CN109402826B - A kind of flexible electromagnetic shielding material, preparation method and applications - Google Patents
A kind of flexible electromagnetic shielding material, preparation method and applications Download PDFInfo
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- CN109402826B CN109402826B CN201811098678.2A CN201811098678A CN109402826B CN 109402826 B CN109402826 B CN 109402826B CN 201811098678 A CN201811098678 A CN 201811098678A CN 109402826 B CN109402826 B CN 109402826B
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- carbon fiber
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- electromagnetic shielding
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
- D02J13/00—Heating or cooling the yarn, thread, cord, rope, or the like, not specific to any one of the processes provided for in this subclass
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06C—FINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
- D06C7/00—Heating or cooling textile fabrics
Abstract
The invention discloses a kind of flexible electromagnetic shielding materials, preparation method and applications, including flexible carbon fiber is prepared under oxygen-free atmosphere through high-temperature process；The temperature of the high temperature is 1200~1600 DEG C.Using flexible carbon fiber as raw material, through 1200~1600 DEG C of argon atmosphere heat treatment in tube furnace, regulate and control carbon ordering degree, optimize electromagnetic shielding performance of the active carbon fiber felt in 8.2~12.4GHz frequency range, after heat treatment active carbon fiber felt shielding properties reaches 32dB-38dB, improves about 110% than original activity carbon fiber felt.Method therefor of the present invention is simple, effective, can be used for preparing flexibility, lightweight, extraordinary electro-magnetic screen function material resistant to high temperature.
Description
Technical field
The invention belongs to carbon-based electromagnetic functional material technical field, in particular to a kind of flexible electromagnetic shielding material, preparation
Method and its application.
Technical background
The electromagnetic radiation that the electronic devices such as computer, telecommunication technology generate, not only threatens human physical and mental health, and
And the normal work of sophisticated electronics is influenced, have become a kind of one of internationally recognized important pollution sources.Inhibit electromagnetism spoke
The main means for penetrating pollution are using electromagnetic shielding material.Currently used electromagnetic shielding material be mainly conductive metal, carbon or
Metallic conductor filled polymer based composites, density metal is larger and perishable, and polymer matrix composites are dfficult to apply to
Hot environment.Carbon material has the characteristics that density is low, conducting electricity very well is suitable as high-temperature electromagnetic shielding material application.Activated carbon
Fibrofelt has many advantages, such as that flexible, yield is big, at low cost, Residual carbon is high, is common carbon material precursor, but active carbon fiber
Carbon in dimension felt belongs to agraphitic carbon, there is a problem of that degree of graphitization is low, conductivity is low.
Summary of the invention
For overcome the deficiencies in the prior art, carbon-based electromagnetic shielding material is developed, and improves the electromagnetism of active carbon fiber felt
Shielding properties, the invention proposes a kind of flexible electromagnetic shielding materials, preparation method and applications.
Technical solution is as follows:
A kind of preparation method of flexible electromagnetic shielding material, including by flexible carbon fiber under oxygen-free atmosphere through high-temperature process
It is prepared；
The temperature of the high temperature is 1200~1600 DEG C.
Optionally, the oxygen-free atmosphere is inert gas atmosphere, and the pressure of inert gas atmosphere is 0.1MPa.
Optionally, the flexible carbon fiber be carbon fiber or activated carbon fiber be compiled into longitude and latitude interlock net, cloth, plate, felt,
The flexible article formed after chip architecture.
Optionally, the flexible carbon fiber is selected from carbon fiber felt, carbon cloth, carbon fiber sheet, carbon fiber board, carbon fiber
One of net, active carbon fiber felt, activated carbon fiber cloth, activated carbon fiber piece, activated carbon fiber plate and absorbent carbon fibrous reticulum.
Optionally, the density of the flexible carbon fiber is 7.08 × 10-2g/cm3, carbon fiber is straight in flexible carbon fiber
4~6 μm of diameter, resistivity 2.9042 × 10-5Ωm。
Optionally, by flexible carbon fiber under oxygen-free atmosphere through high-temperature process before also by pretreatment, the pretreatment
Including successively through acetone and washes of absolute alcohol or obtained by drying.
