CN106028767B - A kind of composite electromagnetic absorption material and preparation method thereof - Google Patents
A kind of composite electromagnetic absorption material and preparation method thereof Download PDFInfo
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- CN106028767B CN106028767B CN201610313074.XA CN201610313074A CN106028767B CN 106028767 B CN106028767 B CN 106028767B CN 201610313074 A CN201610313074 A CN 201610313074A CN 106028767 B CN106028767 B CN 106028767B
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Abstract
The invention discloses a kind of composite electromagnetic absorption materials.The invention also discloses the preparation methods of above-mentioned composite electromagnetic absorption material, and bismuth nitrate is added in ethylene glycol and is stirred, is then recrystallized, and wash, being dried to obtain surface has the bismuth nitrate of hydroxyl modified；There is the bismuth nitrate of hydroxyl modified to be added in valine aqueous solution on surface once to be disperseed, add thiophene monomer and carry out twice dispersing, be then stirred, ammonium persulfate aqueous solution is added dropwise in whipping process, be then allowed to stand to obtain mixed material；After mixed material is filtered, washing, vacuum drying obtains composite electromagnetic absorption material.The present invention increases effectively electromagnetic wave receiving area compared with the existing technology, with higher electromagnetic consumable characteristic, reflection of electromagnetic wave loss can be effectively improved, enhance electromaganic wave absorbing property, there is good electromagnetic wave absorption performance in 9 13GHz microwave frequency bands, maximum inhales depth of convolution degree and reaches 39dB or more, and preparation process is simple, cost is easily-controllable.
Description
Technical field
The present invention relates to absorbing material technical field more particularly to a kind of composite electromagnetic absorption material and its preparation sides
Method.
Background technology
Polythiophene is a kind of excellent electro-magnetic wave absorption and shielding material at present, and bismuth nitrate is 7-15GHz microwave frequency bands
Interior excellent electromagnetic wave absorbent material, the composite material being made of conductive polythiophene cladding bismuth nitrate not only have good machinery
Intensity and processing performance, and since the two interface cooperates with generated Interfacial relaxation effect to be allowed to than single conductive polythiophene
Or bismuth nitrate has more superior electromaganic wave absorbing property, therefore have broad application prospects in electro-magnetic wave absorption field.
Application discloses " a kind of preparation method of polythiophene absorbing material " for 201410164105.0 patent, uses
Thiophene monomer after heat treatment, forms polythiophene, then is mixed in proportion with thermosetting polymer, coated in substrate or being solidified into
Type obtain include thermosetting polymer and the polythiophene absorbing material.The invention can be applied by the polythiophene of solid-state polymerization
Cover or curing molding after can obtain continuous conduction material；Take the polythiophene that solid-state polymerization obtains and thermosetting polymer compound
After form absorbing material.But the polythiophene degree of polymerization prepared by this method is not easy to control, and use in-situ polymerization molecular weight distribution
Unevenness is unfavorable for commercial application and cost control, and product absorbing property is difficult to obtain the promotion of essence, to influence the material
Extensive use.
Invention content
Technical problems based on background technology, the present invention propose a kind of composite electromagnetic absorption material and its preparation
Method increases effectively electromagnetic wave receiving area compared with the existing technology, has higher electromagnetic consumable characteristic, can effectively improve
Reflection of electromagnetic wave is lost, and enhances electromaganic wave absorbing property, has good electromagnetic wave absorbability in 9-13GHz microwave frequency bands
Can, maximum inhales depth of convolution degree and reaches -39dB or more, while preparation process of the present invention is simple, cost is easily-controllable.
A kind of preparation method of composite electromagnetic absorption material proposed by the present invention, includes the following steps：
S1, bismuth nitrate is added in ethylene glycol and is stirred, then recrystallized, washed, being dried to obtain surface has hydroxyl to repair
The bismuth nitrate of decorations；
S2, surface is had hydroxyl modified bismuth nitrate be added valine aqueous solution in once disperseed, add thiophene
Monomer carries out twice dispersing, is then stirred, ammonium persulfate aqueous solution is added dropwise in whipping process, be then allowed to stand to obtain mixture
Material；
S3, it after filtering mixed material, washs, vacuum drying obtains composite electromagnetic absorption material.
Preferably, in S1, the mass volume ratio (g/mL) of bismuth nitrate and ethylene glycol is 20~100：1000.
Preferably, in S1, the time of stirring is 24~72h.
Preferably, in S1, the speed of stirring is 100~300rpm.
Preferably, in S2, bismuth nitrate, thiophene monomer, valine and ammonium persulfate mass ratio be 1：1.6~4.8：0.4
~1.2：2.4~5.8.
Preferably, in S2, disperseed using ultrasound, the time of primary dispersion and twice dispersing is 0.8~1.2h.
