CN110295415A - A kind of preparation method of intercalated graphite alkene/carbon fiber magnetism Wave suction composite material - Google Patents
A kind of preparation method of intercalated graphite alkene/carbon fiber magnetism Wave suction composite material Download PDFInfo
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- CN110295415A CN110295415A CN201910577069.3A CN201910577069A CN110295415A CN 110295415 A CN110295415 A CN 110295415A CN 201910577069 A CN201910577069 A CN 201910577069A CN 110295415 A CN110295415 A CN 110295415A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/16—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from products of vegetable origin or derivatives thereof, e.g. from cellulose acetate
Abstract
The invention belongs to absorbing material preparation technical fields, more particularly to a kind of intercalated graphite alkene/carbon fiber magnetism Wave suction composite material preparation method, graphene layer expansion expansion layer is carried out including multilayer graphene oxide to be distributed in deionized water, obtains drying for standby after layer expansion graphite alkene；Layer expansion graphite alkene after drying is put into metal salt solution, and hydroxylated cellulose dispersing agent is added, is evaporated to after stirring and is dried to obtain intercalated graphite alkene；Intercalated graphite alkene is distributed to solution of the acquisition containing intercalated graphite alkene powder in viscose solution；Solution is prepared into after strip and block undulation degree pre-oxidize and obtains intercalated graphite alkene/carbon fiber magnetism suction wave composite fibre with carbonization treatment.Absorbing material, light weight are prepared using this method, and molding thickness is easy to control, there are preferable absorbent properties for the electromagnetic wave of high band.There is carbon fiber protection outside intercalated graphite alkene simultaneously, it is not perishable and be oxidized, it can be used in harsh climate and environment.
Description
Technical field
The invention belongs to absorbing material preparation technical fields more particularly to a kind of intercalated graphite alkene/carbon fiber magnetism to inhale wave
The preparation method of composite material.
Background technique
In recent years, the microwave absorbing material of radar invisible is widely applied to the stealthy of the military platforms such as ocean, land
In system of defense, target radar reflective surface area can be effectively reduced, increases the difficulty that target is found.It is excellent in order to obtain
Magnetic loss is the effective way for improving electromaganic wave absorbing property in conjunction with dielectric material by microwave absorbing material.At present in carbonaceous
Material, such as carbon fiber, graphene and carbon nano tube surface modify various magnetic-particles to improve the absorbing property of carbonaceous material,
It can effectively be merged when it was found that preferable Fe, Co, Ni metal base magnetic material of soft magnet performance is in conjunction with carbonaceous absorbing material each
From the advantage and disadvantage of dielectric loss and magnetic loss, the wide Wave suction composite material of lightweight, absorption band is prepared.However, at present in carbon
The methods of plating, chemical plating, reduction are generallyd use on material and prepares magnetisable coating, and the shortcomings that these methods is on the one hand to produce
There is the defects of certain pollution, another aspect magnetisable coating is easy to fall off to environment in the process, it is soft and more to need a kind of material
Durable absorbing carbon fiber wave material.The Chinese patent of Publication No. CN107567272 disclose a kind of absorbing carbon fiber wave material and
Preparation method, this method by carbon fiber oxidization fiber felt is padded in metal salt solution drying after high temperature cabonization prepare and
It is light at, the product quality, in certain frequency range good absorption effect, but to reach ideal wave-absorbing effect, need to load more
Magnetic-particle, while particle is also distributed in fiber surface that non-uniform phenomenon can also occur.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of intercalated graphite alkene/carbon fiber magnetism Wave suction composite materials
Preparation method.Intercalated graphite alkene/carbon fiber magnetism Wave suction composite material provided by the invention is by the way that intercalated graphite alkene to be added to
Fibrous inside generates more interfacial polarization effects, to reach better electromagnetic wave absorption performance.
The present invention provides the preparation method that a kind of intercalated graphite alkene/carbon fiber magnetism inhales wave composite fibre, key is
The following steps are included:
S1. multilayer graphene oxide is distributed in deionized water, it is swollen that graphene layer is then carried out under microwave field action
Swollen expansion layer, obtains layer expansion graphite alkene；
S2. layer expansion graphite alkene is dried；
S3. using the mixed liquor of second alcohol and water as solvent, saccharide compound and acetyl acetone salt is added, prepares metal salt
Solution, the acetyl acetone salt are one or more of acetylacetone cobalt, ferric acetyl acetonade, nickel acetylacetonate；
S4. the layer expansion graphite alkene after drying is put into the metal salt solution, microwave stirs 40min~60min, so
Hydroxylated cellulose dispersing agent is added afterwards, is stirred for being evaporated to drying after five minutes, obtains intercalated graphite alkene；
S5. the intercalated graphite alkene is distributed in viscose solution, be stirred well to it is uniformly mixed, obtain contain intercalation stone
The solution of black alkene powder；
S6. strip and block fibrous material is prepared in the step S5 solution being prepared；
S7. the strip and block fibrous material that step S6 is prepared is pre-oxidized and is carbonized, obtain intercalated graphite alkene/carbon
Fiber magnetism inhales wave composite fibre.
