CN109862631A - A kind of preparation method of NEW TYPE OF COMPOSITE plate Electric radiant Heating Film - Google Patents
A kind of preparation method of NEW TYPE OF COMPOSITE plate Electric radiant Heating Film Download PDFInfo
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- CN109862631A CN109862631A CN201910272686.2A CN201910272686A CN109862631A CN 109862631 A CN109862631 A CN 109862631A CN 201910272686 A CN201910272686 A CN 201910272686A CN 109862631 A CN109862631 A CN 109862631A
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Abstract
The present invention discloses a kind of preparation method of NEW TYPE OF COMPOSITE plate Electric radiant Heating Film, and this method is specifically by monobutyl-tin-trichloride (MBTC), SbCl3And NH4F is dissolved in the solvent that second alcohol and water configures in proportion as predecessor, as precursor liquid 1；It disperses silver nano-grain in deionized water as precursor liquid 2；Acrylic resin is configured to template to be added drop-wise in quartz substrate, the dry template network for forming chap；Precursor liquid 2 is added dropwise and is spun in the substrate to form template, dry after annealing processing；Precursor liquid 1 is deposited on and is heat-treated with the method for ultrasonic spray pyrolysis again；It makes electrode and forms electrothermal film device.The advantage of the invention is that outermost SnO 2 thin film makes it have stronger antioxygenic property, stable film layer resistance can be maintained in use；Silver nano-grain has excellent electric conversion efficiency, can reach higher temperature at low voltage；There is excellent translucency using quartz substrate simultaneously, light transmittance reaches 80% or more.
Description
Technical field
The invention belongs to heating material fields, and in particular to a kind of preparation method of NEW TYPE OF COMPOSITE flexible electrothermal membrane.Mainly
Using template spin-coating method and ultrasonic spray pyrolysis, what the conductive mesh network layers and Sb, F for preparing silver nano-grain composition were adulterated
SnO2The two-layer compound Electric radiant Heating Film of base film layer composition.
Background technique
In field of electric heating, there are resistance heating, electromagnetic induction heating and microwave heating three types, wherein using most wide
General is resistance heating manner.There are various heating elements in resistance heating, such as heating wire, electrothermal tube, electric hot plate, quartz ampoule, PTC
Heating element etc., in addition to PTC heating element, other heater elements are using heating wire as in heat source, using electric-heating-wire-heating in it
Mode continued more than 100 years.Electric radiant Heating Film constantly came out as the product of heating element in recent years.In fact, electrothermal film technology
Development and application had good decades, only because its enter civil field than later, in addition China is to electrothermal film technology
Development and application also than later, so people just seem stranger to Electric radiant Heating Film and products thereof.
Heated by electrothermal film belongs to resistance heating method, compared with other conductive exothermal materials, has more clear advantage,
Such as thermal efficiency height, energy saving, the service life is long, external form alternative is strong, applied widely, processing technology is simple, structure is simple, at
This low, flames of anger, safe and reliable etc..The conception of this heating technique is that foreign countries propose and begin one's study in early fifties,
Some industrially developed country, which proposed, at that time sets the fields such as petroleum delivery pipeline, wire and cable using film-type electric heating material
Apply carry out heat-preserving anti-freezing.
Electric radiant Heating Film is mainly made of conductive materials and film forming matter or film material.Different conductive materials and film forming matrix
Many kinds of Electric radiant Heating Films can be formed.Its processing method has plenty of and directly prepares film on being heated carrier, formed on carrier
Film cannot be separated with carrier, such as after conductive materials and film forming matter are mixed into slurry, coated in need to heat on object,
Film forming, spray pyrolysis film forming etc. is dried；Have plenty of electrothermic film element, such as conductive materials and film forming matter are mixed
Extrusion forming afterwards；Also some use the methods of physical vapour deposition (PVD), airless spraying, plasma spray, sputtering, make conductive material with it is membranaceous
Substrate group is integral, or transfer paper etc. is made in Electric radiant Heating Film slurry.
