CN107197551A - A kind of thin film heater and preparation method thereof - Google Patents
A kind of thin film heater and preparation method thereof Download PDFInfo
- Publication number
- CN107197551A CN107197551A CN201710554359.7A CN201710554359A CN107197551A CN 107197551 A CN107197551 A CN 107197551A CN 201710554359 A CN201710554359 A CN 201710554359A CN 107197551 A CN107197551 A CN 107197551A
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- thin film
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- film heater
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Classifications
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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
- H05B3/20—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
-
- 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
- H05B3/14—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 the material being non-metallic
- H05B3/145—Carbon only, e.g. carbon black, graphite
-
- 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
- H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
- H05B2203/013—Heaters using resistive films or coatings
-
- 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
- H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
- H05B2203/017—Manufacturing methods or apparatus for heaters
Abstract
The invention provides a kind of preparation method of thin film heater, comprise the following steps:One layer of carbon nano-tube solution coating is set in substrate, coated substrate is obtained;The coated substrate is washed, the coated substrate after being washed;The coated substrate after the washing is handled using salpeter solution, conductive film substrate is obtained;A pair of electrodes is set in the conductive film substrate, thin film heater is obtained.The preparation method for the thin film heater that the present invention is provided is simple, easy to use.Present invention also offers the thin film heater that the preparation method described in a kind of above-mentioned technical proposal any one is obtained, comprising substrate, the carbon nanotube conductive thin film of the substrate surface is arranged at, and is arranged at a pair of electrodes on the carbon nanotube conductive thin film surface.The thin film heater that the present invention is provided can be used in the form of the plane or in the form of curved surface.
Description
Technical field
The present invention relates to heater technical field, more particularly to a kind of thin film heater and preparation method thereof.
Background technology
Flexible, thin film heater is that a class controls the power that FPC is produced, work(by applying voltage on loop
A part for rate is converted to fuel factor, so as to reach the heater that purpose is heated to object.
In the prior art, flexible, thin film heater mainly makes loop with plain conductor, by applying electricity on loop
Pressure, to control the power that FPC is produced.The requirement of flexible, thin film heater not only to plain conductor is high, and to production
Also there are strict requirements with use environment, production technology is excessively cumbersome.
The content of the invention
It is an object of the invention to provide simple, easy to use thin film heater of a kind of technique and preparation method thereof.
In order to realize foregoing invention purpose, the present invention provides following technical scheme:
The invention provides a kind of preparation method of thin film heater, comprise the following steps:
One layer of carbon nano-tube solution coating is set in substrate, coated substrate is obtained;
The coated substrate is washed, the coated substrate after being washed;
The coated substrate after the washing is handled using salpeter solution, conductive film substrate is obtained;
A pair of electrodes is set in the conductive film substrate, thin film heater is obtained.
It is preferred that, the substrate is PET substrate or polyimide substrate.
It is preferred that, the CNT is single-walled carbon nanotube or multi-walled carbon nanotube.
It is preferred that, external diameter≤2nm of the single-walled carbon nanotube, length is 5~30 μm.
It is preferred that, the carbon nano-tube solution includes CNT, dispersant and water;
The dispersant is neopelex or lauryl sodium sulfate.
It is preferred that, the mass ratio of the CNT and dispersant is (8~12):1;
Concentration of the CNT in carbon nano-tube solution is 0.05~0.2mg/mL.
It is preferred that, described to set the process of one layer of carbon nano-tube solution coating to carry out under an inert atmosphere in substrate, institute
The temperature for stating substrate is 101~110 DEG C.
It is preferred that, the electrode is copper conductive adhesive or silver conductive adhesive.
Present invention also offers the thin film heater that the preparation method described in a kind of above-mentioned technical proposal any one is obtained,
Comprising substrate, the carbon nanotube conductive thin film of the substrate surface is arranged at, and is arranged at the carbon nanotube conductive thin film
The a pair of electrodes on surface.
The invention provides a kind of preparation method of thin film heater, comprise the following steps:One layer of carbon is set in substrate
Nanotube solution coating, obtains coated substrate;The coated substrate is washed, the coated substrate after being washed;Use
Salpeter solution is handled the coated substrate after the washing, obtains conductive film substrate;In the conductive film substrate
A pair of electrodes is set, thin film heater is obtained.The preparation method for the thin film heater that the present invention is provided is simple, easy to use.