Preferably, in S2, the speed of stirring is 45~55rpm.
Preferably, in S2, the rate of addition of ammonium persulfate aqueous solution is 1~2.5 drop/s.
Preferably, in S2, it is 20~30 DEG C that the temperature of solution system is maintained during the dropwise addition of ammonium persulfate aqueous solution.
Preferably, in S2, time of repose is 23~25h.
Preferably, in S3, vacuum drying temperature is 58~62 DEG C, and the vacuum drying time is 23~25h.
Preferably, in S3, the concrete operations of washing are as follows：Obtained solid material will be filtered and use distilled water and nothing successively
Water-ethanol is washed to filtrate in colourless.
The composite electromagnetic that a kind of preparation method for above-mentioned composite electromagnetic absorption material that the present invention also proposes is prepared
Wave absorbing material.
The present invention uses the bismuth nitrate by the modification of ethylene glycol surface hydroxylation to can be good at being scattered in valine solution
In, under the action of suitable temperature and appropriate initiator ammonium persulfate, thiophene easily slowly gathers on the bismuth nitrate surface of modified
Conjunction obtains the sheet polythiophene nanometer sheet of high molecular weight, and the polythiophene nanostructure of this special appearance increases effectively electromagnetic wave
Receiving area has higher electromagnetic consumable characteristic, can effectively improve reflection of electromagnetic wave loss, increase the electro-magnetic wave absorption of material
Characteristic.
Gained of the invention is had by the compound electromagnetic wave absorbent material of polythiophene/bismuth nitrate in 9-13GHz microwave frequency bands
Good electromagnetic wave absorption performance, the suction depth of convolution degree for the polythiophene microballoon -18dB that compares, the present invention is maximum inhale depth of convolution degree reach -
39dB or more is a kind of excellent electromagnetic wave absorbent material；Preparation process of the present invention is simple simultaneously, cost is easily-controllable.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of 3 gained composite electromagnetic absorption material of the embodiment of the present invention.
Fig. 2 is the scanning electron microscope (SEM) photograph of polythiophene trepanning microballoon obtained by comparative example.
Fig. 3 is the reflection of electromagnetic wave damage curve of 3 gained composite electromagnetic absorption material of the embodiment of the present invention.
Fig. 4 is the reflection of electromagnetic wave damage curve of polythiophene trepanning microballoon obtained by comparative example.
Specific implementation mode
In the following, technical scheme of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of preparation method of composite electromagnetic absorption material proposed by the present invention, includes the following steps：
S1, by bismuth nitrate and ethylene glycol by mass volume ratio (g/mL) it is 20：1000 stirrings, the speed of stirring are
300rpm, the time of stirring are for 24 hours, then to be recrystallized, and are washed, being dried to obtain surface has the bismuth nitrate of hydroxyl modified；
S2, by weight by 1 part of surface have hydroxyl modified bismuth nitrate be added containing 1.2 parts of valines aqueous solution in carry out
Ultrasonic disperse 0.8h is added 4.8 parts of thiophene monomers and carries out ultrasonic disperse 0.8h, then stirred with the mixing speed of 55rpm
It mixes, the aqueous solution containing 2.4 parts of ammonium persulfates is added dropwise in whipping process, rate of addition is 2.5 drops/s, and solution is maintained during being added dropwise
The temperature of system is 20 DEG C, is then allowed to stand 25h and obtains mixed material；
S3, after filtering mixed material, distilled water and absolute ethyl alcohol is then used to wash to filtrate in colourless successively, 58 DEG C
Vacuum drying 25h obtains composite electromagnetic absorption material.
Embodiment 2
A kind of preparation method of composite electromagnetic absorption material proposed by the present invention, includes the following steps：
S1, by bismuth nitrate and ethylene glycol by mass volume ratio (g/mL) it is 100：1000 stirrings, the speed of stirring are
The time of 100rpm, stirring are 72h, are then recrystallized, and are washed, being dried to obtain surface has the bismuth nitrate of hydroxyl modified；
S2, by weight by 1 part of surface have hydroxyl modified bismuth nitrate be added containing 0.4 part of valine aqueous solution in carry out
Ultrasonic disperse 1.2h is added 1.6 parts of thiophene monomers and carries out ultrasonic disperse 1.2h, then stirred with the mixing speed of 45rpm
It mixes, the aqueous solution containing 5.8 parts of ammonium persulfates is added dropwise in whipping process, rate of addition is 1 drop/s, and solution body is maintained during being added dropwise
The temperature of system is 30 DEG C, is then allowed to stand 23h and obtains mixed material；
S3, after filtering mixed material, distilled water and absolute ethyl alcohol is then used to wash to filtrate in colourless successively, 62 DEG C
Vacuum drying 23h obtains composite electromagnetic absorption material.