Preferably, the time of microwave field action is 60~100min in the step S1.
Preferably, drying temperature is 20~150 DEG C in the step S2, and drying time is 10~100min.
Preferably, the step S6 is specially that the solution that will contain intercalated graphite alkene powder carries out Static Spinning as spinning solution
Silk, then obtains the strip and block fibrous material by multistage stretching.
Preferably, the step S6 is specially that will inject high speed shear coagulating bath containing the solution of intercalated graphite alkene powder
In, ribbon fibrous material is prepared.
Preferably, sulfuric acid, aluminum sulfate, sodium sulphate are dissolved in deionized water and are prepared by the high speed shear coagulating bath
Mixed liquor, wherein each component mass percent be sulfuric acid 6.5~12%, aluminum sulfate 0.5~2.0%, sodium sulphate 18~26%,
Deionized water 60~75%.
Preferably, pre-oxidation described in step S7 is specially after being warming up to 200~400 DEG C by the rate of 5~10 DEG C/min
It is down to room temperature naturally after 2~5h of heat preservation.
Preferably, carbonization described in step S7 is specially to protect after being warming up to 500~1000 DEG C by the rate of 5~10 DEG C/min
100~500min of temperature, then natually cooled to room temperature.
Preferably, carbonization described in step S7 is specially to protect after being warming up to 550~750 DEG C by the rate of 5~10 DEG C/min
100~500min of temperature, then natually cooled to room temperature.
Compared with prior art, intercalated graphite alkene is added to fibrous inside, intercalated graphite alkene middle layer well by the present invention
Between magnetic-particle and graphene layer between produce than more rich interfacial effect, the graphene of dielectric loss and magnetic loss
Magnetic-particle synergistic effect and graphene are distributed along the axial direction of carbon fiber, these all promote the electro-magnetic wave absorption of material
Performance.The present invention passes through the dielectric constant that carburizing temperature controls carbon fiber simultaneously, and carbonizing degree deficiency will cause dielectric loss
It is smaller, it is excessively carbonized, carbon fiber is caused to reinforce reflection of electromagnetic wave, the present invention only controls carbon fibre carbonizing temperature one
The electromagnetic wave absorption performance of competence exertion good material in fixed range.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, rather than whole embodiments.Based on the embodiments of the present invention, ordinary skill
Personnel's every other embodiment obtained without making creative work, belongs to the model that the present invention protects
It encloses.
A kind of preparation method of intercalated graphite alkene/carbon fiber magnetism Wave suction composite material, comprising the following steps:
S1. multilayer graphene oxide is distributed in deionized water, it is swollen that graphene layer is then carried out under microwave field action
Swollen expansion layer, obtains layer expansion graphite alkene；
S2. layer expansion graphite alkene is dried；
S3. using the mixed liquor of second alcohol and water as solvent, saccharide compound and acetyl acetone salt is added, prepares metal salt
Solution, the acetyl acetone salt are one or more of acetylacetone cobalt, ferric acetyl acetonade, nickel acetylacetonate；
S4. the layer expansion graphite alkene after drying is put into the metal salt solution, microwave stirs 40min~60min, so
Hydroxylated cellulose dispersing agent is added afterwards, is stirred for being evaporated to drying after five minutes, obtains intercalated graphite alkene；
S5. the intercalated graphite alkene is distributed in viscose solution, be stirred well to it is uniformly mixed, obtain contain intercalation stone
The solution of black alkene powder；
S6. strip and block fibrous material is prepared in the step S5 solution being prepared；
S7. the strip and block fibrous material that step S6 is prepared is pre-oxidized and is carbonized, obtain intercalated graphite alkene/carbon
Fiber magnetism inhales wave composite fibre.
