CN107545958A - A kind of method and its device for reducing carbon-based conductive membrane volume resistivity - Google Patents
A kind of method and its device for reducing carbon-based conductive membrane volume resistivity Download PDFInfo
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- CN107545958A CN107545958A CN201710536492.XA CN201710536492A CN107545958A CN 107545958 A CN107545958 A CN 107545958A CN 201710536492 A CN201710536492 A CN 201710536492A CN 107545958 A CN107545958 A CN 107545958A
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Abstract
The invention discloses a kind of method and its device for reducing carbon-based conductive membrane volume resistivity, this method is to be higher than by applying to conducting film usually using that can produce the temperature higher than common operating temperature after voltage to carry out joule heat treatment to conducting film itself, and the specific insulation of carbon-based conductive film can be effectively reduced in the process.This method step is as follows：A) carbon-based conductive film is accessed into joule annealing device；b)：Applying stable voltage or changing voltage keeps stable joule heat treatment temperature to be handled；c)：Cool down conducting film.This method is related to a set of special energization joule annealing device, including adjustable voltage-stabilized power supply, wire, holding electrode, voltage and current detecting device and device for detecting temperature.Energization joule heat treatment method advantage compared with external heat transfer processing method is：Easily operated, convenient control, time-consuming short and positive effect, while expand the scope of application of heat treatment.
Description
Technical field
The present invention relates to a kind of processing method and its device of carbon-based conductive film, to reduce the volume of carbon-based conductive film electricity
Resistance rate.
Background technology
Carbon-based conductive film causes domestic and international researcher to carry out related research with its excellent performance at present, especially with
CNT and graphene have electrical conductivity height, light weight, good in optical property, pliability good for the carbon-based conductive film of conductive filler
Deng excellent properties, the fields such as antistatic, electromagnetic shielding, Electric radiant Heating Film, battery and ultracapacitor are widely used.
An important target is exactly to reduce its specific insulation, Yan et al. (Yan J, Y for carbon-based conductive film
G Jeong.Composites Science and Technology, 2015,106：134-140.) by changing conductive filler
Species, content or it is comprehensive using a variety of conductive fillers to reach the purpose of reduction specific insulation, the A of CN 103665908
Disclose a kind of by controlling CNT to form carbon nano tube bundle to realize the method for reducing specific insulation, Cristhian
Et al. (Garzon Cristhian, Palza Humberto.Composite Science and Technology, 2014,
99：Outer heat treatment 117-123.) is carried out to carbon-based conductive film to reduce the specific insulation of carbon-based conductive film.
The content of the invention
Heat is being produced after being applied in high voltage and then the characteristics of can be heat-treated to itself with reference to carbon-based conductive film,
The present invention is a kind of method and its device of new reduction carbon-based conductive membrane volume resistivity, i.e., carbon-based conductive film is powered
Joule heat treatment, while contain the device for implementing this method.This method has simple to operate, time-consuming short, positive effect, without dirt
The characteristics of dye, it is adapted to the advantages that scale is to carbon-based conductive film progress processing.
The technical scheme is that：
The method for reducing carbon-based conductive membrane volume resistivity is to carry out joule heat treatment to conducting film, i.e., is led to carbon-based
Electrolemma applies to be come to conducting film in itself beyond it usually using conducting film generation during voltage higher than the temperature of its usual operating temperature
Carry out the process of joule heat treatment.
Described apply routinely use voltage beyond it, and the voltage is 0.01~10000V, it is preferred that voltage for 5~
1000V。
The joule heat treatment temperature higher than the usual operating temperature of conducting film is 50~400 DEG C, it is preferred that at Joule heat
It is 70~180 DEG C to manage temperature.
The heat treatment of energization joule is carried out to carbon-based conductive film to comprise the following steps：A) carbon that energization joule will be needed to be heat-treated
Base conducting film accesses joule annealing device；b)：Power supply is connected, applies the voltage treatment temperature of determination in the temperature described in right 3
The voltage for fluctuating or keeping the joule heat treatment temperature of determination to be applied without disconnected adjustment in the range of degree, voltage is in right 2
In required voltage range；c)：Deenergization, cool down carbon-based conductive film.
C) deenergization described in step, carbon-based conductive film is cooled down, can quickly be cooled down for cooling velocity, it is natural
Cooling and Slow cooling.
The device for implementing energization joule heat treatment method is examined by adjustable voltage-stabilized power supply, wire, holding electrode, voltage x current
Survey device and device for detecting temperature composition.
Described adjustable voltage-stabilized power supply is D.C. regulated power supply or alternating current steady voltage plug.