Present invention also offers the thin film heater that the preparation method described in a kind of above-mentioned technical proposal any one is obtained,
Comprising substrate, the carbon nanotube conductive thin film of the substrate surface is arranged at, and is arranged at the carbon nanotube conductive thin film
The a pair of electrodes on surface.The thin film heater that the present invention is provided can be used in the form of the plane or in the form of curved surface,
And with high light transmittance, fast heating rate and the characteristics of low surface resistance, when light transmittance is more than 70%, surface resistance as little as 94.7
Ω/sq;Under 35V voltages, heater heating rate is up to 6.1 DEG C/s.
Brief description of the drawings
Fig. 1 is the schematic flow sheet that embodiment 1 prepares thin film heater;
Fig. 2 is pressurization schematic diagram of the embodiment 1 to thin film heater;
Fig. 3 is the heat transfer schematic diagram that the midplane of embodiment 1 is heated;
Fig. 4 is the heating curve of the thin film heater of embodiment 1 film surface under different voltages;
Fig. 5 is the temperature lowering curve of 50 DEG C of distilled water;
Fig. 6 is the temperature lowering curve of 60 DEG C of distilled water;
Fig. 7 is the SEM image of the thin film heater of different conditions, the film heating that wherein a obtains for omission nitric acid treatment
The SEM image of device, b is omits the SEM image for the thin film heater that the water-washing process before nitric acid treatment is obtained, and c obtains for embodiment 1
The SEM image of the thin film heater arrived;
Fig. 8 is the heat transfer schematic diagram that the mean camber of embodiment 3 is heated.
Embodiment
The invention provides a kind of preparation method of thin film heater, comprise the following steps:
One layer of carbon nano-tube solution coating is set in substrate, coated substrate is obtained;
The coated substrate is washed, the coated substrate after being washed;
The coated substrate after the washing is handled using salpeter solution, conductive film substrate is obtained;
A pair of electrodes is set in the conductive film substrate, thin film heater is obtained.
The present invention sets one layer of carbon nano-tube solution coating in substrate, obtains coated substrate.In the present invention, the base
Bottom is preferably PET substrate or polyimide substrate.The present invention is to the polyethylene terephthalate
Ester group bottom and the source of polyimide substrate are gathered to benzene without any particular/special requirement using what those skilled in the art commonly used
Naphthalate substrate and polyimide substrate.The present invention do not have to the thickness of the substrate it is any it is special will
Ask, be configured according to specific technological requirement.
In the present invention, the CNT is preferably single-walled carbon nanotube or multi-walled carbon nanotube.The present invention is to described
Commonly used without any particular/special requirement using those skilled in the art in the source of single-walled carbon nanotube and multi-walled carbon nanotube
Single-walled carbon nanotube and multi-walled carbon nanotube.In the present invention, the external diameter of the single-walled carbon nanotube it is preferred≤2nm,
More preferably≤1.5nm, most preferably≤1nm;The length of the single-walled carbon nanotube is preferably 5~30 μm, more preferably 10
~25 μm, most preferably 15~20 μm.
In the present invention, the carbon nano-tube solution preferably comprises CNT, dispersant and water;The dispersant is preferred
For neopelex (SDBS) or lauryl sodium sulfate (SDS).In the present invention, the CNT and dispersant
Mass ratio be preferably (8~12):1, more preferably (9~11):1, most preferably 10:1;The CNT is in CNT
Concentration in solution is preferably 0.05~0.2mg/mL, more preferably 0.08~0.15mg/mL, most preferably 0.1mg/mL.This
The carbon nano-tube solution that the preferred first configuration concentration of invention is 0.5~2mg/mL, is then diluted to 0.05~0.2mg/mL again,
To reduce loss of the CNT in configuration process.
After the present invention preferably mixes the CNT, dispersant and water, obtained mixed liquor is sequentially subjected to water-bath
Ultrasonically treated and ultrasonic grinder is ultrasonically treated.In the present invention, the power of water bath sonicator processing be preferably 80~
120W, more preferably 100~110W;The time of the water bath sonicator processing is preferably 30~50min, more preferably 35~
45min, most preferably 40min.In the present invention, the ultrasonically treated power of the ultrasonic grinder is preferably 100~120W,
More preferably 105~110W;The ultrasonic grinder ultrasonically treated time is preferably 60~80min, more preferably 65~
75min, most preferably 70min.
The ultrasonically treated obtained mixed liquor of ultrasonic grinder described in preferred pair of the present invention carries out centrifugal treating, obtains supernatant
Liquid.In the present invention, the centrifugation rate of the centrifugal treating is preferably 7000~9000r/min, more preferably 7500~
8500r/min, most preferably 8000r/min;The centrifugation time of the centrifugal treating is preferably 10~30min, and more preferably 15
~25min, most preferably 20min.The supernatant that the present invention preferably obtains centrifugal treating is used for carbon nano-tube solution coating.
