CN108377637A - A kind of activated carbon fiber-ferriferrous oxide composite material and preparation method thereof - Google Patents
A kind of activated carbon fiber-ferriferrous oxide composite material and preparation method thereof Download PDFInfo
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- CN108377637A CN108377637A CN201810148448.6A CN201810148448A CN108377637A CN 108377637 A CN108377637 A CN 108377637A CN 201810148448 A CN201810148448 A CN 201810148448A CN 108377637 A CN108377637 A CN 108377637A
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- carbon fiber
- activated carbon
- composite material
- oxide composite
- ferriferrous oxide
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- 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
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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
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- 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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- Electromagnetism (AREA)
- Microelectronics & Electronic Packaging (AREA)
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- General Chemical & Material Sciences (AREA)
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Abstract
The present invention provides a kind of activated carbon fiber ferriferrous oxide composite materials and preparation method thereof, viscose felt is placed in phosphoric acid solution and impregnates preset time, after taking out drying, it is placed in progress first time carbonization in the Muffle furnace full of inert gas, obtains viscose based activated carbon fiber felt；The viscose based activated carbon fiber felt is impregnated in the ferric chloride solution of thermostat water bath；It after taking out drying, then is placed in glucose solution, is dried after taking-up, obtain iron content active carbon fiber felt；The iron content active carbon fiber felt is placed in the Muffle furnace full of inert gas and carries out second of carbonization, obtains activated carbon fiber ferriferrous oxide composite material.It has the advantages that：First, experiment condition is simple, and raw materials are cheap；Second activated carbon fiber high yield rate；Ferroso-ferric oxide is supported on active carbon fiber felt by the method for third, in-situ reducing, and binding strength is higher, composite material lighter weight, and the wave-absorbing effect with wideband.
Description
Technical field
This specification be related to absorbing material field more particularly to a kind of activated carbon fiber-ferriferrous oxide composite material and
Preparation method.
Background technology
Since LAN, radar system, mobile phone etc. increase what GHz microwave sections were applied, electromagnetic wave is as transmission matchmaker
Matter is widely applied, and the electromagnetic pollution that electromagnetic wave generates seriously destroys ecological environment, threatens people's health.With science
The development of technology, absorbing material suffer from extremely wide application in terms of civilian and military, and the application of absorbing material is to prevent
Electromagnetic pollution, the effective means for realizing radar invisible, electromagnetic compatibility, therefore the superior absorbing material of processability have far-reaching
Meaning.
Currently, absorbing material just develops towards the direction of " thin, light, wide, strong ", but the absorbing material of one-component can not be same
When meet these requirements.
Invention content
A kind of activated carbon fiber-ferriferrous oxide composite material of this specification embodiment offer and preparation method thereof, prepares
The composite wave absorption material gone out can overcome the shortcomings that one-component in current absorbing material.
In order to solve the above technical problems, what this specification embodiment was realized in：
It is multiple for controlling the present invention provides a kind of preparation method of activated carbon fiber-ferriferrous oxide composite material
Terminal device, including：
Viscose felt is placed in phosphoric acid solution and impregnates preset time, after taking out drying, is placed in the Muffle full of inert gas
First time carbonization is carried out in stove, obtains viscose based activated carbon fiber felt；
The viscose based activated carbon fiber felt is impregnated in the ferric chloride solution of thermostat water bath；After taking out drying, then
It is placed in glucose solution, is dried after taking-up, obtain iron content active carbon fiber felt；
The iron content active carbon fiber felt is placed in the Muffle furnace full of inert gas and carries out second of carbonization, is lived
Property carbon fiber-ferriferrous oxide composite material.
Preferably, in the preparation method of above-mentioned activated carbon fiber-ferriferrous oxide composite material, the phosphoric acid solution
A concentration of 0.5-5mol/L.
Preferably, in the preparation method of above-mentioned activated carbon fiber-ferriferrous oxide composite material, the preset time
For 1-12h.
Preferably, in the preparation method of above-mentioned activated carbon fiber-ferriferrous oxide composite material, the first time carbon
The carburizing temperature of change is 500-750 DEG C, and heating rate is 5-15 DEG C/min, and atmosphere is nitrogen or argon gas, sintering time 1-3h.