Described holding electrode is that electrode is bonded on the inside of clip, clip is clipped on conducting film can be achieved conducting film and
The good contact of electrode.
Device for detecting temperature in described joule annealing device is contact temperature monitoring device, such as thermocouple and its
Display device, or non-contact temperature monitoring device, such as infrared thermoviewer.
Compared with the existing progress external heat transfer processing to carbon-based conductive film, the present invention has the following advantages：
(1) joule heat treatment method can make conducting film volume resistance compared with general outer heat under same treatment temperature
Rate reduces more, i.e., treatment effect is more notable.
(2) general outer heat treatment method is by heat transfer from outside to inside, treatment temperature heterogeneity, causes to produce inside conducting film
Raw stress, influence the mechanical performance of conducting film；Joule heat treatment method is due to being conducting film itself heat production, so to conducting film
Processing is more homogeneous, it is possible to prevente effectively from above mentioned problem.
(3) annealing device needed for the present invention is very simple, and easy to operate, processing procedure is easily controlled, and takes short, volume
Resistivity reduces obvious, processing procedure efficiency high；And be heat-treated needs firing equipment outside, heat treatment efficiency is relatively low.
(4) present invention can be heat-treated to the carbon-based conductive film of outdoor fixed object surface, such as petroleum pipeline；To multiple
Miscellaneous large scale industry equipment surfaces carbon-based conductive film carries out thermal anneal process, and this is externally heat-treated and is difficult to, you can
With the scope of application of extension heat treatment.
Brief description of the drawings
In order that technical scheme and beneficial effect are clearer, the present invention provides the one of accompanying drawing constitution instruction
Part, the present invention is explained together with embodiments of the present invention, is not construed as limiting the invention, accompanying drawing is said as follows
It is bright：
Fig. 1 energization joule annealing device schematic diagrames；
In energization Joule heat, specific insulation changes graphene/epoxy resin conducting film before and after the processing in Fig. 2 embodiments 1
Figure；
Joule heat treatment and general outer heat treatment when Fig. 3 identicals treatment temperature (130 DEG C) and processing time (30 minutes)
The comparison diagram of conducting film specific insulation afterwards
Surface SEM comparison diagram of the graphene/epoxy resin conducting film in energization Joule heat before and after the processing in Fig. 4 embodiments 1
(a：Before processing, b：After processing)；
Multi-walled carbon nanotube/epoxy resin conducting film is in energization Joule heat specific insulation before and after the processing in Fig. 5 embodiments 2
Variation diagram；
Carbon black/epoxy resin conducting film is in energization Joule heat specific insulation variation diagram before and after the processing in Fig. 6 embodiments 3；
Graphene/polyurethane guide electrolemma is in energization Joule heat specific insulation variation diagram before and after the processing in Fig. 7 embodiments 4；
In energization Joule heat, specific insulation becomes multi-walled carbon nanotube/polyurethane guide electrolemma before and after the processing in Fig. 8 embodiments 5
Change figure；
Carbon Black/polyurethane conducting film is in energization Joule heat specific insulation variation diagram before and after the processing in Fig. 9 embodiments 6；
In figure, 1- can adjust voltage-stabilized power supply, and 2- Acquisition Instruments gather electric current wire, 3- data collecting instruments, and 4- Acquisition Instruments are adopted
Collecting voltage wire, 5- holding electrodes, 6- carbon-based conductive films, 7- thermocouples.
Embodiment
Embodiments of the invention are not considered as limiting the invention, only several preferred embodiments, protection domain
Still it is defined by the content disclosed in claims.
Energization joule heat-treating methods are as follows：By carbon-based conductive film folder between the electrodes, electrode and carbon-based conductive film it
Between apply conductive silver paste, burning voltage joule heat treatment is carried out to carbon-based conductive film, the voltage of application is 5~1000V, or stably
The joule heat treatment of temperature, the heating temp of carbon-based conductive film is controlled by constantly adjusting the size of application magnitude of voltage, is entered
The temperature of row joule heat treatment is 70~180 DEG C；Deenergization, carbon-based conductive film is cooled down, can be carried out quickly for cooling velocity
Cooling, natural cooling and Slow cooling.
Energization joule annealing device of the present invention, the device include：Adjustable voltage-stabilized power supply, wire, clamping
Electrode, voltage and current detecting device and device for detecting temperature composition；Adjustable voltage-stabilized power supply is D.C. regulated power supply or exchange
Voltage-stabilized power supply, holding electrode are that electrode is bonded on the inside of clip, clip are clipped on conducting film conducting film and electrode can be achieved
Good contact；Device for detecting temperature is contact temperature monitoring device, such as thermocouple and its display device, or it is contactless
Device for detecting temperature, such as infrared thermoviewer.