In the present invention, it is described that the process of one layer of carbon nano-tube solution coating is set preferably under an inert atmosphere in substrate
Carry out, more preferably nitrogen atmosphere.In the present invention, the temperature of the substrate is preferably 101~110 DEG C, more preferably 105~
108℃.The carbon nano-tube solution is arranged on high temperature substrate by the present invention, while coating is set, enables to carbon to receive
Water evaporation in mitron solution, leaves behind CNT and dispersant.
It is described to set one layer of carbon nano-tube solution coating to be preferred to use spraying in substrate in the specific embodiment of the invention
Mode is carried out.The present invention does not have any particular/special requirement to the embodiment of the spraying, using those skilled in the art
Known spraying method is carried out.The present invention do not have to the thickness of the carbon nano-tube solution coating it is any it is special will
Ask, can be configured according to specific technological requirement.
Obtain after the coated substrate, the present invention is washed to the coated substrate, the coated substrate after being washed.
In the present invention, the washing can remove in setting coating procedure and there may be impurity, moreover it is possible to while tentatively removing dispersant.
The present invention does not have any particular/special requirement to the mode of the washing, and the water-washing method commonly used using those skilled in the art is entered
Row.
Processing is dried in coated substrate after being washed described in preferred pair of the present invention, and the temperature of the drying process is preferably
50~70 DEG C, most preferably more preferably 55~65 DEG C, 60 DEG C;The time of the drying process is preferably 1~3h, more preferably
2h。
Obtain after the coated substrate after the washing, the present invention is entered using salpeter solution to the coated substrate after the washing
Row processing, obtains conductive film substrate.In the present invention, the salpeter solution is preferably to be obtained after mixing concentrated nitric acid and water;
The mass concentration of the concentrated nitric acid is preferably 65~70%, and more preferably 68%;The volume ratio of the concentrated nitric acid and water is preferably
(5~7):1, more preferably 6:1.In the present invention, the salpeter solution has oxidisability, while also hydrogen ion, Ke Yiyu
Dispersant is combined, and the dispersant in coated substrate is removed.
In the present invention, salpeter solution processing it is specific be by the coated substrate after the washing in salpeter solution
Soaked;The time of the immersion is preferably 30~50min, more preferably 35~45min, most preferably 40min.
Coated substrate after nitric acid treatment described in preferred pair of the present invention is sequentially washed and drying process.The present invention is to institute
Stating the mode of washing does not have any particular/special requirement, and the water-washing method commonly used using those skilled in the art is carried out.
In the present invention, the washing can wash away the nitric acid and other impurity sticked in coated substrate.In the present invention, at the drying
The temperature of reason is preferably 50~70 DEG C, more preferably 55~65 DEG C, most preferably 60 DEG C;The time of the drying process is preferably
1~3h, more preferably 2h.
Obtain after the conductive film substrate, the present invention sets a pair of electrodes in the conductive film substrate, obtains thin
Film heater.In the present invention, the electrode is copper conductive adhesive or silver conductive adhesive.The present invention does not appoint to the size of the electrode
What particular/special requirement, is configured according to the size of substrate and specific technological requirement.In the present invention, the electrode
Width be preferably 4~6mm, more preferably 5mm.The present invention does not have any particular/special requirement to the method to set up of the electrode,
It is configured using conventional method well-known to those skilled in the art.
Source of the invention to the copper conductive adhesive and silver conductive adhesive is without any particular/special requirement, using art technology
Copper conductive adhesive and silver conductive adhesive that personnel commonly use.
Present invention also offers the thin film heater that the preparation method described in a kind of above-mentioned technical proposal any one is obtained,
Comprising substrate, the carbon nanotube conductive thin film of the substrate surface is arranged at, and is arranged at the carbon nanotube conductive thin film
The a pair of electrodes on surface.The thin film heater that the present invention is provided can be used in the form of the plane or in the form of curved surface.
Thin film heater provided with reference to embodiment the present invention and preparation method thereof is described in detail, still
They can not be interpreted as limiting the scope of the present invention.