The current most common Electric radiant Heating Film is the composed structure that conductive wire is coiled in substrate, such electric heating membrane environment
The case where stability is poor, will appear wire oxidation or fracture in use causes resistivity to increase, so that power declines
Subtract serious.Also there is part Electric radiant Heating Film using semiconductor material, semiconductor thermoelectric film, also known as metal oxide Electric radiant Heating Film, being can be tight
Thickly combine on dielectric surfaces, become the film-form semi-conductive heating substance of planar heat source after energization, it have fusing point it is high,
The features such as hardness is big, resistance is low, the thermal efficiency is high, chemical stability is good, especially resistance to bronsted lowry acids and bases bronsted lowry, the during heating flames of anger
Characteristic.
The research work of domestic semiconductor thermoelectric film, the mainly tin dioxide film carried out earliest.Stannic oxide is this
The Typical Representative of metal-oxide semiconductor (MOS), it has important role in national defence and industrial technology.But two are prepared at present
The raw material of SnO 2 thin film is mainly stanniferous hydrochloride, so can generate a large amount of hydrochloric acid mist during the preparation process, not only
It can accelerate equipment corrosion, also have serious harm to the health of operator.The skill of tin dioxide thin film is currently prepared simultaneously
Art is still relatively rough, can not prepare the film of high quality, more serious so as to cause power attenuation, therefore can not also advise greatly
Mould application.
In view of the above problems, the present invention is combined by template spin-coating method and ultrasonic spray pyrolysis prepares two-layer compound knot
The Electric radiant Heating Film of structure solves.The network-like silver nano-grain conductive layer prepared first with template, more uniformly spreads, no
The problem of will appear hot-spot, while the conductive network that template is prepared is not in contact resistance, prevents from using
It is excessive and make wire breakage to occur contact resistance in journey.In addition to this tin source that the present invention uses is MBTC, in preparation process
In will not generate serious acid mist, production environment is more friendly, and the thin film composition prepared using ullrasonic spraying is uniform, ensure that
Certain service life.
Summary of the invention
Oxidizable it is an object of the invention to solve wire Electric radiant Heating Film environmental stability difference, tin oxide Electric radiant Heating Film produces ring
The problems such as border is severe provides a kind of preparation method of NEW TYPE OF COMPOSITE plate Electric radiant Heating Film.
The present invention solves the above problems by the following technical programs:
A kind of NEW TYPE OF COMPOSITE plate Electric radiant Heating Film, main body are the conductive mesh network layers that silver nano-grain is constituted and Sb, F doping
SnO2The two-layer compound electric heating membrane structure of base film layer composition, wherein for the diameter of silver nano-grain between 20-30nm, silver is conductive
The thickness of layer is adjusted between 50-200nm, and total doping ratio of Sb, F are to be adjusted between the 2%-15% of Sn, SnO2Base
The thickness of film layer is adjusted between 100-300nm.Silver nano-grain conductive layer has excellent electric conductivity, and tin oxide is thin
Film layer can enhance the stability in use of Electric radiant Heating Film.
The NEW TYPE OF COMPOSITE plate Electric radiant Heating Film, it is specific the preparation method is as follows:
Step 1, by monobutyl-tin-trichloride (MBTC), SbCl3And NH4F is dissolved in second alcohol and water in proportion as predecessor
In the solvent of configuration, as precursor liquid 1；
Step 2, it disperses commercially available silver nano-grain in deionized water, forms 0.01mg.mL-1Solution, as forerunner
Liquid 2；
Step 3, acrylic resin is dissolved in the template that 0.4g/mL is configured in diluent；
Step 4, template obtained in step 3 is added drop-wise in quartz substrate, and is coated uniformly, then using spin-coating method
It dries in air, the template network of self-assembling formation chap；
Step 5, precursor liquid 2 is added drop-wise in the substrate for having formed template, and is coated uniformly using spin-coating method, and drying
It is dry in case, and cleaned out template with chloroform；
Step 6, precursor liquid 1 is deposited to and forms tin oxide base thin film in substrate, finally with the method for ultrasonic spray pyrolysis
It is heat-treated again；
Step 7, the half-finished product of electric heating film both ends prepared are stained with copper electrode band with elargol, form electrothermal film device.
When coating in step 4 and 5 using spin-coating method, most start that institute's spin coating liquid should be made within spin coating 15 seconds under the revolving speed of 600rpm
Body uniformly scatter, and later again by rotational speed regulation between 1000-2000rpm, the time of coating is between 15-50 seconds.