In above-mentioned preparation method provided by the invention, the microwave time is preferably 60min~100min in step S1, more excellent
Be selected as 100min, in addition, the multilayer graphene oxide in step S1 can be used commercial goods, but commercial goods may exist it is pure
The problems such as not high is spent, can also be prepared by following steps:
(1) graphene oxide is prepared by Hummers oxidizing process: first using natural flaky graphite powder as raw material, with two
Then secondary distilled water eccentric cleaning disperses graphene oxide in dehydrated alcohol, 50Hz ultrasonic disperse 20min to neutrality；Its
In, the dosage of dehydrated alcohol used in 100mg graphene oxide is 100mL；
(2) separate graphene oxide and multilayer graphene oxide: the graphene oxide ethyl alcohol that step (1) is prepared is molten
Liquid, which is placed in supercentrifuge, carries out centrifugal treating, and 5min is centrifuged under the revolving speed of 3000r/min, after centrifugation, by upper layer
Solution and the separation of bottom sediment object, upper solution are graphene oxide, and bottom sediment object is multilayer graphene oxide.
In step S2, drying temperature is preferably 20~150 DEG C, and more preferably 150 DEG C, drying time is preferably 10~
100min, more preferably 100min；
The time that microwave stirs in step S4 is preferably 40min~60min, more preferably 60min；
The method that the solution containing intercalated graphite alkene powder is prepared into strip and block fibrous material in step S6 is preferably quiet
Electrospinning process or fibrid technique.Electrostatic spinning process refers to the solution using intercalated graphite alkene powder is contained as spinning solution
Electrostatic spinning is carried out, then multistage stretching is prepared into strip and block fibrous material.Fibrid technique refers to containing intercalated graphite alkene
In the solution injection high speed shear coagulating bath of powder, be prepared ribbon fibrous material, high speed shear coagulating bath be by sulfuric acid,
Aluminum sulfate, sodium sulphate are dissolved in the mixed liquor that deionized water is prepared, wherein each component mass percent is preferably sulfuric acid 6.5-
12%, aluminum sulfate 0.5-2.0%, sodium sulphate 18-26%, deionized water 60-75%, more preferably sulfuric acid 8%, aluminum sulfate 2%,
Sodium sulphate 25%, deionized water 65%.Compare electrostatic spinning process, and chromatography fibre technology has spinning speed fast, and molding produces
The high advantage of product intensity.
After keeping the temperature 2-5h after preoxidation process is preferably warming up to 100-400 DEG C by the rate of 5-10 DEG C/min in step S7
Naturally it is down to room temperature.It is down to room temperature naturally after keeping the temperature 3h after being more preferably warming up to 300 DEG C by the rate of 6 DEG C/min.It was carbonized
Journey keeps the temperature 100-500min after being preferably warming up to 500-1000 DEG C by the rate of 5-10 DEG C/min, and then natural cooling is down to room
Temperature.300min is kept the temperature after being more preferably warming up to 550-750 DEG C by the rate of 6 DEG C/min, then natually cooled to room temperature.
Embodiment 1
S1. multilayer graphene oxide is distributed in deionized water, it is swollen that graphene layer is then carried out under microwave field action
Swollen expansion layer obtains layer expansion graphite alkene, and the microwave time is 100min；
S2. layer expansion graphite alkene is dried, drying temperature is 150 DEG C, drying time 100min；
S3. using the mixed liquor of second alcohol and water as solvent, saccharide compound and ferric acetyl acetonade is added, it is molten to prepare metal salt
Liquid；
S4. the layer expansion graphite alkene after drying is put into metal salt solution, microwave stirs 60min, and hydroxyl is then added
Cellulose dispersant is stirred for being evaporated to drying after five minutes, obtains intercalated graphite alkene；
S5. the intercalated graphite alkene is distributed in viscose solution, be stirred well to it is uniformly mixed, obtain contain intercalation stone
The solution of black alkene powder；
S6. solution step S5 being prepared carries out electrostatic spinning, and strip and block fibre is prepared by multistage stretching
Tie up material；
S7. 4h is kept the temperature after the strip and block fibrous material that step S6 is prepared being warming up to 300 DEG C by the rate of 6 DEG C/min
Be down to room temperature naturally afterwards and realize pre-oxidation, then keep the temperature 300min by being warming up to after 600 DEG C by the rate of 6 DEG C/min, then oneself
It so cools down to room temperature and realizes carbonization, obtain intercalated graphite alkene/carbon fiber magnetism and inhale wave composite fibre.
Embodiment 2
Ferric acetyl acetonade, acetylacetone cobalt, nickel acetylacetonate are used in step S3 as acetyl acetone salt prepares gold
Belong to salting liquid；Carbonisation is to be warming up to after 550 DEG C to keep the temperature 300min by the rate of 6 DEG C/min in step S7, then naturally cold
But it is down to room temperature.Other are the same as embodiment 1.