Preferably, in the preparation method of above-mentioned activated carbon fiber-ferriferrous oxide composite material, the water bath with thermostatic control
The temperature of pot is 40-70 DEG C.
Preferably, in the preparation method of above-mentioned activated carbon fiber-ferriferrous oxide composite material, the water bath with thermostatic control
The concussion speed of pot is 40-70r/min, time 1-3h.
Preferably, in the preparation method of above-mentioned activated carbon fiber-ferriferrous oxide composite material, the iron chloride is molten
Liquid is saturation ferric chloride solution.
Preferably, in the preparation method of above-mentioned activated carbon fiber-ferriferrous oxide composite material, the glucose is molten
The molar ratio of liquid and the ferric chloride solution is 1：1-1：5.
Preferably, in the preparation method of above-mentioned activated carbon fiber-ferriferrous oxide composite material, second of the carbon
The carburizing temperature of change is 700-850 DEG C, and heating rate is 10-20 DEG C/min, and atmosphere is nitrogen or argon gas, sintering time 1-2h.
The present invention also provides a kind of activated carbon fiber-ferriferrous oxide composite material ,-four oxygen of the activated carbon fiber
Change three iron composite material the process described above to be prepared.
In activated carbon fiber-ferriferrous oxide composite material provided by the invention and preparation method thereof, viscose felt is set
Preset time is impregnated in phosphoric acid solution, after taking out drying, is placed in progress first time carbonization in the Muffle furnace full of inert gas,
Obtain viscose based activated carbon fiber felt；The viscose based activated carbon fiber felt is impregnated in the ferric chloride solution of thermostat water bath
In；It after taking out drying, then is placed in glucose solution, is dried after taking-up, obtain iron content active carbon fiber felt；The iron content is lived
Property carbon fiber felt be placed in the Muffle furnace full of inert gas and carry out second and be carbonized, obtain activated carbon fiber-ferroso-ferric oxide
Composite material.It has the advantages that：First, experiment condition is simple, and raw materials are cheap；Second activated carbon fiber finished product
Rate is high；Ferroso-ferric oxide is supported on active carbon fiber felt by the method for third, in-situ reducing, and binding strength is higher, composite wood
Expect lighter weight, and the wave-absorbing effect with wideband.
Description of the drawings
In order to illustrate more clearly of this specification embodiment or technical solution in the prior art, below will to embodiment or
Attached drawing needed to be used in the description of the prior art is briefly described, it should be apparent that, the accompanying drawings in the following description is only
Some embodiments described in this specification, for those of ordinary skill in the art, in not making the creative labor property
Under the premise of, other drawings may also be obtained based on these drawings.
Fig. 1 is the flow chart of the preparation method of activated carbon fiber-ferriferrous oxide composite material in one embodiment of the invention；
Fig. 2 is the scanning electron microscope collection of illustrative plates of the activated carbon fiber-ferriferrous oxide composite material prepared according to method in Fig. 1.
Specific implementation mode
To keep the purpose, technical scheme and advantage of the application clearer, below in conjunction with the application specific embodiment and
Technical scheme is clearly and completely described in corresponding attached drawing.Obviously, described embodiment is only the application one
Section Example, instead of all the embodiments.Based on the embodiment in the application, those of ordinary skill in the art are not doing
Go out the every other embodiment obtained under the premise of creative work, shall fall in the protection scope of this application.
Activated carbon fiber belongs to carbon system absorbing material, is a kind of resistor-type absorbing material.Its carbon content is high, specific surface area
Greatly, micropore is abundant, and aperture is small and narrowly distributing, meets light weight, absorbs the requirements such as strong, at low cost, easily designed, in absorbing material
Field has broad prospects.Ferrite wave-absorbing material is the more also more ripe absorbing material of research.Ferrimagnetism inhales wave
Material is a kind of composite dielectric material, has magnetic loss effect again to the polarity effect in terms of the existing dielectric property of absorption of electromagnetic wave.