Embodiment 1
With purity>95wt%, external diameter<2nm, length is that 5~30 μm of single-walled carbon nanotube is raw material, and SDBS is as scattered
Agent, distilled water is solvent.Using CNT and SDBS ratio as 10:1 is weighed, and then adds the distillation of corresponding proportion
Water so that concentration of the single-walled carbon nanotube in dispersion liquid is 1mg/mL, then first with 100W power water bath sonicator 40min,
Use ultrasonic grinder to carry out ultrasound 70min with 120W power again, then centrifuged with centrifuge with 8000r/min speed
20min, extracts supernatant, obtains concentration about 1mg/mL carbon nano tube dispersion liquid.
The dispersion liquid prepared is diluted 10 times, the solution that concentration is about 0.1mg/mL is obtained, then again by cleaned PET
Film is pasted on hot plate, and the temperature control in heating plate is sprayed at 105 DEG C, then with spray gun with nitrogen.It will spray
To coated substrate washed, 2h is dried with 60 DEG C of temperature after washing.
By mass concentration for 68% concentrated nitric acid and water with 6:1 volume ratio mixing, obtains salpeter solution.By above-mentioned drying
Obtained coated substrate is immersed in salpeter solution, and the immersion laggard water-fillings of 40min are washed, and 2h is dried with 60 DEG C of temperature after washing,
Obtain conductive film substrate.
A pair of copper electrodes are set in obtained conductive film substrate, thin film heater is obtained.
The schematic flow sheet that the present embodiment prepares thin film heater is as shown in Figure 1.
The present embodiment loads different voltages to thin film heater two ends and carries out Heating Experiment, and the present embodiment is to film heating
The pressuring method schematic diagram of device is as shown in Fig. 2 the heat transfer schematic diagram of the present embodiment midplane heating is as shown in Figure 3.
The heating curve for thin film heater film surface under different voltages that the present embodiment is provided is as shown in figure 4, by Fig. 4
Understand under different voltage, the response time of film electric heater is different, and the response time is most short under 35V voltages.
Tested by taking 35V as an example, the distillation moisture that initial temperature is respectively 50 DEG C and 60 DEG C is being placed on the thin of energization
On film heater, water temperature is measured, the temperature lowering curve of distilled water is obtained respectively as shown in the good Fig. 6 of Fig. 5.Wherein, Fig. 5 is 50
The temperature lowering curve of DEG C distilled water, Fig. 6 is the temperature lowering curve of 60 DEG C of distilled water;In Fig. 5 and Fig. 6, PET refers to PET in the present embodiment
The thin film heater of substrate, CNT-TCF- I, CNT-TCF- II and CNT-TCF- III are represented with CNT-TCF- I, CNT-TCF- respectively
The thin film heater that II and CNT-TCF- III is obtained as substrate.
Nonlinear fitting is carried out to the curve in Fig. 5 and Fig. 6, corresponding fitting formula is obtained:
(a)(50 DEG C of water);
(b)(60 DEG C of water).
In formula (a) and formula (b), T1, T2- real time temperature;T1 *, T2 *- steady temperature is represented, that is, carry out hot friendship with the external world
Change temperature when reaching balance;Tc- the maximum temperature difference with environment;k1, k2In the formula of-calibration factor, time quantum and temperature
Error is calibrated by this parameter;The t- times.
Embodiment 2
Scheme in embodiment 1 is improved, to obtain the thin film heater of different conditions.
Scheme one:
Nitric acid treatment step is omitted, remaining process is constant;
Scheme two:
The water-washing process before nitric acid treatment is omitted, remaining process is constant.
The SEM image of the thin film heater of different conditions is as shown in fig. 7, wherein a obtains to omit nitric acid treatment in the present invention
The SEM image of the thin film heater arrived, the SEM image for the thin film heater that b obtains for the water-washing process before omission nitric acid treatment,
C is the SEM image for the thin film heater that embodiment 1 is obtained.
As shown in Figure 7, the thin film heater surface impurity that embodiment 1 is obtained is significantly reduced.
Embodiment 3
Using multi-walled carbon nanotube as raw material, SDBS is as dispersant, and distilled water is solvent.With CNT and SDBS ratio
Example is 10:1 is weighed, and then adds the distilled water of corresponding proportion so that concentration of the single-walled carbon nanotube in dispersion liquid is
1mg/mL, then first with 100W power water bath sonicator 40min, then uses ultrasonic grinder to carry out ultrasound with 120W power
70min, then extracted supernatant with 8000r/min speed centrifugation 20min with centrifuge, obtain concentration about 1mg/mL carbon
Nanotube dispersion liquid.