Optionally, the high-temperature process carries out in tube furnace, and detailed process includes:
Heating: for the air in extraction tube furnace to 5kPa hereinafter, being passed through argon gas, flow 50ml/min keeps furnace pressure flat
Weighing apparatus is to 0.1MPa, and after 30min, 0~300 DEG C of speed with 4 DEG C/min heats up, and 300~800 DEG C of speed with 5 DEG C/min heats up,
It is heated up after 800 DEG C with the speed of 3 DEG C/min, is warming up to high-temperature process temperature, keep the temperature 2h；
Cooling:, being cooled down with the speed of 3 DEG C/min by 900 DEG C or more, and 900~300 DEG C of speed with 5 DEG C/min cools down, and 300
DEG C hereinafter, being down to room temperature with furnace.
A kind of flexible electromagnetic shielding material, the flexible electromagnetic shielding material are prepared into using method of the present invention
It arrives.
Flexible electromagnetic shielding material is used for the application of electronic instrument electromagnetic protection.
Application of the flexible electromagnetic shielding material for precision electronic device electromagnetic protection in hot environment.
Activated carbon fiber prepared by the present invention with electro-magnetic screen function has the advantage that
(1) active carbon fiber felt has many advantages, such as flexibility, lightweight, high temperature resistant as electro-magnetic screen function material.
(2) method that the present invention uses can obviously improve the electromagnetic shielding performance of active carbon fiber felt, (i.e. relative to raw material
Untreated active carbon fiber felt), electromagnet shield effect can be improved 110% or more, and simple process, economy, be easy to control.
Detailed description of the invention
Fig. 1 is tubular type furnace apparatus figure of the invention；
Fig. 2 is the SEM figure of sample prepared by the embodiment of the present invention 1,2,3,4,5,6.
Fig. 3 is the Raman figure of sample prepared by the embodiment of the present invention 1,2,3,4,5,6；
Fig. 4 is the electromagnet shield effect figure of sample prepared by the embodiment of the present invention 1,2,3,4,5,6；
Fig. 5 is to be heat-treated the place to active carbon fiber felt using carbon burial sintering method and tube furnace for 1400 DEG C in comparative example
Manage effect photo；
Fig. 6 is to be heat-treated the place to active carbon fiber felt using carbon burial sintering method and tube furnace for 1500 DEG C in comparative example
Manage effect photo；
Below in conjunction with drawings and examples, the present invention is described in further detail.
Specific embodiment
The flexible carbon fiber that the present invention mentions includes: carbon fiber or activated carbon fiber be compiled into longitude and latitude interlock net, cloth, plate,
The flexible article formed after felt, chip architecture.Can be selected from carbon fiber felt, carbon cloth, carbon fiber sheet, carbon fiber board, carbon fibre web,
One of active carbon fiber felt, activated carbon fiber cloth, activated carbon fiber piece, activated carbon fiber plate and absorbent carbon fibrous reticulum.
Flexible electromagnetic shielding material and its performance improvement method of the invention, detailed process are as follows: be with active carbon fiber felt
Raw material is prepared into the block materials of 40mm × 40mm, after argon gas be protective atmosphere tube furnace in be heat-treated, utilize height
Warm environment improves the crystallinity of carbon in active carbon fiber felt.
Specifically, active carbon fiber felt density is 7.08 × 10-2g/cm3, the block materials of 40mm × 40mm are prepared into, it is right
Active carbon fiber felt is pre-processed, and is impregnated with acetone, after be placed in dehydrated alcohol, clean 2 times repeatedly with ultrasonic wave, often
Secondary 15min.Then, it is put into baking oven, 60 DEG C, 5h, is dried.The heat treatment of tube furnace high temperature, 1200~1600 DEG C for the treatment of temperature.
Further, the heat treatment process parameter: protective gas is argon gas, and flow 50ml/min adjusts air outlet valve, makes
Furnace pressure is balanced to 0.1MPa, and after 30min, 0~300 DEG C of speed with 4 DEG C/min heats up, and 300~800 DEG C with 5 DEG C/min
Speed heating, heated up after 800 DEG C with the speed of 3 DEG C/min, be warming up to 1200,1300,1400,1500,1600 DEG C respectively,
2 hours are kept the temperature respectively, 900 DEG C or more, is cooled down with the speed of 3 DEG C/min, 900~300 DEG C of speed with 5 DEG C/min cools down, and 300
DEG C hereinafter, being down to room temperature with furnace.
