CN110258106A - A kind of preparation method of the sandwich-type flexible electromagnetic shielding material based on carbon fibre fabric, metallic nickel nano granule and graphene - Google Patents
A kind of preparation method of the sandwich-type flexible electromagnetic shielding material based on carbon fibre fabric, metallic nickel nano granule and graphene Download PDFInfo
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- CN110258106A CN110258106A CN201910657184.1A CN201910657184A CN110258106A CN 110258106 A CN110258106 A CN 110258106A CN 201910657184 A CN201910657184 A CN 201910657184A CN 110258106 A CN110258106 A CN 110258106A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
- H05K9/009—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive fibres, e.g. metal fibres, carbon fibres, metallised textile fibres, electro-conductive mesh, woven, non-woven mat, fleece, cross-linked
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
Abstract
A kind of preparation method of the sandwich-type flexible electromagnetic shielding material based on carbon fibre fabric, metallic nickel nano granule and graphene, it is related to the preparation method of electromagnetic shielding material.The traditional preparation methods that the present invention solves existing electromagnetic shielding composite material " mixing-molding " influence the pliability of composite material, and it is related to the chemical reagent of some non-environmental protections, the problem of being difficult to accurately control the distribution of active constituent and construct specific microscopic appearance simultaneously, and then shielding properties is caused to be difficult to improve.Preparation method: one, carbon fibre fabric is prepared；Two, magnetron sputtering prepares metallic nickel nano granule/carbon fabric composite material；Three, plasma enhanced chemical vapor deposition.The present invention is used for the preparation of electromagnetic shielding material.
Description
Technical field
The present invention relates to the preparation methods of electromagnetic shielding material.
Background technique
In recent years, radio-frequency apparatus produces large-scale electromagnetic pollution in being widely used for the numerous areas such as communication, medical treatment,
This not only disturbs the normal operation of precision equipment, also causes grave danger to the health of the mankind.Therefore, develop ring
Guarantor, lightweight, high performance Combined Electromagnetic Shielding Materials have significant research significance.The active constituent of electromagnetic shielding material can be with
Three classes are roughly classified into, i.e. magnetic material (such as: carbonyl iron, ferriferous oxide), dielectric material (such as: carbon material) and conduction is poly-
It closes object (such as: polypyrrole, polyaniline).So far, carbon material is due to high conductivity, strong anti-oxidation, high heat stability
The advantages such as property, lightweight nature, are widely applied in electromagnetic shielding field.Wherein, graphene is as a kind of new carbon,
Obtained when due to high-specific surface area, wide aspect ratio and high conductivity, being advantageously used as electromagnetic shielding material high polarization amount and
Polarization loss.In addition, compared with the electromagnetic shielding materials such as metal or polymer, grapheme material usually have it is good it is flexible,
Significantly lower density and excellent machinability, can satisfy the need of the electro-magnetic screen layer as current portable electronic equipment
It asks.Due to the higher cost of graphene, in order to preferably utilize graphene in electromagnetic shielding field, by graphene and matrix material
Expecting the mode of doping, obviously than directly preparing graphene amount used in the mode of one pack system graphene product, less (i.e. cost is more
It is low), and preparation method is more flexible.In the preparation method of graphene-based electromagnetic shielding composite material, " mixing-molding " is one
Graphene isoreactivity material, i.e., be mixed into polymer substrate by kind simple and very common method, then again via polymerization,
The processing such as molding.However, this method usually will affect the pliability of composite material and be related to the chemistry examination of some non-environmental protections
Agent, while many polymer substrates (such as: polyvinylidene fluoride, epoxy resin, polyvinyl alcohol) used in this method
It is insulation, i.e., does not have significant responsiveness in electromagnetic field.In addition, be difficult to accurately control in this way activity at
Point distribution and construct specific microscopic appearance, and this two o'clock be proved to for electromagnetic shielding performance have important shadow
It rings.
Summary of the invention
The invention solves the traditional preparation methods of existing electromagnetic shielding composite material " mixing-molding " to influence composite material
Pliability, and be related to the chemical reagent of some non-environmental protections, while being difficult to accurately control the distribution of active constituent and constructing spy
Fixed microscopic appearance, and then the problem of cause shielding properties to be difficult to improve, and provide and a kind of received based on carbon fibre fabric, metallic nickel
The preparation method of the sandwich-type flexible electromagnetic shielding material of rice grain and graphene.