Embodiment 3
A kind of preparation method of composite electromagnetic absorption material proposed by the present invention, includes the following steps：
20g bismuth nitrates are weighed under S1, room temperature, grinding is uniform；1000ml ethylene glycol is measured as coating material and solvent,
And the bismuth nitrate after itself and grinding is mixed and is placed in 1000ml beakers, magnetic stick is added, is placed in constant temperature blender with magnetic force,
It is at the uniform velocity stirred for 24 hours with 100r/min, is then rotated, extra ethylene glycol is washed away with distilled water, be placed in vacuum in vacuum drying chamber
It is dry to obtain the bismuth nitrate for having hydroxyl modified to surface for 24 hours；
S2, the surfaces 1g are weighed there is the bismuth nitrate of hydroxyl modified to be dispersed in the 500ml aqueous solutions containing 0.4g valines
In, then 1.6g thiophene monomers are added in valine solution by ultrasonic 1h, and ultrasonic 1h is uniformly dispersed；Weigh 2.4g ammonium persulfates
It is dissolved in 100ml distilled water, after ultrasonic disperse is uniform, by ammonium persulfate aqueous solution under the at the uniform velocity agitation that magnetic stirs 50r/min
It is added drop-wise in reaction solution, rate of addition is 2 drops/s, and reaction temperature is controlled at 25 DEG C, after being added dropwise, continues to stand reaction for 24 hours
Obtain mixed material；
S3, it is filtered after mixed material is removed supernatant liquor, it is in nothing to be washed respectively to filtrate with distilled water and absolute ethyl alcohol
Color, then 60 DEG C of vacuum drying obtain composite electromagnetic absorption material for 24 hours in vacuum drying oven.
Embodiment 4
A kind of preparation method of composite electromagnetic absorption material proposed by the present invention, includes the following steps：
40g bismuth nitrates are weighed under S1, room temperature, grinding is uniform；1000ml ethylene glycol is measured as coating material and solvent,
And the bismuth nitrate after itself and grinding is mixed and is placed in 1000ml beakers, magnetic stick is added, is placed in constant temperature blender with magnetic force,
36h is at the uniform velocity stirred with 150r/min, is then rotated, extra ethylene glycol is washed away with distilled water, is placed in vacuum in vacuum drying chamber
It is dry to obtain the bismuth nitrate for having hydroxyl modified to surface for 24 hours；
S2, the surfaces 1g are weighed there is the bismuth nitrate of hydroxyl modified to be dispersed in the 500ml aqueous solutions containing 0.8g valines
In, then 2.4g thiophene monomers are added in valine solution by ultrasonic 1h, and ultrasonic 1h is uniformly dispersed；Weigh 3.0g ammonium persulfates
It is dissolved in 100ml distilled water, after ultrasonic disperse is uniform, by ammonium persulfate aqueous solution under the at the uniform velocity agitation that magnetic stirs 50r/min
It is added drop-wise in reaction solution, rate of addition is 2 drops/s, and reaction temperature is controlled at 25 DEG C, after being added dropwise, continues to stand reaction for 24 hours
Obtain mixed material.
S3, it is filtered after mixed material is removed supernatant liquor, it is in nothing to be washed respectively to filtrate with distilled water and absolute ethyl alcohol
Color, then 60 DEG C of vacuum drying obtain composite electromagnetic absorption material for 24 hours in vacuum drying oven.
Embodiment 5
A kind of preparation method of composite electromagnetic absorption material proposed by the present invention, includes the following steps：
60g bismuth nitrates are weighed under S1, room temperature, grinding is uniform；1000ml ethylene glycol is measured as coating material and solvent,
And the bismuth nitrate after itself and grinding is mixed and is placed in 1000ml beakers, magnetic stick is added, is placed in constant temperature blender with magnetic force,
48h is at the uniform velocity stirred with 200r/min, is then rotated, extra ethylene glycol is washed away with distilled water, is placed in vacuum in vacuum drying chamber
It is dry to obtain the bismuth nitrate for having hydroxyl modified to surface for 24 hours；
S2, the surfaces 1g are weighed there is the bismuth nitrate of hydroxyl modified to be dispersed in the 500ml aqueous solutions containing 1.2g valines
In, then 3.2g thiophene monomers are added in valine solution by ultrasonic 1h, and ultrasonic 1h is uniformly dispersed；Weigh 3.6g ammonium persulfates
It is dissolved in 100ml distilled water, after ultrasonic disperse is uniform, by ammonium persulfate aqueous solution under the at the uniform velocity agitation that magnetic stirs 50r/min
It is added drop-wise in reaction solution, rate of addition is 2 drops/s, and reaction temperature is controlled at 25 DEG C, after being added dropwise, continues to stand reaction for 24 hours
Obtain mixed material；
S3, it is filtered after mixed material is removed supernatant liquor, it is in nothing to be washed respectively to filtrate with distilled water and absolute ethyl alcohol
Color, then 60 DEG C of vacuum drying obtain composite electromagnetic absorption material for 24 hours in vacuum drying oven.