Have many advantages, such as that absorptivity is high, coating is thin and bandwidth, is widely used in radar absorbing field.Prepare activated carbon fiber
Technology tended to be ripe, ferrite is but single since larger magnetic loss also has larger advantage in terms of absorbing material
Activated carbon fiber absorbing property frequency band is narrow, and Ferrite Material density is big, limits its application.Based on this, the present invention proposes
A kind of activated carbon fiber-ferriferrous oxide composite material and preparation method thereof.
Below in conjunction with attached drawing, the technical solution that each embodiment of this specification provides is described in detail.
One embodiment of the invention provides a kind of activated carbon fiber-ferriferrous oxide composite material and preparation method thereof, such as
Shown in Fig. 1, Fig. 1 is the flow chart of the preparation method of activated carbon fiber-ferriferrous oxide composite material in one embodiment of the invention.
The method includes：Viscose felt is placed in phosphoric acid solution and impregnates preset time, after taking out drying, is placed in full of inert gas
First time carbonization is carried out in Muffle furnace, viscose based activated carbon fiber felt is obtained, such as the step S101 in Fig. 1；By the viscose base
Active carbon fiber felt is impregnated in the ferric chloride solution of thermostat water bath；It after taking out drying, then is placed in glucose solution, takes out
After dry, obtain iron content active carbon fiber felt, such as the step S103 in Fig. 1；The iron content active carbon fiber felt is placed in and is full of
It carries out being carbonized for second in the Muffle furnace of inert gas, activated carbon fiber-ferriferrous oxide composite material is obtained, in Fig. 1
Step S105.
Viscose felt is placed in phosphoric acid solution and impregnates preset time by step S101, after taking out drying, is placed in full of indifferent gas
First time carbonization is carried out in the Muffle furnace of body, obtains viscose based activated carbon fiber felt.
A concentration of 0.5-5mol/L of the phosphoric acid solution, the preset time impregnated in the phosphoric acid solution are 1-
12h.The carburizing temperature of the first time carbonization is 500-750 DEG C, and heating rate is 5-15 DEG C/min, and atmosphere is nitrogen or argon
Gas, sintering time 1-3h.
The viscose based activated carbon fiber felt is impregnated in the FeCl3 solution of thermostat water bath by step S103；It takes out and dries
It after dry, then is placed in glucose solution, is dried after taking-up, obtain iron content active carbon fiber felt.
The temperature of the thermostat water bath is 40-70 DEG C, and the concussion speed of the thermostat water bath is 40-70r/min,
Time is 1-3h, and the ferric chloride solution is saturation ferric chloride solution, the glucose solution and the ferric chloride solution
Molar ratio is 1：1-1：5.So that making Fe3+Fully it is supported on active carbon fiber felt.
The iron content active carbon fiber felt is placed in the Muffle furnace full of inert gas and carries out second of carbon by step S105
Change, obtains activated carbon fiber-ferriferrous oxide composite material.
Specifically, the carburizing temperature of second of carbonization is 700-850 DEG C, heating rate is 10-20 DEG C/min, atmosphere
For nitrogen or argon gas, sintering time 1-2h.Make Fe3+Under the action of glucose, by in-situ reducing, four oxidations three are ultimately generated
Iron obtains activated carbon fiber/ferriferrous oxide composite material.
The embodiment of the present invention additionally provides a kind of activated carbon fiber prepared according to above method-ferroso-ferric oxide composite wood
Material, specifically, barcode scanning Electronic Speculum collection of illustrative plates such as Fig. 2 of the activated carbon fiber-ferriferrous oxide composite material prepared according to above method
It is shown.
Next, being illustrated respectively with three specific embodiments.
Embodiment 1
First, the viscose felt of clip 25cm × 25cm, which is placed in the phosphoric acid solution of 2mol/L, impregnates 2h, dries, sets after taking-up
It is carbonized under nitrogen protection in Muffle furnace, carburizing temperature is 600 DEG C, and heating rate is 8 DEG C/min, soaking time
30min。
Secondly, active carbon fiber felt is cut to 18cm × 18cm, is impregnated in the ferric chloride solution prepared, is placed in perseverance
In warm water bath, 60 DEG C of water-bath 1h make Fe3+Fully it is supported on active carbon fiber felt.It is dried after taking-up, then is placed in and has configured
It in glucose solution, takes out and dries after a period of time, for being carbonized.