A kind of system of the sandwich-type flexible electromagnetic shielding material based on carbon fibre fabric, metallic nickel nano granule and graphene
Preparation Method, it is carried out according to the following steps:
One, carbon fibre fabric is prepared:
Container equipped with biomass fiber fabric is placed in high temperature pyrolysis device, is passed through inertia into high temperature pyrolysis device
Gas 1min~60min, under the protection of inert gas, with heating rate for 0.1 DEG C/min~10 DEG C/min, by high temperature pyrolysis
The temperature of device rises to 200 DEG C~2000 DEG C, and under conditions of temperature is 200 DEG C~2000 DEG C, keeps the temperature 0.1h~10h, then
With rate of temperature fall for 0.1 DEG C/min~10 DEG C/min, high temperature pyrolysis unit temp is down to room temperature by 200 DEG C~2000 DEG C, is obtained
To carbon fibre fabric；
Two, magnetron sputtering prepares metallic nickel nano granule/carbon fabric composite material:
Carbon fibre fabric is placed in magnetron sputtering apparatus, nickel target is fixed on cathode first, carbon fibre fabric is fixed
On the anode of sample stage, and controlling the distance between nickel target and carbon fibre fabric is 1mm~100mm, then splashes magnetic control
Pressure is evacuated to 0.001Pa~1Pa in the reaction chamber of jet device, then is passed through argon gas with flow velocity for 1sccm~100sccm, finally exists
Sputtering power be 10W~1000W and sample stage rotation speed be 1rpm~100rpm under conditions of sputtered, until sputtering
Metallic nickel nano granule layer obtains metallic nickel nano granule/carbon fabric composite material with a thickness of 100~10000nm；
Three, plasma enhanced chemical vapor deposition:
1., metallic nickel nano granule/carbon fabric composite material is placed in plasma enhanced chemical vapor deposition and set
In standby, pressure in the reaction chamber of plasma enhanced chemical vapor deposition equipment is evacuated to 1Pa~100Pa first, then with stream
Speed is the mixed gas that 1sccm~100sccm is passed through methane and hydrogen；
The velocity ratio of methane and hydrogen is 3:(1.5~2.5 in the mixed gas of the methane and hydrogen)；
2., under conditions of radio-frequency power is 10W~1000W, deposit 0.1h~10h, take out the post-depositional material of one side；
3., 1. and 2. the post-depositional material another side of one side is repeated 1 times by step 3, the material after obtaining double-sided deposition
Material；
4., by the material after double-sided deposition by step 3 1. to 3. repeating 0 time~4 times, obtain based on carbon fibre fabric, gold
Belong to the sandwich-type flexible electromagnetic shielding material of nano nickel particles and graphene；
The sandwich-type flexible electromagnetic shielding material based on carbon fibre fabric, metallic nickel nano granule and graphene
With a thickness of 0.62mm or more.
The beneficial effects of the present invention are:
One, the sandwich-type flexibility electromagnetism prepared by the present invention based on carbon fibre fabric, metallic nickel nano granule and graphene
Shielding material has excellent electric conductivity, and conductivity is up to 625S m-1。
Two, the sandwich-type flexibility electromagnetism prepared by the present invention based on carbon fibre fabric, metallic nickel nano granule and graphene
Shielding material has the multidimensional heterojunction structure of sandwich-type, may advantageously facilitate synergistic effect of each component during electromagnetic shielding,
Its total electromagnetic shielding efficiency is up to 50.6dB.
Three, the sandwich-type flexibility electromagnetism prepared by the present invention based on carbon fibre fabric, metallic nickel nano granule and graphene
Shielding material has high flexibility (flexible, foldable, can distort), lightweight and a ultra-slim features, and density is down to 113mg/cm3,
Its thickness is down to 0.65mm.