For clearer explanation technical scheme, it is described in further detail with reference to embodiment and accompanying drawing.
Embodiment 1
Energization joule heat treatment is carried out to graphene/epoxy resin conducting film, graphene content is 15wt% in conducting film,
Conducting film test sample size is 1 centimetre of 2 cm x, and it is 110 Ω cm to test the sample treatment front volume resistivity, with clamping electricity
Pole accesses conducting film in energization joule annealing device, switches on power, and applies voltage 85V and reaches 130 DEG C, starts at Joule heat
Reason, according to the temperature feedback of device for detecting temperature, by adjustable voltage-stabilized power supply constantly adjust voltage keep its temperature 130 ±
2 DEG C, the voltage being applied on conducting film is defined by data collecting instrument display data, 30 minutes processing times, last required application
Voltage is 77V, deenergization, naturally cools to room temperature (25 ± 2 DEG C), and test sample specific insulation is 24.1 Ω cm, is reduced
78.1%.
Embodiment 2
Carry out energization joule heat treatment to multi-walled carbon nanotube/epoxy resin conducting film, content of carbon nanotubes in conducting film
For 35wt%, conducting film test sample size is 2 centimetres of 2 cm x, and it is 14.44 Ω to test the sample treatment front volume resistivity
Cm, conducting film is accessed in energization joule annealing device, 100 DEG C, the energization joule heat treatment of 10 minutes are carried out to it, is applied
Voltage constantly adjusts from 79V and is reduced to 70V, to keep its temperature control deenergization, to naturally cool to room temperature at 120 ± 2 DEG C
(25 ± 2 DEG C), test sample specific insulation are 3.28 Ω cm, reduce 77.3%.
Embodiment 3
Energization joule heat treatment is carried out to carbon black/epoxy resin conducting film, content of carbon black is 45wt% in conducting film, conductive
Film test sample size is 2 centimetres of 2 cm x, and it is 2.13 Ω cm to test the sample treatment front volume resistivity, and conducting film is connect
Enter to be powered in joule annealing device, 120 DEG C, the energization joule heat treatment of 10 minutes are carried out to it, it is continuous from 70V to apply voltage
Adjustment is reduced to 66V, to keep its temperature control deenergization, to naturally cool to room temperature (25 ± 2 DEG C) at 120 ± 2 DEG C, surveys
Test agent specific insulation is 1.64 Ω cm, reduces 23.2%.
Embodiment 4
Energization joule heat treatment is carried out to graphene/polyurethane guide electrolemma, graphene content is 15wt% in conducting film, is led
Electrolemma test sample size is 2 centimetres of 2 cm x, and it is 1.95 Ω cm to test the sample treatment front volume resistivity, by conducting film
Access in energization joule annealing device, 90 DEG C, the heat treatment of the energization joule of 10 minutes are carried out to it, apply voltage from 29V not
Disconnected adjustment is reduced to 28V, to keep its temperature control deenergization, to naturally cool to room temperature (25 ± 2 DEG C) at 90 ± 2 DEG C, surveys
Test agent specific insulation is 1.73 Ω cm, reduces 11.4%.
Embodiment 5
Energization joule heat treatment is carried out to multi-walled carbon nanotube/polyurethane guide electrolemma, content of carbon nanotubes is in conducting film
15wt%, conducting film test sample size are 2 centimetres of 2 cm x, and it is 30.94 Ω to test the sample treatment front volume resistivity
Cm, conducting film is accessed in energization joule annealing device, 90 DEG C are carried out to it, the energization joule heat treatment of 10 minutes, is applied
Voltage constantly adjusts from 130V and is reduced to 122V, to keep its temperature control deenergization, to naturally cool to room at 90 ± 2 DEG C
Warm (25 ± 2 DEG C), test sample specific insulation is 22.03 Ω cm, reduces 28.8%.
Embodiment 6
Energization joule heat treatment is carried out to Carbon Black/polyurethane conducting film, graphene content is 45wt% in conducting film, conductive
Film test sample size is 2 centimetres of 2 cm x, and it is 0.85 Ω cm to test the sample treatment front volume resistivity, and conducting film is connect
Enter to be powered in joule annealing device, 90 DEG C, the energization joule heat treatment of 10 minutes are carried out to it, it is continuous from 45V to apply voltage
Adjustment is reduced to 43V, to keep its temperature control deenergization, to naturally cool to room temperature (25 ± 2 DEG C) at 90 ± 2 DEG C, test
Sample volume resistivity is 0.8 Ω cm, reduces 5.3%.