Then, the above-mentioned active carbon fiber felt handled well is again placed in Muffle furnace, is carbonized, is carbonized under the protection of nitrogen body
700 DEG C of temperature, 10 DEG C/min of heating rate make Fe3+Under the action of glucose, by in-situ reducing, four oxidations three are ultimately generated
Iron obtains activated carbon fiber/ferriferrous oxide composite material.
Embodiment 2
First, the viscose felt of clip 25cm × 25cm, which is placed in the phosphoric acid solution of 2mol/L, impregnates 5h, dries, sets after taking-up
It is carbonized under nitrogen protection in vacuum Muffle furnace, carburizing temperature is 650 DEG C, and heating rate is 10 DEG C/min, when heat preservation
Between 1h.
Secondly, active carbon fiber felt is cut to 18cm × 18cm, is impregnated in the ferric chloride solution prepared, is placed in perseverance
In warm water bath, 60 DEG C of water-bath 2h make Fe3+Fully it is supported on active carbon fiber felt.It is dried after taking-up, then is placed in and has configured
It in glucose solution, takes out and dries after a period of time, for being carbonized.
Finally, the above-mentioned active carbon fiber felt handled well is again placed in vacuum Muffle furnace, is carbonized under the protection of nitrogen body,
750 DEG C of carburizing temperature, 15 DEG C/min of heating rate make Fe3+Under the action of glucose, by in-situ reducing, four oxidations are ultimately generated
Three-iron obtains activated carbon fiber/ferriferrous oxide composite material.
Embodiment 3
First, the viscose felt of clip 25cm × 25cm, which is placed in the phosphoric acid solution of 3mol/L, impregnates 2h, dries, sets after taking-up
It is carbonized under nitrogen protection in vacuum Muffle furnace, carburizing temperature is 700 DEG C, and heating rate is 10 DEG C/min, when heat preservation
Between 1h.
Secondly, active carbon fiber felt is cut to 18cm × 18cm, is impregnated in the ferric chloride solution prepared, is placed in perseverance
In warm water bath, 60 DEG C of water-bath 3h make Fe3+Fully it is supported on active carbon fiber felt.It is dried after taking-up, then is placed in and has configured
It in glucose solution, takes out and dries after a period of time, for being carbonized.
Finally, the above-mentioned active carbon fiber felt handled well is again placed in Muffle furnace, is carbonized, is carbonized under the protection of nitrogen body
750 DEG C of temperature, 20 DEG C/min of heating rate make Fe3+Under the action of glucose, by in-situ reducing, four oxidations three are ultimately generated
Iron obtains activated carbon fiber/ferriferrous oxide composite material.
In activated carbon fiber-ferriferrous oxide composite material provided in an embodiment of the present invention and preparation method thereof, it will stick
Rubber mat, which is placed in phosphoric acid solution, impregnates preset time, after taking out drying, is placed in the Muffle furnace full of inert gas and carries out first
Secondary carbonization obtains viscose based activated carbon fiber felt；The viscose based activated carbon fiber felt is impregnated in the chlorination of thermostat water bath
In ferrous solution；It after taking out drying, then is placed in glucose solution, is dried after taking-up, obtain iron content active carbon fiber felt；It will be described
Iron content active carbon fiber felt, which is placed in the Muffle furnace full of inert gas, carries out second of carbonization, obtains-four oxygen of activated carbon fiber
Change three iron composite materials.Ferroso-ferric oxide is supported on active carbon fiber felt by the method for in-situ reducing, and binding strength is higher, multiple
Condensation material lighter weight, and the wave-absorbing effect with wideband.
Above is only an example of the present application, it is not intended to limit this application.For those skilled in the art
For, the application can have various modifications and variations.It is all within spirit herein and principle made by any modification, equivalent
Replace, improve etc., it should be included within the scope of claims hereof.
Claims (10)
1. a kind of preparation method of activated carbon fiber-ferriferrous oxide composite material, which is characterized in that including：
Viscose felt is placed in phosphoric acid solution and impregnates preset time, after taking out drying, is placed in the Muffle furnace full of inert gas
First time carbonization is carried out, viscose based activated carbon fiber felt is obtained；
The viscose based activated carbon fiber felt is impregnated in the ferric chloride solution of thermostat water bath；After taking out drying, then it is placed in
It in glucose solution, is dried after taking-up, obtains iron content active carbon fiber felt；
The iron content active carbon fiber felt is placed in the Muffle furnace full of inert gas and carries out second of carbonization, obtains activated carbon
Fiber-ferriferrous oxide composite material.