The present invention is used for a kind of sandwich-type flexibility electromagnetic screen based on carbon fibre fabric, metallic nickel nano granule and graphene
Cover the preparation method of material.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of the carbon fibre fabric of one step 1 of embodiment preparation；
Fig. 2 is metallic nickel nano granule/carbon fabric composite material scanning electron microscope of one step 2 of embodiment preparation
Figure；
Fig. 3 is that the sandwich-type based on carbon fibre fabric, metallic nickel nano granule and graphene prepared by embodiment one is flexible
The scanning electron microscope (SEM) photograph of electromagnetic shielding material；
Fig. 4 is X-ray diffractogram, and 1 is the preparation of embodiment one based on carbon fibre fabric, metallic nickel nano granule and graphite
The sandwich-type flexible electromagnetic shielding material of alkene, 2 be the X-ray diffraction standard card of metallic nickel；
Fig. 5 is that the sandwich-type based on carbon fibre fabric, metallic nickel nano granule and graphene prepared by embodiment one is flexible
The electromagnetic shielding efficiency of electromagnetic shielding material and the relational graph of wave frequency, 1 is total electromagnetic shielding efficiency, and 2 be electromagnetic absorption
Loss, 3 are lost for ELECTROMAGNETIC REFLECTION；
Fig. 6 is that the sandwich-type based on carbon fibre fabric, metallic nickel nano granule and graphene prepared by embodiment one is flexible
The bending effect figure of electromagnetic shielding material；
Fig. 7 is that the sandwich-type based on carbon fibre fabric, metallic nickel nano granule and graphene prepared by embodiment one is flexible
The folding effect figure of electromagnetic shielding material；
Fig. 8 is that the sandwich-type based on carbon fibre fabric, metallic nickel nano granule and graphene prepared by embodiment one is flexible
The distortion effects figure of electromagnetic shielding material.
Specific embodiment
Specific embodiment 1: present embodiment is a kind of based on carbon fibre fabric, metallic nickel nano granule and graphene
The preparation method of sandwich-type flexible electromagnetic shielding material, it is carried out according to the following steps:
One, carbon fibre fabric is prepared:
Container equipped with biomass fiber fabric is placed in high temperature pyrolysis device, is passed through inertia into high temperature pyrolysis device
Gas 1min~60min, under the protection of inert gas, with heating rate for 0.1 DEG C/min~10 DEG C/min, by high temperature pyrolysis
The temperature of device rises to 200 DEG C~2000 DEG C, and under conditions of temperature is 200 DEG C~2000 DEG C, keeps the temperature 0.1h~10h, then
With rate of temperature fall for 0.1 DEG C/min~10 DEG C/min, high temperature pyrolysis unit temp is down to room temperature by 200 DEG C~2000 DEG C, is obtained
To carbon fibre fabric；
Two, magnetron sputtering prepares metallic nickel nano granule/carbon fabric composite material:
Carbon fibre fabric is placed in magnetron sputtering apparatus, nickel target is fixed on cathode first, carbon fibre fabric is fixed
On the anode of sample stage, and controlling the distance between nickel target and carbon fibre fabric is 1mm~100mm, then splashes magnetic control
Pressure is evacuated to 0.001Pa~1Pa in the reaction chamber of jet device, then is passed through argon gas with flow velocity for 1sccm~100sccm, finally exists
Sputtering power be 10W~1000W and sample stage rotation speed be 1rpm~100rpm under conditions of sputtered, until sputtering
Metallic nickel nano granule layer obtains metallic nickel nano granule/carbon fabric composite material with a thickness of 100~10000nm；
Three, plasma enhanced chemical vapor deposition:
1., metallic nickel nano granule/carbon fabric composite material is placed in plasma enhanced chemical vapor deposition and set
In standby, pressure in the reaction chamber of plasma enhanced chemical vapor deposition equipment is evacuated to 1Pa~100Pa first, then with stream
Speed is the mixed gas that 1sccm~100sccm is passed through methane and hydrogen；
The velocity ratio of methane and hydrogen is 3:(1.5~2.5 in the mixed gas of the methane and hydrogen)；
2., under conditions of radio-frequency power is 10W~1000W, deposit 0.1h~10h, take out the post-depositional material of one side；
3., 1. and 2. the post-depositional material another side of one side is repeated 1 times by step 3, the material after obtaining double-sided deposition
Material；
4., by the material after double-sided deposition by step 3 1. to 3. repeating 0 time~4 times, obtain based on carbon fibre fabric, gold
Belong to the sandwich-type flexible electromagnetic shielding material of nano nickel particles and graphene；
The sandwich-type flexible electromagnetic shielding material based on carbon fibre fabric, metallic nickel nano granule and graphene
With a thickness of 0.62mm or more.