The dispersion liquid prepared is diluted 10 times, the solution that concentration is about 0.1mg/mL is obtained, then again by cleaned PET
Film is pasted on hot plate, and the temperature control in heating plate is sprayed at 105 DEG C, then with spray gun with nitrogen.It will spray
To coated substrate washed, 2h is dried with 60 DEG C of temperature after washing.
By mass concentration for 68% concentrated nitric acid and water with 6:1 volume ratio mixing, obtains salpeter solution.By above-mentioned drying
Obtained coated substrate is immersed in salpeter solution, and the immersion laggard water-fillings of 40min are washed, and 2h is dried with 60 DEG C of temperature after washing,
Obtain conductive film substrate.
A pair of copper electrodes are set in obtained conductive film substrate, thin film heater is obtained.
The thin film heater that the present embodiment is obtained is used in the form of curved surface, and view when it is used is such as
Shown in Fig. 8.
As seen from the above embodiment, the invention provides a kind of preparation method of thin film heater, comprise the following steps:
One layer of carbon nano-tube solution coating is set in substrate, coated substrate is obtained;The coated substrate is washed, obtained after washing
Coated substrate;The coated substrate after the washing is handled using salpeter solution, conductive film substrate is obtained;Described
A pair of electrodes is set in conductive film substrate, thin film heater is obtained.The preparation method letter for the thin film heater that the present invention is provided
It is single, it is easy to use.
Present invention also offers the thin film heater that the preparation method described in a kind of above-mentioned technical proposal any one is obtained,
Comprising substrate, the carbon nanotube conductive thin film of the substrate surface is arranged at, and is arranged at the carbon nanotube conductive thin film
The a pair of electrodes on surface.The thin film heater that the present invention is provided can be used in the form of the plane or in the form of curved surface.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of preparation method of thin film heater, is comprised the following steps:
One layer of carbon nano-tube solution coating is set in substrate, coated substrate is obtained;
The coated substrate is washed, the coated substrate after being washed;
The coated substrate after the washing is handled using salpeter solution, conductive film substrate is obtained;
A pair of electrodes is set in the conductive film substrate, thin film heater is obtained.
2. preparation method according to claim 1, it is characterised in that the substrate is polyethylene terephthalate base
Bottom or polyimide substrate.
3. preparation method according to claim 1, it is characterised in that the CNT is single-walled carbon nanotube or many walls
CNT.
4. preparation method according to claim 3, it is characterised in that external diameter≤2nm of the single-walled carbon nanotube, length
For 5~30 μm.
5. the preparation method according to Claims 1 to 4 any one, it is characterised in that the carbon nano-tube solution is included
CNT, dispersant and water;
The dispersant is neopelex or lauryl sodium sulfate.
6. preparation method according to claim 5, it is characterised in that the mass ratio of the CNT and dispersant is (8
~12):1;
Concentration of the CNT in carbon nano-tube solution is 0.05~0.2mg/mL.
7. preparation method according to claim 1, it is characterised in that described that one layer of carbon nano-tube solution is set in substrate
The process of coating is carried out under an inert atmosphere, and the temperature of the substrate is 101~110 DEG C.
8. preparation method according to claim 1, it is characterised in that the electrode is copper conductive adhesive or silver conductive adhesive.
9. the thin film heater that the preparation method described in claim 1~8 any one is obtained, comprising substrate, be arranged at it is described
The carbon nanotube conductive thin film of substrate surface, and it is arranged at a pair of electrodes on the carbon nanotube conductive thin film surface.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114258167A (en) * | 2020-09-23 | 2022-03-29 | 天津工业大学 | Preparation method of carbon nanotube/glass fiber cloth flexible film heater |
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CN104575687A (en) * | 2014-10-28 | 2015-04-29 | 天津工业大学 | Carbon nano tube flexible and transparent conductive thin film with strong adhesive force and method for preparing thin film |
CN106060983A (en) * | 2016-06-03 | 2016-10-26 | 苏州捷迪纳米科技有限公司 | Low-voltage driven high-temperature electrothermal film, electric heating module and preparation method of low-voltage driven high-temperature electrothermal film |
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CN103531304A (en) * | 2013-09-18 | 2014-01-22 | 天津工业大学 | Method for quickly preparing large-area carbon nanometer tube flexible transparent conductive thin films and improving electric conductibility of thin films |
CN104021879A (en) * | 2013-09-18 | 2014-09-03 | 天津工业大学 | Preparation method for strong-adhesion-force carbon nanotube flexible transparent conductive thin film and adhesion force detection method |
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Application publication date: 20170922 |