The ultrasonic spray pyrolysis method of step 6, device following points improve:
1. being also equipped with precise pressure-reducing valve in carrier gas inlet, can be divided with accuracy controlling carrier gas；2. precursor liquid arrival end is furnished with
Supersonic frequency regulation module can be used for adjusting different supersonic frequencies to obtain the droplet of different fogging degrees；3. in reaction chamber
Main heating module is arranged in bottom end, and maximum temperature can reach 700 DEG C or more, and auxiliary heating module is arranged in reaction chamber side, to guarantee
Whole environment temperature.
The power of ullrasonic spraying is 1-3W, and carrier gas is that compressed air partial pressure is 0.02-0.04MPa.
Used quartz glass substrate needs first to be placed on acetone, dehydrated alcohol, is cleaned by ultrasonic in deionized water,
Every kind of reagent at least cleans 10min, is finally rinsed in drying box and is dried for standby with dehydrated alcohol.
The temperature in deposition film stage, main heating module controls between 300-600 DEG C, and the temperature of auxiliary heating module is
Between 200-300 DEG C, sedimentation time 10-60min；Temperature when heat treatment should be slightly below main heating module when film deposition
Temperature, time of heat treatment is 30min-60min.
The present invention prepares film by the way of ultrasonic spray pyrolysis, and the film layer structure of acquisition is more uniform, and film
Thickness is easy to control, thus the Electric radiant Heating Film power adjustable section of preparation.
Half-finished product of electric heating film is dried and is made annealing treatment in the present invention combination that can be enhanced between film and substrate
Power.Using transparent quartz glass as base material in the present invention, the Electric radiant Heating Film light transmittance of preparation is higher, and application range is more
Extensively.Electric radiant Heating Film endothecium structure is that Silver nano-particle layer ensure that excellent electric conductivity, outer layer Sb, F doping in the present invention
Tin oxide film layer not only ensure that electric conductivity but also the oxidation of Silver nano-particle layer can be prevented.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the ultrasonic spray pyrolysis equipment used；
Wherein: the main heating module 6. of 1. ultrasonic nozzle, 2. precursor liquid entrance, 3. carrier gas inlet, 4. reaction chamber 5. assists
7. quartz plate substrate of heating module, 8. bearing rotating module, 9. negative pressure ventilation module；
Fig. 2 is spin coating device schematic diagram；
Fig. 3 is the schematic diagram that template prepares silver nano-grain conductive layer；
The schematic diagram of the position Fig. 4 electrothermal film device.
Specific embodiment
NEW TYPE OF COMPOSITE plate Electric radiant Heating Film, it is characterised in that main body is that the conductive mesh network layers that silver nano-grain is constituted and Sb, F mix
Miscellaneous SnO2The two-layer compound electric heating membrane structure of base film layer composition.
It is specific the preparation method is as follows: step 1, by monobutyl-tin-trichloride (MBTC), SbCl3And NH4F as predecessor,
It is dissolved in the solvent that second alcohol and water configures in proportion, as precursor liquid 1；Step 2, deionization is dispersed by commercially available silver nano-grain
In water, 0.01mg.mL is formed-1Solution, as precursor liquid 2；Step 3, acrylic resin is dissolved in diluent and is configured to
The template of 0.4g/mL；Step 4, template obtained in step 3 is added drop-wise in quartz substrate, and is coated using spin-coating method
Uniformly, it then dries in air, the template network of self-assembling formation chap；Step 5, precursor liquid 2 is added drop-wise to and has formed mould
It in the substrate of plate, and is coated uniformly using spin-coating method, and dry in the baking oven of certain temperature, and is cleared up template with chloroform
Completely；Step 6, precursor liquid 1 is deposited to and forms tin oxide base thin film in substrate, finally again with the method for ultrasonic spray pyrolysis
It is heat-treated；Step 7, the half-finished product of electric heating film both ends prepared are stained with copper electrode band with elargol, form electrothermal film device.