Flexible electromagnetic shielding block materials are prepared using active carbon fiber felt, with easily molded, required equipment is simple, technique
The advantages that process is simple, process flow is short, and the degree of order of carbon can be improved by carbonization treatment, and keep activated carbon fiber
The flexibility of felt, as shown in SEM in Fig. 2.Flexible electromagnetic shielding material produced by the present invention is in hot environment (400~800
DEG C) application of precision electronic device electromagnetic protection.
It is the embodiment that inventor provides below, the present invention is not limited to embodiments below, in the range that the present invention provides
It is interior, it can prepare the preferable carbonaceous block of electromagnetic shielding performance.
Embodiment 1:
The present embodiment uses density for 7.08 × 10-2g/cm3, it is prepared into the active carbon fiber felt block material of 40mm × 40mm
Material.Raman analysis has been carried out to active carbon fiber felt block materials according to test request, raw material sample during the results are shown in attached figure 3, meter
It calculates it can be concluded that ID/IG=1.768034.Its resistivity is 2.9042 × 10-5Ωm.Using rectangular wave inducing defecation by enema and suppository in vector network point
Analyse the scattering parameter S on platform in test sample 8.2~12.4GHz frequency range11、S12、S21、S22, its screen is calculated according to formula
Cover efficiency, shield effectiveness value SETBetween 14.5~17dB, as shown in raw material in attached drawing 4.
Embodiment 2:
In conjunction with Fig. 1, the present embodiment uses density for 7.08 × 10-2g/cm3, it is prepared into the activated carbon fiber of 40mm × 40mm
Felt block materials.
Pretreatment: pretreatment includes by carbon fiber felt block materials successively through acetone and washes of absolute alcohol, obtained by drying.
The structure of the tube furnace of high-temperature process used is shown in Fig. 1, including alundum tube, corundum Noah's ark, places in corundum Noah's ark
The active carbon fiber felt pre-processed is passed through argon gas in alundum tube and is protected；
It is heat-treated in the tube furnace that argon gas is protective atmosphere, heat treatment process parameter: protective gas is argon gas, stream
50ml/min is measured, air outlet valve is adjusted, balances furnace pressure to 0.1MPa, after 30min, 0~300 DEG C of speed with 4 DEG C/min
Heating, 300~800 DEG C of speed with 5 DEG C/min are heated up, are heated up after 800 DEG C with the speed of 3 DEG C/min, be warming up to respectively
1200 DEG C, 2 hours are kept the temperature respectively, 900 DEG C or more, is cooled down with the speed of 3 DEG C/min, 900~300 DEG C of speed with 5 DEG C/min
Cooling, 300 DEG C hereinafter, be down to room temperature with furnace.
According to test request to blocky sample sample preparation obtained, Raman analysis is carried out, 1200 DEG C of examinations during the results are shown in attached figure 3
Sample calculates it can be concluded that ID/IG=1.619025.Its resistivity is 5.559 × 10-6Ωm.Using rectangular wave inducing defecation by enema and suppository in vector net
Scattering parameter S on network analysis platform in 8.2~12.4GHz of test sample frequency range11、S12、S21、S22, calculated according to formula
Its shield effectiveness, shield effectiveness value SETBetween 34.5~36dB, as shown in 1200 DEG C in attached drawing 4.
Embodiment 3:
As different from Example 2, tubular type furnace temperature rises to 1300 DEG C to the present embodiment, other technological parameters and embodiment 2
It is all the same.1300 DEG C of samples during the results are shown in attached figure 3 calculate it can be concluded that ID/IG=1.674774.Its resistivity be 6.026 ×
10-6Ωm.Using scattering of the rectangular wave inducing defecation by enema and suppository on vector network analysis platform in 8.2~12.4GHz of test sample frequency range
Parameter S11、S12、S21、S22, its shield effectiveness, shield effectiveness value SE are calculated according to formulaTIt is such as attached between 31.4~32.4dB
In Fig. 4 shown in 1300 DEG C.