2. the preparation method of activated carbon fiber-ferriferrous oxide composite material according to claim 1, which is characterized in that
A concentration of 0.5-5mol/L of the phosphoric acid solution.
3. the preparation method of activated carbon fiber-ferriferrous oxide composite material according to claim 1, which is characterized in that
The preset time is 1-12h.
4. the preparation method of activated carbon fiber-ferriferrous oxide composite material according to claim 1, which is characterized in that
The carburizing temperature of the first time carbonization is 500-750 DEG C, and heating rate is 5-15 DEG C/min, and atmosphere is nitrogen or argon gas, is burnt
The knot time is 1-3h.
5. the preparation method of activated carbon fiber-ferriferrous oxide composite material according to claim 1, which is characterized in that
The temperature of the thermostat water bath is 40-70 DEG C.
6. the preparation method of activated carbon fiber-ferriferrous oxide composite material according to claim 1, which is characterized in that
The concussion speed of the thermostat water bath is 40-70r/min, time 1-3h.
7. the preparation method of activated carbon fiber-ferriferrous oxide composite material according to claim 1, which is characterized in that
The ferric chloride solution is saturation ferric chloride solution.
8. the preparation method of activated carbon fiber-ferriferrous oxide composite material according to claim 1, which is characterized in that
The molar ratio of the glucose solution and the ferric chloride solution is 1：1-1：5.
9. the preparation method of activated carbon fiber-ferriferrous oxide composite material according to claim 1, which is characterized in that
The carburizing temperature of second of carbonization is 700-850 DEG C, and heating rate is 10-20 DEG C/min, and atmosphere is nitrogen or argon gas, is burnt
Tie time 1-2h.
10. a kind of activated carbon fiber-ferriferrous oxide composite material, which is characterized in that the activated carbon fiber-ferroso-ferric oxide
Composite material is prepared according to requiring the method described in any one of 1 to 9.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1057241A (en) * | 1990-06-13 | 1991-12-25 | 李孝忠 | A kind of processing method of making activated carbon fiber |
| CN1295142A (en) * | 2000-10-28 | 2001-05-16 | 中山大学 | Phosphoric acid activation process of producing active carbon fiber |
| JP2002180370A (en) * | 2000-12-15 | 2002-06-26 | Toho Tenax Co Ltd | Carbon fiber for metal oxide coating and method for producing the same |
| CN1632199A (en) * | 2004-11-29 | 2005-06-29 | 东华大学 | Process for preparing big aperture active carbon fibers |
| CN101227770A (en) * | 2008-01-30 | 2008-07-23 | 谭羽非 | Activated carbon fiber soft body electric heating product and manufacturing method thereof |
| CN103241777A (en) * | 2013-05-22 | 2013-08-14 | 中国科学院长春应用化学研究所 | Preparation method of carbon material and carbon-ferroferric oxide composite material |
-
2018
- 2018-02-13 CN CN201810148448.6A patent/CN108377637B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1057241A (en) * | 1990-06-13 | 1991-12-25 | 李孝忠 | A kind of processing method of making activated carbon fiber |
| CN1295142A (en) * | 2000-10-28 | 2001-05-16 | 中山大学 | Phosphoric acid activation process of producing active carbon fiber |
| JP2002180370A (en) * | 2000-12-15 | 2002-06-26 | Toho Tenax Co Ltd | Carbon fiber for metal oxide coating and method for producing the same |
| CN1632199A (en) * | 2004-11-29 | 2005-06-29 | 东华大学 | Process for preparing big aperture active carbon fibers |
| CN101227770A (en) * | 2008-01-30 | 2008-07-23 | 谭羽非 | Activated carbon fiber soft body electric heating product and manufacturing method thereof |
| CN103241777A (en) * | 2013-05-22 | 2013-08-14 | 中国科学院长春应用化学研究所 | Preparation method of carbon material and carbon-ferroferric oxide composite material |
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