Embodiment 1: template prepares the conductive film of silver nano-grain
Step 1, it disperses commercially available silver nano-grain in deionized water, forms 0.01mg.mL-1Solution, as forerunner
Liquid；Step 2, acrylic resin is dissolved in the template that 0.4g/mL is configured in diluent；It step 3, will be obtained in step 2
Template is added drop-wise in quartz substrate, and is coated uniformly using spin-coating method, is then dried in air, the mould of self-assembling formation chap
Expanded metals network；Step 4, precursor liquid is added drop-wise in the substrate for having formed template, and is coated uniformly using spin-coating method, and certain
It is dry in the baking oven of temperature, and cleaned out template with chloroform；Step 5, the half-finished product of electric heating film both ends prepared are used
Elargol is stained with copper electrode band, forms electrothermal film device.
The conductive film for the silver nano-grain prepared, when changing the thickness of coating (50-200nm), sheet resistance is in 15-40
Change between Ω/sq, coating thickness is thicker, and sheet resistance is smaller, but as film layer thickens, light transmittance is reduced to from 90%
85%.Under the driving of 6V voltage, the attainable equilibrium temperature of highest is 73 DEG C, and thermal response time is 25 seconds.Simple Yin Na
Rice grain conductive film heats 30 days in continuous logical 6V voltage, and sheet resistance increases 76.5%, and environmental stability is very poor.
Embodiment 2: ultrasonic spray pyrolysis prepares the SnO 2 thin film of F, Sb doping
Step 1, by monobutyl-tin-trichloride (MBTC), SbCl3And NH4F is dissolved in second alcohol and water in proportion as predecessor
In the solvent of configuration, as precursor liquid；Step 2, precursor liquid is deposited to the method for ultrasonic spray pyrolysis and forms oxygen in substrate
Change tinbase film, is finally heat-treated again；Step 3, the half-finished product of electric heating film both ends prepared are stained with copper electrode with elargol
Band forms electrothermal film device.
By the doping ratio of F and Sb, total doping ratio regulates and controls between 2%-15%, and sheet resistance is in 60-300 Ω/sq
Between change, with the raising of doping ratio, sheet resistance first becomes smaller to become larger afterwards.Under the driving of 6V voltage, highest is attainable steady
Determining temperature is 56 DEG C, and thermal response time is 40 seconds.The SnO 2 thin film of simple F, Sb doping is in continuous logical 6V voltage heating 30
It, power attenuation 13.6%, environmental stability is relatively preferable, but electric conductivity is general, and thermal response time is slower.
Embodiment 3: preparation two-layer compound Electric radiant Heating Film
Step 1, by monobutyl-tin-trichloride (MBTC), SbCl3And NH4F is dissolved in second alcohol and water in proportion as predecessor
In the solvent of configuration, as precursor liquid 1；Step 2, it disperses commercially available silver nano-grain in deionized water, is formed
0.01mg.mL-1Solution, as precursor liquid 2；Step 3, acrylic resin is dissolved in the mould that 0.4g/mL is configured in diluent
Plate agent；Step 4, template obtained in step 3 is added drop-wise in quartz substrate, and is coated uniformly using spin-coating method, then existed
Air drying, the template network of self-assembling formation chap；Step 5, precursor liquid 2 is added drop-wise in the substrate for having formed template,
And it is coated uniformly using spin-coating method, and dry in the baking oven of certain temperature, and cleaned out template with chloroform；Step 6,
With the method for ultrasonic spray pyrolysis by precursor liquid 1, deposits to and form tin oxide base thin film in substrate, be finally heat-treated again；
Step 7, the half-finished product of electric heating film both ends prepared are stained with copper electrode band with elargol, form electrothermal film device.
The Electric radiant Heating Film of this double-layer structure is the thickness of silver nanoparticle layer respectively, it can be achieved that power adjustable, there are two types of adjustment mechanisms
The doping ratio of degree and outer oxide tin layers.Under the driving of 6V voltage, the attainable equilibrium temperature of highest is 230 DEG C, heat
Response time is 20 seconds.Continuously logical 6V voltage heats 30 days, and power attenuation only has 8%, it is seen that the good energy of its environmental stability
Enough prolong the service life.
Claims (7)
1. a kind of NEW TYPE OF COMPOSITE plate Electric radiant Heating Film, which is characterized in that main body be silver nano-grain constitute conductive mesh network layers and Sb,
The SnO of F doping2Base film layer composition two-layer compound electric heating membrane structure, wherein the diameter of silver nano-grain 20-30nm it
Between, for the thickness of conductive mesh network layers between 50-200nm, total foreign atom ratio of Sb, F are the 2%-15%, SnO of Sn2Base is thin
The thickness of film layer is between 100-300nm.