Embodiment 4:
As different from Example 2, tubular type furnace temperature rises to 1400 DEG C to the present embodiment, other technological parameters and embodiment 2
It is all the same.1400 DEG C of samples during the results are shown in attached figure 3 calculate it can be concluded that ID/IG=1.470894.Its resistivity be 3.889 ×
10-6Ωm.Using scattering of the rectangular wave inducing defecation by enema and suppository on vector network analysis platform in 8.2~12.4GHz of test sample frequency range
Parameter S11、S12、S21、S22, its shield effectiveness, shield effectiveness value SE are calculated according to formulaTBetween 38~39dB, in attached drawing 4
Shown in 1400 DEG C.
Embodiment 5:
As different from Example 2, tubular type furnace temperature rises to 1500 DEG C to the present embodiment, other technological parameters and embodiment 2
It is all the same.1500 DEG C of samples during the results are shown in attached figure 3 calculate it can be concluded that ID/IG=1.615861.Its resistivity be 2.306 ×
10-6Ωm.Using scattering of the rectangular wave inducing defecation by enema and suppository on vector network analysis platform in test sample 8.2-12.4GHz frequency range
Parameter S11、S12、S21、S22, its shield effectiveness, shield effectiveness value SE are calculated according to formulaTIt is such as attached between 37.5~39.5dB
In Fig. 4 shown in 1500 DEG C.
Embodiment 6:
As different from Example 2, tubular type furnace temperature rises to 1600 DEG C to the present embodiment, other technological parameters and embodiment 2
It is all the same.1600 DEG C of samples during the results are shown in attached figure 3 calculate it can be concluded that ID/IG=1.82892.Its resistivity is 3.838 × 10-6Ωm.Using scattering ginseng of the rectangular wave inducing defecation by enema and suppository on vector network analysis platform in 8.2~12.4GHz of test sample frequency range
Number S11、S12、S21、S22, its shield effectiveness, shield effectiveness value SE are calculated according to formulaTBetween 35.8~37.6dB, such as attached drawing 4
In shown in 1600 DEG C.
In summary experimental result, from Fig. 2, it can be seen that as the temperature rises, the active carbon fiber after heat treatment
The flexibility for tieing up felt is constant, and wherein the diameter of carbon fiber does not change.Fig. 3 explanation, with the rising of temperature, ID/IGRatio it is opposite
All reducing in the raw material of active carbon fiber felt, ID/IGRatio it is smaller, the crystallization degree of carbon is higher.To electromagnet shield effect
Positive interaction it is better.In Fig. 4, SETFor electromagnet shield effect, SEATo absorb efficiency, SERFor reflection performance, SET=SER+SEA,
It is not that temperature gets over Gao Yue by the result of Fig. 4 it is found that shielding properties and heat treatment temperature directly have uncertain correlation
Good, under 1400~1500 DEG C of heat treatment temperature, shield effectiveness is best.
In order to compare at the tube oven method heat treatment and the difference of other heat treatment methods that the present invention uses, compared
1400 DEG C and 1500 DEG C are heat-treated the treatment effect to active carbon fiber felt using carbon burial sintering method:
Comparative example one:
The heat treatment of same active carbon fiber felt is carried out using carbon burial sintering method, density is 7.08 × 10-2g/cm3, preparation
At the active carbon fiber felt block materials of 40mm × 40mm；
The active fiber C felt prepared is put in diameter 50mm, in the graphite crucible with cover of high 50mm, then uses scale stone
Ink, which is buried, to be placed in corundum crucible with cover.Then 1400 DEG C, 1500 DEG C of guarantors are warming up to respectively with high temperature box type resistance furnace
Temperature 2 hours.Temperature increasing schedule is as follows: 800 DEG C hereinafter, the speed of 5 DEG C/min heats up；800 DEG C -1200 DEG C, with the speed of 4 DEG C/min
Heating；1200 DEG C or more, the speed heating of 3 DEG C/min.2 hours are kept the temperature to 1400 DEG C, 1500 DEG C.Cooling system is natural cooling
Cooling.It is cooled to room temperature, takes out style.
Fig. 5 and Fig. 6 is carbon burial sintering and tube furnace style comparison diagram: as seen from the figure, the work that carbon burial sintering is prepared
Property carbon fiber felt, do not have the flexibility of active carbon fiber felt, and an active carbon fiber felt of tube furnace sintering, also keep original good
Good flexibility.