The beneficial effect of present embodiment is:
One, the sandwich-type based on carbon fibre fabric, metallic nickel nano granule and graphene of present embodiment preparation is flexible
Electromagnetic shielding material has excellent electric conductivity, and conductivity is up to 625S m-1。
Two, the sandwich-type based on carbon fibre fabric, metallic nickel nano granule and graphene of present embodiment preparation is flexible
Electromagnetic shielding material has the multidimensional heterojunction structure of sandwich-type, may advantageously facilitate collaboration of each component during electromagnetic shielding and makees
With total electromagnetic shielding efficiency is up to 50.6dB.
Three, the sandwich-type based on carbon fibre fabric, metallic nickel nano granule and graphene of present embodiment preparation is flexible
Electromagnetic shielding material has high flexibility (flexible, foldable, can distort), lightweight and a ultra-slim features, and density is down to 113mg
cm-3, thickness is down to 0.65mm.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: biology described in step 1
Matter fabric is bamboo fiber, cotton fabric, hemp fabric or regeneration spinning fibre fabric.Other and specific implementation
Mode one is identical.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that: described in step 2
The purity of nickel target is 90.00%~99.99%.It is other the same as one or two specific embodiments.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three: institute in step 2
The purity of argon stated is 90.00%~99.99%.It is other identical as specific embodiment one to three.
Specific embodiment 5: unlike one of present embodiment and specific embodiment one to four: institute in step 3
The methane purity stated is 90.00%~99.99%；Hydrogen purity described in step 3 is 90.00%~99.99%.It is other
It is identical as specific embodiment one to four.
Specific embodiment 6: unlike one of present embodiment and specific embodiment one to five: will in step 1
Container equipped with biomass fiber fabric is placed in high temperature pyrolysis device, and inert gas 30min is passed through into high temperature pyrolysis device
~60min, under the protection of inert gas, with heating rate for 5 DEG C/min~10 DEG C/min, by the temperature of high temperature pyrolysis device
200 DEG C~1000 DEG C are risen to, and under conditions of temperature is 200 DEG C~1000 DEG C, keeps the temperature 1h~10h, then with rate of temperature fall for 5
DEG C/min~10 DEG C/min, high temperature pyrolysis unit temp is down to room temperature by 200 DEG C~1000 DEG C, obtains carbon fibre fabric.Its
It is identical as specific embodiment one to five.
Specific embodiment 7: unlike one of present embodiment and specific embodiment one to six: being controlled in step 2
The distance between nickel target and carbon fibre fabric processed are 60mm~100mm, then by pressure in the reaction chamber of magnetron sputtering apparatus
It is evacuated to 0.003Pa~1Pa, then argon gas is passed through for 11sccm~100sccm with flow velocity.It is other with one to six phase of specific embodiment
Together.
Specific embodiment 8: unlike one of present embodiment and specific embodiment one to seven: in step 2 most
It is sputtered under conditions of sputtering power is 100W~1000W and sample stage rotation speed is 20rpm~100rpm afterwards.It is other
It is identical as specific embodiment one to seven.
Specific embodiment 9: unlike one of present embodiment and specific embodiment one to eight: step 3 1. in
Pressure in the reaction chamber of plasma enhanced chemical vapor deposition equipment is evacuated to 50Pa~100Pa first.Other and specific reality
It is identical to apply mode one to eight.
Specific embodiment 10: unlike one of present embodiment and specific embodiment one to nine: step 3 2. in
Under conditions of radio-frequency power is 200W~1000W, 1h~10h is deposited.It is other identical as specific embodiment one to nine.