Embodiment 3
Ferric acetyl acetonade, acetylacetone cobalt, nickel acetylacetonate are used in step S3 as acetyl acetone salt prepares gold
Belong to salting liquid；Solution containing intercalated graphite alkene powder is prepared into strip and block undulation degree using fibrid technique by step S6
Material, specially first by the sulfuric acid of 80g, the aluminum sulfate of 20g, 250g sodium sulphate be dissolved in the deionized water of 650g be prepared into high speed
Coagulating bath is sheared, then by containing in the injection high speed shear coagulating bath of the solution of intercalated graphite alkene powder, ribbon is prepared
Fibrous material；Carbonisation is to be warming up to after 750 DEG C to keep the temperature 300min by the rate of 6 DEG C/min in step S7, then naturally cold
But it is down to room temperature.Other are the same as embodiment 1.
The alkene of intercalated graphite prepared by the present invention/carbon fiber magnetism Wave suction composite material have lighter quality, and
Electromagnetic wave absorption performance is more superior in 12-14GHz frequency range.Fibrid preparation process more can control material thickness and close simultaneously
Degree, can satisfy product demand of different shapes.
Finally it is to be appreciated that foregoing description is merely a preferred embodiment of the present invention, those skilled in the art is in the present invention
Enlightenment under, without prejudice to the purpose of the present invention and the claims, multiple similar transformation, such change can be made
It changes and falls within the protection scope of the present invention.
Claims (9)
1. a kind of intercalated graphite alkene/carbon fiber magnetism Wave suction composite material preparation method, which is characterized in that including following step
It is rapid:
S1. multilayer graphene oxide is distributed in deionized water, graphene layer expansion is then carried out under microwave field action and is expanded
Layer, obtains layer expansion graphite alkene；
S2. layer expansion graphite alkene is dried；
S3. using the mixed liquor of second alcohol and water as solvent, saccharide compound and acetyl acetone salt is added, it is molten to prepare metal salt
Liquid, the acetyl acetone salt are one or more of acetylacetone cobalt, ferric acetyl acetonade, nickel acetylacetonate；
S4. the layer expansion graphite alkene after drying is put into the metal salt solution, microwave stir 40min~60min, then plus
Enter hydroxylated cellulose dispersing agent, be stirred for being evaporated to drying after five minutes, obtains intercalated graphite alkene；
S5. the intercalated graphite alkene is distributed in viscose solution, be stirred well to it is uniformly mixed, obtain contain intercalated graphite alkene
The solution of powder；
S6. strip and block fibrous material is prepared in the step S5 solution being prepared；
S7. the strip and block fibrous material that step S6 is prepared is pre-oxidized and is carbonized, obtain intercalated graphite alkene/carbon fiber
Magnetism inhales wave composite fibre.
2. preparation method according to claim 1, which is characterized in that the time of microwave field action is 60 in the step S1
~100min.
3. preparation method according to claim 1, which is characterized in that drying temperature is 20~150 DEG C in the step S2,
Drying time is 10~100min.
4. preparation method according to claim 1, which is characterized in that the step S6 is specially that will contain intercalated graphite alkene
The solution of powder carries out electrostatic spinning as spinning solution, then obtains the strip and block fibrous material by multistage stretching.
5. preparation method according to claim 1, which is characterized in that the step S6 is specially that will contain intercalated graphite alkene
In the solution injection high speed shear coagulating bath of powder, ribbon fibrous material is prepared.
6. preparation method according to claim 5, which is characterized in that the high speed shear coagulating bath is by sulfuric acid, sulfuric acid
Aluminium, sodium sulphate are dissolved in the mixed liquor that deionized water is prepared, wherein each component mass percent is sulfuric acid 6.5~12%, sulphur
Sour aluminium 0.5~2.0%, sodium sulphate 18~26%, deionized water 60~75%.
7. preparation method according to claim 1, which is characterized in that pre-oxidation described in step S7 is specially to press 5~10
DEG C/rate of min is down to room temperature after keeping the temperature 2~5h after being warming up to 200~400 DEG C naturally.
8. preparation method according to claim 1, which is characterized in that described in step S7 carbonization be specially by 5~10 DEG C/
The rate of min keeps the temperature 100~500min after being warming up to 500~1000 DEG C, then natually cooled to room temperature.
9. preparation method according to claim 1, which is characterized in that described in step S7 carbonization be specially by 5~10 DEG C/
The rate of min keeps the temperature 100~500min after being warming up to 550~750 DEG C, then natually cooled to room temperature.
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