Claims (6)
1. a kind of preparation method of flexible electromagnetic shielding material, which is characterized in that including by flexible carbon fiber under oxygen-free atmosphere
It is prepared through high-temperature process；
The temperature of the high temperature is 1400~1500 DEG C；
The density of the flexible carbon fiber is 7.08 × 10-2g/cm3, 4~6 μm of diameter of carbon fiber in flexible carbon fiber, electricity
Resistance rate 2.9042 × 10-5Ωm；
The high-temperature process carries out in tube furnace, and detailed process includes:
Heating: the air in extraction tube furnace is to 5kPa hereinafter, be passed through argon gas, flow 50ml/min, make furnace pressure balance to
After 0.1MPa, 30min, 0~300 DEG C of speed with 4 DEG C/min heats up, and 300~800 DEG C of speed with 5 DEG C/min heats up, and 800
It is heated up after DEG C with the speed of 3 DEG C/min, is warming up to high-temperature process temperature, keep the temperature 2h；
Cooling:, being cooled down with the speed of 3 DEG C/min by 900 DEG C or more, and 900~300 DEG C of speed with 5 DEG C/min cools down, 300 DEG C with
Under, room temperature is down to furnace.
2. the preparation method of flexible electromagnetic shielding material according to claim 1, which is characterized in that the flexible carbon fiber
Dimension is that carbon fiber or activated carbon fiber are compiled into longitude and latitude and interlock the flexible article formed after net, cloth or hardened structure.
3. the preparation method of flexible electromagnetic shielding material according to claim 1, which is characterized in that flexible carbon fiber exists
Under oxygen-free atmosphere through before high-temperature process also by pre-processing, the pretreatment include successively through acetone and washes of absolute alcohol or
It is obtained by drying.
4. a kind of flexible electromagnetic shielding material, which is characterized in that the flexible electromagnetic shielding material is appointed using claim 1-3
Method described in one claim is prepared.
5. the application that flexible electromagnetic shielding material as claimed in claim 4 is used for electronic instrument electromagnetic protection.
6. flexible electromagnetic shielding material as claimed in claim 4 is answered for precision electronic device electromagnetic protection in hot environment
With.
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| CN101188927A (en) * | 2007-12-10 | 2008-05-28 | 盛虹集团有限公司 | Electromagnetic shielding fabric for carbon fiber |
| CN101583747A (en) * | 2007-01-09 | 2009-11-18 | 新日本特克斯株式会社 | Method for production of carbonized cloth, and carbonized cloth produced by the method |
| CN102465459A (en) * | 2010-11-16 | 2012-05-23 | 大连兆阳软件科技有限公司 | Novel weaving method of carbon fiber electromagnetic shielding textile fabric |
| CN104047071A (en) * | 2014-07-07 | 2014-09-17 | 扬州大学 | Preparation method for magnetic active carbon fibers |
| CN105421036A (en) * | 2015-12-23 | 2016-03-23 | 北京航空航天大学 | Graphene modification method for high-temperature composite material, the high-temperature composite material and preparation method |
| CN107541996A (en) * | 2016-06-25 | 2018-01-05 | 董晓 | A kind of preparation method of modified carbon nano-tube electromagnetic shielding paper |
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- 2018-09-20 CN CN201811098678.2A patent/CN109402826B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101583747A (en) * | 2007-01-09 | 2009-11-18 | 新日本特克斯株式会社 | Method for production of carbonized cloth, and carbonized cloth produced by the method |
| CN101188927A (en) * | 2007-12-10 | 2008-05-28 | 盛虹集团有限公司 | Electromagnetic shielding fabric for carbon fiber |
| CN102465459A (en) * | 2010-11-16 | 2012-05-23 | 大连兆阳软件科技有限公司 | Novel weaving method of carbon fiber electromagnetic shielding textile fabric |
| CN104047071A (en) * | 2014-07-07 | 2014-09-17 | 扬州大学 | Preparation method for magnetic active carbon fibers |
| CN105421036A (en) * | 2015-12-23 | 2016-03-23 | 北京航空航天大学 | Graphene modification method for high-temperature composite material, the high-temperature composite material and preparation method |
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