Beneficial effects of the present invention are verified using following embodiment:
Embodiment one:
A kind of system of the sandwich-type flexible electromagnetic shielding material based on carbon fibre fabric, metallic nickel nano granule and graphene
Preparation Method, it is carried out according to the following steps:
One, carbon fibre fabric is prepared:
Container equipped with biomass fiber fabric is placed in high temperature pyrolysis device, is passed through inertia into high temperature pyrolysis device
The temperature of high temperature pyrolysis device, with heating rate for 5 DEG C/min, is risen to 1000 under the protection of inert gas by gas 30min
DEG C, and temperature be 1000 DEG C under conditions of, keep the temperature 1h, then with rate of temperature fall be 5 DEG C/min, by high temperature pyrolysis unit temp by
1000 DEG C are down to room temperature, obtain carbon fibre fabric；
Two, magnetron sputtering prepares metallic nickel nano granule/carbon fabric composite material:
Carbon fibre fabric is placed in magnetron sputtering apparatus, nickel target is fixed on cathode first, carbon fibre fabric is fixed
On the anode of sample stage, and controlling the distance between nickel target and carbon fibre fabric is 60mm, then by magnetron sputtering apparatus
Reaction chamber in pressure be evacuated to 0.003Pa, then with flow velocity be that 11sccm is passed through argon gas, be finally 100W and sample in sputtering power
Platform rotation speed is sputtered under conditions of being 20rpm, until the metallic nickel nano granule layer of sputtering obtains with a thickness of 500nm
Metallic nickel nano granule/carbon fabric composite material；
Three, plasma enhanced chemical vapor deposition:
1., metallic nickel nano granule/carbon fabric composite material is placed in plasma enhanced chemical vapor deposition and set
In standby, pressure in the reaction chamber of plasma enhanced chemical vapor deposition equipment is evacuated to 50Pa first, then pass to methane and
The mixed gas of hydrogen；
The flow velocity of methane is 8.4sccm in the mixed gas of the methane and hydrogen, and the flow velocity of hydrogen is 5.6sccm；
2., under conditions of radio-frequency power is 200W, deposit 1h, take out the post-depositional material of one side；
3., 1. and 2. the post-depositional material another side of one side is repeated 1 times by step 3, obtain based on carbon fibre fabric,
The sandwich-type flexible electromagnetic shielding material of metallic nickel nano granule and graphene；
The sandwich-type flexible electromagnetic shielding material based on carbon fibre fabric, metallic nickel nano granule and graphene
With a thickness of 0.65mm.
Biomass fiber fabric described in step 1 is cotton fabric.
The purity of nickel target described in step 2 is 99.99%.
Purity of argon described in step 2 is 99.99%.
Methane purity described in step 3 is 99.99%；Hydrogen purity described in step 3 is 99.99%.
Fig. 1 is the scanning electron microscope (SEM) photograph of the carbon fibre fabric of one step 1 of embodiment preparation；As seen from the figure, carbon fiber surface phase
To coarse, the metal nanoparticle and carbon fiber surface for being conducive to subsequent magnetron sputtering deposition generate mechanical interlock, and increase
Interfacial adhesion power between the two by force.
Fig. 2 is metallic nickel nano granule/carbon fabric composite material scanning electron microscope of one step 2 of embodiment preparation
Figure；By figure can observe the coarse surface of original carbon fiber metallic nickel nano granule deposition after become uniform.
Fig. 3 is that the sandwich-type based on carbon fibre fabric, metallic nickel nano granule and graphene prepared by embodiment one is flexible
The scanning electron microscope (SEM) photograph of electromagnetic shielding material；Metallic nickel nano granule/carbon fabric composite material surface can observe by figure
A large amount of, the fine and close dandelion shape graphene of successful growth.
Fig. 4 is X-ray diffractogram, and 1 is the preparation of embodiment one based on carbon fibre fabric, metallic nickel nano granule and graphite
The sandwich-type flexible electromagnetic shielding material of alkene, 2 be the X-ray diffraction standard card of metallic nickel；As seen from the figure, by comparing metal
The X-ray diffraction standard card of nickel, the composite material contain the ingredient of metallic nickel.In addition, the X-ray diffraction signal at 26.7 °
Also show the ingredient that the composite material contains graphene.