Claims (9)
- A kind of 1. method for reducing carbon-based conductive membrane volume resistivity, it is characterised in that：The reduction carbon-based conductive membrane volume electricity The method of resistance rate is to carry out joule heat treatment to conducting film, i.e., carbon-based conductive film is applied beyond it usually using conductive during voltage Film produces the temperature higher than its usual operating temperature to carry out the process of joule heat treatment in itself to conducting film.
- A kind of 2. processing unit for reducing carbon-based conductive membrane volume resistivity, it is characterised in that：The device is to implement claim 1 The corresponding intrument of described energization joule heat treatment method, device is by adjustable voltage-stabilized power supply, wire, holding electrode, voltage electricity Flow detection device and device for detecting temperature composition.
- A kind of 3. method for reducing carbon-based conductive membrane volume resistivity according to claim 1, it is characterised in that：The application Voltage routinely is used beyond it, the voltage is 0.01~10000V, it is preferred that voltage is 5~1000V.
- A kind of 4. method for reducing carbon-based conductive membrane volume resistivity according to claim 1, it is characterised in that：It is described to be higher than The joule heat treatment temperature of the usual operating temperature of conducting film is 50~400 DEG C, it is preferred that joule heat treatment temperature is 70~180 ℃。
- A kind of 5. method for reducing carbon-based conductive membrane volume resistivity according to claim 1, it is characterised in that：Led to carbon-based Electrolemma carries out the heat treatment of energization joule and comprised the following steps：A) the carbon-based conductive film for needing energization joule to be heat-treated is accessed into joule Annealing device；b)：Power supply is connected, the voltage treatment temperature for applying determination fluctuates within the scope of the temperature described in claim 3 Or the voltage that the joule heat treatment temperature for keeping determining is applied without disconnected adjustment, voltage is required by claim 2 In voltage range；c)：Deenergization, cool down carbon-based conductive film.
- A kind of 6. method for reducing carbon-based conductive membrane volume resistivity according to claim 5, it is characterised in that：Led to carbon-based Electrolemma carries out the deenergization described in the step c) that the heat treatment of energization joule includes, and cools down carbon-based conductive film, for cooling speed Degree can be cooled down quickly, natural cooling and Slow cooling.
- A kind of 7. processing unit for reducing carbon-based conductive membrane volume resistivity according to claim 2, it is characterised in that：It is described Adjustable voltage-stabilized power supply be D.C. regulated power supply or alternating current steady voltage plug.
- A kind of 8. processing unit for reducing carbon-based conductive membrane volume resistivity according to claim 2, it is characterised in that：It is described Holding electrode be that electrode is bonded on the inside of clip, clip is clipped in well connecing for conducting film and electrode can be achieved on conducting film Touch.
- A kind of 9. processing unit for reducing carbon-based conductive membrane volume resistivity according to claim 2, it is characterised in that：It is described Joule annealing device in device for detecting temperature be contact temperature monitoring device, such as thermocouple and its display device, or Person's non-contact temperature monitoring device, such as infrared thermoviewer.
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| CN2016104803200 | 2016-06-28 | ||
| CN201610480320 | 2016-06-28 |
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Cited By (3)
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| CN112291868A (en) * | 2020-09-14 | 2021-01-29 | 兰州大学 | Self-annealing graphene self-supporting high-temperature electrothermal film and preparation method thereof |
| CN115160866A (en) * | 2022-05-11 | 2022-10-11 | 北京邮电大学 | Method for preparing surface modified electromagnetic shielding material by joule heat treatment |
| CN115161737A (en) * | 2022-05-11 | 2022-10-11 | 北京邮电大学 | Method for preparing electromagnetic shielding material for copper electrodeposition on surface of flexible substrate |
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| CN103052682A (en) * | 2010-08-06 | 2013-04-17 | 日立化成工业株式会社 | Liquid composition, and resistor film, resistor element and circuit board using same |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112291868A (en) * | 2020-09-14 | 2021-01-29 | 兰州大学 | Self-annealing graphene self-supporting high-temperature electrothermal film and preparation method thereof |
| CN112291868B (en) * | 2020-09-14 | 2021-12-14 | 兰州大学 | Self-annealing graphene self-supporting high-temperature electrothermal film and preparation method thereof |
| CN115160866A (en) * | 2022-05-11 | 2022-10-11 | 北京邮电大学 | Method for preparing surface modified electromagnetic shielding material by joule heat treatment |
| CN115161737A (en) * | 2022-05-11 | 2022-10-11 | 北京邮电大学 | Method for preparing electromagnetic shielding material for copper electrodeposition on surface of flexible substrate |
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Application publication date: 20180105 |