2. a kind of method for preparing NEW TYPE OF COMPOSITE plate Electric radiant Heating Film as described in claim 1, which is characterized in that including walking as follows
It is rapid:
Step 1, by monobutyl-tin-trichloride (MBTC), SbCl3And NH4F is dissolved in second alcohol and water and configures in proportion as predecessor
Solvent in, as precursor liquid 1；
Step 2, it disperses commercially available silver nano-grain in deionized water, forms 0.01mg.mL-1Solution, as precursor liquid 2；
Step 3, acrylic resin is dissolved in the template that 0.4g/mL is configured in diluent；
Step 4, template obtained in step 3 is added drop-wise in quartz substrate, and is coated using spin-coating method uniformly, then in sky
It is dry in gas, the template network of self-assembling formation chap；
Step 5, precursor liquid 2 is added drop-wise in the substrate for having formed template, and is coated uniformly using spin-coating method, and in an oven
It is dry, template is cleaned out with chloroform；
Step 6, precursor liquid 1 is deposited to the method for ultrasonic spray pyrolysis and forms tin oxide base thin film in substrate, carry out hot place
Reason；
Step 7, the half-finished product of electric heating film both ends prepared are stained with copper electrode band with elargol, form electrothermal film device.
3. the preparation method of NEW TYPE OF COMPOSITE plate Electric radiant Heating Film according to claim 2, which is characterized in that institute in step 4 and 5
The spin-coating method stated, when coating most start should under the revolving speed of 600rpm spin coating 15 seconds, later again by rotational speed regulation in 1000-
Between 2000rpm, the time of coating is between 15-50 seconds.
4. the preparation method of NEW TYPE OF COMPOSITE plate Electric radiant Heating Film according to claim 2, which is characterized in that the ultrasound spray
It is divided equipped with precise pressure-reducing valve for accuracy controlling carrier gas in the device that mist method for pyrolysis uses in carrier gas inlet, in precursor liquid
Arrival end, for regulating and controlling supersonic frequency to obtain the drop of different fogging degrees, is matched equipped with supersonic frequency regulation module in reaction chamber
The auxiliary heating module set on the main heating module of reaction chamber bottom and set on reaction chamber side is had, to guarantee environment temperature.
5. the preparation method of NEW TYPE OF COMPOSITE plate Electric radiant Heating Film according to claim 4, which is characterized in that the step 6
At 300-600 DEG C, the temperature of auxiliary heating module is for the temperature control of main heating module in reaction chamber when middle ultrasonic spray pyrolysis
200-300 DEG C, sedimentation time 10-60min；Main heating block temperature when temperature when heat treatment should be lower than film deposition,
The time of heat treatment is 30min-60min.
6. the preparation method of NEW TYPE OF COMPOSITE plate Electric radiant Heating Film according to claim 2, which is characterized in that the ultrasound spray
The power of mist is 1-3W, and carrier gas is that compressed air partial pressure is 0.02-0.04MPa.
7. the preparation method of NEW TYPE OF COMPOSITE plate Electric radiant Heating Film according to claim 2, which is characterized in that the quartz glass
Substrate needs first to be placed on acetone, dehydrated alcohol, is cleaned by ultrasonic in deionized water, and every kind of reagent at least cleans 10min, most
It is rinsed in drying box and is dried for standby with dehydrated alcohol afterwards.
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Cited By (4)
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| CN112752360A (en) * | 2020-08-17 | 2021-05-04 | 杭州热威电热科技股份有限公司 | Al3+、Ga3+、Ag+Doped ZnO-based electrothermal film, preparation device and preparation method |
| CN113140833A (en) * | 2021-04-14 | 2021-07-20 | 星光新能源科技(深圳)有限公司 | Battery module with heating function |
| CN114242906A (en) * | 2021-12-23 | 2022-03-25 | 佛山仙湖实验室 | Preparation method of tin oxide electron transport layer and perovskite solar cell |
| CN115121466A (en) * | 2022-07-11 | 2022-09-30 | 桂阳县华毅石墨有限公司 | Supported preformed nano silver film and preparation method and application thereof |
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