The sandwich-type flexible electrical based on carbon fibre fabric, metallic nickel nano granule and graphene prepared using embodiment one
Magnetic shielding material carries out electromagnetic shielding performance, and test and calculating process are as follows:
It one, will be having a size of 22.9mm × 10.2mm × 0.65mm based on carbon fibre fabric, metallic nickel nano granule and stone
The sandwich-type flexible electromagnetic shielding material of black alkene is fixed on sample stage；
Two, using PNA-X N5244a type Network Analyzer be based on waveguide method test S parameter, test scope be 8.2GHz~
12.4GHz；
Three, total electromagnetic shielding efficiency (SEtotal), electromagnetic absorption be lost (SEA) and ELECTROMAGNETIC REFLECTION loss (SET) by following
Formula is calculated:
SEtotal(dB)=- 10log [| S21|2]
SER=-10log (1- | S11|2)
SEA=-10log [| S21|2/(1-|S11|2)]
Fig. 5 is that the sandwich-type based on carbon fibre fabric, metallic nickel nano granule and graphene prepared by embodiment one is flexible
The electromagnetic shielding efficiency of electromagnetic shielding material and the relational graph of wave frequency, 1 is total electromagnetic shielding efficiency, and 2 be electromagnetic absorption
Loss, 3 are lost for ELECTROMAGNETIC REFLECTION；As seen from the figure, which has excellent electromagnetic shielding performance, total electromagnetic screen
Efficiency is covered up to 50.6dB, in addition, the electromagnetic absorption of the electromagnetic shielding material is lost up to 29.7dB, higher than its ELECTROMAGNETIC REFLECTION
It is lost (20.9dB), shows that electromagnetic shielding material absorption loss in electromagnetic shielding action is occupied an leading position.
Fig. 6 is that the sandwich-type based on carbon fibre fabric, metallic nickel nano granule and graphene prepared by embodiment one is flexible
The bending effect figure of electromagnetic shielding material；Fig. 7 is the preparation of embodiment one based on carbon fibre fabric, metallic nickel nano granule and stone
The folding effect figure of the sandwich-type flexible electromagnetic shielding material of black alkene；Fig. 8 is the preparation of embodiment one based on carbon fibre fabric, gold
Belong to the distortion effects figure of the sandwich-type flexible electromagnetic shielding material of nano nickel particles and graphene；As seen from the figure, the composite material
With high flexibility, flexible, folding, torsional deformation.
Using four probe resistance rate testers (model RTS-8, four probe Science and Technology Ltd. of Guangzhou), embodiment one is made
The standby sandwich-type flexible electromagnetic shielding material based on carbon fibre fabric, metallic nickel nano granule and graphene is tested, electricity
Conductance is up to 625S m-1。
Sandwich-type flexibility electromagnetism based on carbon fibre fabric, metallic nickel nano granule and graphene prepared by embodiment one
Shielding material carries out the measurement of volume and quality, and density is calculated down to 113mg/cm3, and thickness is down to 0.65mm.
Claims (10)
1. a kind of preparation of the sandwich-type flexible electromagnetic shielding material based on carbon fibre fabric, metallic nickel nano granule and graphene
Method, it is characterised in that it is carried out according to the following steps:
One, carbon fibre fabric is prepared:
Container equipped with biomass fiber fabric is placed in high temperature pyrolysis device, is passed through inert gas into high temperature pyrolysis device
1min~60min, under the protection of inert gas, with heating rate for 0.1 DEG C/min~10 DEG C/min, by high temperature pyrolysis device
Temperature rise to 200 DEG C~2000 DEG C, and under conditions of temperature is 200 DEG C~2000 DEG C, keep the temperature 0.1h~10h, then with drop
Warm rate is 0.1 DEG C/min~10 DEG C/min, and high temperature pyrolysis unit temp is down to room temperature by 200 DEG C~2000 DEG C, obtains carbon
Fabric；
Two, magnetron sputtering prepares metallic nickel nano granule/carbon fabric composite material:
Carbon fibre fabric is placed in magnetron sputtering apparatus, nickel target is fixed on cathode first, carbon fibre fabric is fixed on sample
On the anode of sample platform, and controlling the distance between nickel target and carbon fibre fabric is 1mm~100mm, then sets magnetron sputtering
Pressure is evacuated to 0.001Pa~1Pa in standby reaction chamber, then is passed through argon gas with flow velocity for 1sccm~100sccm, is finally sputtering
Power be 10W~1000W and sample stage rotation speed be 1rpm~100rpm under conditions of sputtered, until sputtering metal
Nano nickel particles layer obtains metallic nickel nano granule/carbon fabric composite material with a thickness of 100~10000nm；
Three, plasma enhanced chemical vapor deposition:
1., metallic nickel nano granule/carbon fabric composite material is placed in plasma enhanced chemical vapor deposition equipment,
Pressure in the reaction chamber of plasma enhanced chemical vapor deposition equipment is evacuated to 1Pa~100Pa first, is then with flow velocity
1sccm~100sccm is passed through the mixed gas of methane and hydrogen；
The velocity ratio of methane and hydrogen is 3:(1.5~2.5 in the mixed gas of the methane and hydrogen)；
2., under conditions of radio-frequency power is 10W~1000W, deposit 0.1h~10h, take out the post-depositional material of one side；
3., 1. and 2. the post-depositional material another side of one side is repeated 1 times by step 3, the material after obtaining double-sided deposition；
4., by the material after double-sided deposition by step 3 1. to 3. repeating 0 time~4 times, obtain based on carbon fibre fabric, metallic nickel
The sandwich-type flexible electromagnetic shielding material of nano particle and graphene；
The thickness of the sandwich-type flexible electromagnetic shielding material based on carbon fibre fabric, metallic nickel nano granule and graphene
For 0.62mm or more.
