbon material aqueous solution and carbon of the concentration for 20 mM
The mass ratio of material is 50:1, it is standby after 100 DEG C of drying by being cleaned by ultrasonic 30 minutes.Choose the surface sensitizing of certain mass
Agent stannous chloride(SnCl2)Mixed with watery hydrochloric acid(Concentration 5%), the mass ratio dimension 1 of sensitizer and watery hydrochloric acid:8, it is used as sensitizing solution.
Add cleaned nano-carbon material in sensitizing solution, the mass ratio of carbon material and sensitizer is 13:3, stir 5-10 minutes
After standing 6-10 hours under the conditions of room temperature afterwards, sediment is obtained.Sediment is cleaned 3 times with deionized water, Sn2+/CNTs is obtained
Suspension.Silver nitrate is added in Sn2+/CNTs suspension so that SnCl2 and AgNO3Mass ratio be 1.3, and CNTs with
AgNO3Mass ratio be 0.3, it is a small amount of to add D/W, Argent grain is reduced completely, solution stirring 10min leads to
Electrostatic interaction is crossed, AgNPs@CNTs sediments are obtained.Sediment is cleaned after 3 times with deionized water, and standby is dried through 80-100 degree
With.AgNPs CNTs after cleaning are mixed with the binding agent of commercially available silk-screen low temperature silver paste, AgNPs CNTs are in low-temperature sintering silver
It is 20% to starch the weight/mass percentage composition in binding agent,.Carbon silver is printed on the PET substrate of 0.8mm thickness with silk-screen printing technique
The low dimensional nano-sized carbon electric heating film for obtaining Nano Silver surface modification was as a child taken out in film, 130 DEG C of bakings 1.
Embodiment 2
The graphene oxide suspension prepared from routine techniques, adds the hexadecane that mass percent is 10% in suspension
Base trimethylammonium bromide, is stirred 30 minutes.Solution is heated up to 100 DEG C, AgNO is added into solution3The aqueous solution so that oxidation
Graphene and AgNO3Mass ratio be 1.0, be slow added into the concentration ratio 3-5 of the PVP aqueous solution, PVP and silver nitrate solution:1,
It is identical in quality.After stirring 1 hour, solution temperature drops to room temperature.Take out sediment after solution left standstill is precipitated, sediment spend from
It is standby after being dried through 80-100 degree after sub- water is cleaned 3 times.By the AgNPs graphene after cleaning and commercially available silk-screen low temperature silver paste
Binding agent is mixed, and the weight/mass percentage composition in AgNPs@CNTs binding agents is 10%.Printed with silk-screen printing technique on PET substrate
The low dimensional nano-sized carbon electric heating film for obtaining Nano Silver surface modification was as a child taken out in brush carbon Ag films, 150 DEG C of bakings 1.
Claims (1)
1. a kind of low dimensional nano-sized carbon electric heating film preparation method of Nano Silver surface modification, it is characterised in that this method include with
Lower specific steps:
Step 1:Received using surface replacement or/and chemical reduction method in low dimensional nano-carbon material surface modification or covering or parcel
Rice Argent grain, obtains the low dimensional nano-carbon material of surface finish nano Argent grain;Wherein low dimensional nano-carbon material is carbon nanometer
Pipe/fiber, grapheme material;
Step 2:It is prepared by Nano Silver@nano carbon composite materials
Pass through the low dimensional nano-carbon material and low temperature of the surface finish nano Argent grain of ball milling or stirring or roll-in method by obtained by
The mixing of silver paste binding agent is sintered, mixed proportion accounts for 6-35% for the low dimensional nano-carbon material of surface finish nano Argent grain;
Gross mass percentage compositions of the AgNPs in low-temperature sintering silver paste binding agent is 25-50%;
Step 3:Graphical carbon Ag films are directly prepared on flexible cryogenic substrate by silk-screen printing technique, through 130-180 DEG C
Under aerobic conditions after low-temperature sintering 30-90 minutes, the low dimensional nano-sized carbon electric heating film of the Nano Silver surface modification is obtained;Its
In:
It is described low dimensional nano-carbon material surface modification or covering or parcel nano-Ag particles, specifically include:
1)Nano-carbon material is cleaned, first with 20-60mM HCl deionized water solutions immersion low dimensional nano-carbon material, by super
Sound is cleaned 30 minutes, standby after 80-100 DEG C of drying;
2)The surface treatment of low dimensional nano-carbon material:
(a)Choose coating material to mix with watery hydrochloric acid, as sensitizing solution, cleaned low dimensional nanometer is added in sensitizing solution
Carbon material, after standing 6-10 hours under the conditions of room temperature after stirring 5-10 minutes, obtains sediment;Wherein, the sensitizer is chlorine
Change stannous(SnCl2), butter of tin (SnCl4) or stannous sulfate(SnSO4);The quality of low dimensional nano-carbon material and sensitizer
Than for 6 ~ 20:3, watery hydrochloric acid concentration 5-10%;
(b)Or mixed in deionized water with low dimensional nano-carbon material from surfactant, wherein, the surface
Activating agent is cetyl trimethylammonium bromide CTAB or Sodium Polyacrylate PAA;Surfactant and low dimensional nano-carbon material
Mass ratio be 5 ~ 8:10;
(c)Or by low dimensional nano-carbon material and dimethyl sulfoxide and ethylene glycol atom or group transfer reaction and polyelectrolyte hydroxyl
Base practices esterification with α-bromine isobutyl acylbromide or α-chlorpromazine chloride, completes the non-covalent modification of carbon nano tube surface;
3)Low dimensional nano-carbon material after surface treated is cleaned 3 times with deionized water, Nanocarbon-Y is obtained and suspends
Liquid;Wherein, Y is the modification cation in different modifying material;
4)Silver nitrate is added in Nanocarbon-Y suspension so that Y and AgNO3Mass ratio be 1-1.5, and
Nanocarbon and AgNO3Mass ratio be 0.8-1.5, add reducing agent, solution stirred into 10-30min, made by electrostatic
With or coordination, obtain AgNPs@Nanocarbon sediments;Wherein described reducing agent is glucose, chitosan, PVP, lemon
One kind in lemon acid sodium;
5)The AgNPs Nanocarbon sediments of acquisition are cleaned after 3 times with deionized water, through 80-100 DEG C of drying, table are obtained
Face is modified or covering or the low dimensional nano-carbon material for wrapping up nano-Ag particles.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113802372A (en) * | 2021-09-17 | 2021-12-17 | 陕西科技大学 | Ag nano particle coated SnS/C flexible thermoelectric fiber membrane and preparation method thereof |
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Application publication date: 20170922 |