2. a kind of sandwich-type based on carbon fibre fabric, metallic nickel nano granule and graphene according to claim 1 is soft
Property electromagnetic shielding material preparation method, it is characterised in that biomass fiber fabric described in step 1 be bamboo fiber,
Cotton fabric, hemp fabric or regeneration spinning fibre fabric.
3. a kind of sandwich-type based on carbon fibre fabric, metallic nickel nano granule and graphene according to claim 1 is soft
Property electromagnetic shielding material preparation method, it is characterised in that the purity of nickel target described in step 2 be 90.00%~
99.99%.
4. a kind of sandwich-type based on carbon fibre fabric, metallic nickel nano granule and graphene according to claim 1 is soft
Property electromagnetic shielding material preparation method, it is characterised in that purity of argon described in step 2 be 90.00%~99.99%.
5. a kind of sandwich-type based on carbon fibre fabric, metallic nickel nano granule and graphene according to claim 1 is soft
Property electromagnetic shielding material preparation method, it is characterised in that methane purity described in step 3 be 90.00%~99.99%；
Hydrogen purity described in step 3 is 90.00%~99.99%.
6. a kind of sandwich-type based on carbon fibre fabric, metallic nickel nano granule and graphene according to claim 1 is soft
Property electromagnetic shielding material preparation method, it is characterised in that high temperature will be placed in equipped with the container of biomass fiber fabric in step 1
In pyrolysis installation, inert gas 30min~60min is passed through into high temperature pyrolysis device, under the protection of inert gas, with heating
Rate is 5 DEG C/min~10 DEG C/min, the temperature of high temperature pyrolysis device is risen to 200 DEG C~1000 DEG C, and be 200 DEG C in temperature
Under conditions of~1000 DEG C, 1h~10h is kept the temperature, then with rate of temperature fall for 5 DEG C/min~10 DEG C/min, by high temperature pyrolysis device temperature
Degree is down to room temperature by 200 DEG C~1000 DEG C, obtains carbon fibre fabric.
7. a kind of sandwich-type based on carbon fibre fabric, metallic nickel nano granule and graphene according to claim 1 is soft
Property electromagnetic shielding material preparation method, it is characterised in that in step 2 control the distance between nickel target and carbon fibre fabric be
Then pressure in the reaction chamber of magnetron sputtering apparatus is evacuated to 0.003Pa~1Pa by 60mm~100mm, then with flow velocity be 11sccm
~100sccm is passed through argon gas.
8. a kind of sandwich-type based on carbon fibre fabric, metallic nickel nano granule and graphene according to claim 1 is soft
Property electromagnetic shielding material preparation method, it is characterised in that in step 2 finally sputtering power be 100W~1000W and sample
Platform rotation speed is sputtered under conditions of being 20rpm~100rpm.
9. a kind of sandwich-type based on carbon fibre fabric, metallic nickel nano granule and graphene according to claim 1 is soft
The preparation method of property electromagnetic shielding material, it is characterised in that step 3 1. in plasma enhanced chemical vapor deposition is set first
Pressure is evacuated to 50Pa~100Pa in standby reaction chamber.
10. a kind of sandwich-type based on carbon fibre fabric, metallic nickel nano granule and graphene according to claim 1 is soft
Property electromagnetic shielding material preparation method, it is characterised in that step 3 2. in radio-frequency power be 200W~1000W under conditions of,
Deposit 1h~10h.
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| CN114633531A (en) * | 2022-03-01 | 2022-06-17 | 浙江工业大学 | Preparation method of anisotropic heat-conducting electromagnetic shielding nylon composite film |
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