Embodiment 6
A kind of preparation method of composite electromagnetic absorption material proposed by the present invention, includes the following steps：
80g bismuth nitrates are weighed under S1, room temperature, grinding is uniform；1000ml ethylene glycol is measured as coating material and solvent,
And the bismuth nitrate after itself and grinding is mixed and is placed in 1000ml beakers, magnetic stick is added, is placed in constant temperature blender with magnetic force,
60h is at the uniform velocity stirred with 250r/min, is then rotated, extra ethylene glycol is washed away with distilled water, is placed in vacuum in vacuum drying chamber
It is dry to obtain the bismuth nitrate for having hydroxyl modified to surface for 24 hours；
S2, the surfaces 1g are weighed there is the bismuth nitrate of hydroxyl modified to be dispersed in the 500ml aqueous solutions containing 1.0g valines
In, then 4.0g thiophene monomers are added in valine solution by ultrasonic 1h, and ultrasonic 1h is uniformly dispersed；Weigh 4.2g ammonium persulfates
It is dissolved in 100ml distilled water, after ultrasonic disperse is uniform, by ammonium persulfate aqueous solution under the at the uniform velocity agitation that magnetic stirs 50r/min
It is added drop-wise in reaction solution, rate of addition is 2 drops/s, and reaction temperature is controlled at 25 DEG C, after being added dropwise, continues to stand reaction for 24 hours
Obtain mixed material；
S3, it is filtered after mixed material is removed supernatant liquor, it is in nothing to be washed respectively to filtrate with distilled water and absolute ethyl alcohol
Color, then 60 DEG C of vacuum drying obtain composite electromagnetic absorption material for 24 hours in vacuum drying oven.
Embodiment 7
A kind of preparation method of composite electromagnetic absorption material proposed by the present invention, includes the following steps：
100g bismuth nitrates are weighed under S1, room temperature, grinding is uniform；1000ml ethylene glycol is measured as coating material and molten
Agent, and the bismuth nitrate after itself and grinding is mixed and is placed in 1000ml beakers, magnetic stick is added, is placed in constant temperature blender with magnetic force
On, 72h is at the uniform velocity stirred with 300r/min, is then rotated, extra ethylene glycol is washed away with distilled water, is placed in vacuum drying chamber true
Sky is dry to obtain the bismuth nitrate for having hydroxyl modified to surface for 24 hours；
S2, the surfaces 1g are weighed there is the bismuth nitrate of hydroxyl modified to be dispersed in the 500ml aqueous solutions containing 1.2g valines
In, then 4.8g thiophene monomers are added in valine solution by ultrasonic 1h, and ultrasonic 1h is uniformly dispersed；Weigh 5.8g ammonium persulfates
It is dissolved in 100ml distilled water, after ultrasonic disperse is uniform, by ammonium persulfate aqueous solution under the at the uniform velocity agitation that magnetic stirs 50r/min
It is added drop-wise in reaction solution, rate of addition is 2 drops/s, and reaction temperature is controlled at 20-30 DEG C, after being added dropwise, continues to stand reaction
Mixed material is obtained for 24 hours；
S3, it is filtered after mixed material is removed supernatant liquor, it is in nothing to be washed respectively to filtrate with distilled water and absolute ethyl alcohol
Color, then 60 DEG C of vacuum drying obtain composite electromagnetic absorption material for 24 hours in vacuum drying oven.
Comparative example
S1,0.4g valines are scattered in 500ml aqueous solutions, ultrasonic 1h, figured silk fabrics ammonia then is added in 1.6g thiophene monomers
In acid solution, ultrasonic 1h；It weighs 2.4g ammonium persulfates to be dissolved in 100ml distilled water, after ultrasonic disperse is uniform, 50r/ is stirred in magnetic
Ammonium persulfate aqueous solution is added drop-wise in reaction solution under the at the uniform velocity agitation of min, rate of addition is 2 drops/s, and reaction temperature control exists
25 DEG C, after being added dropwise, continues standing reaction and obtain mixed material for 24 hours；
S2, it is filtered after mixed material is removed supernatant liquor, it is in nothing to be washed respectively to filtrate with distilled water and absolute ethyl alcohol
Color, then 60 DEG C of vacuum drying obtain polythiophene trepanning microballoon for 24 hours in vacuum drying oven.
Polythiophene trepanning microballoon obtained by 3 gained composite electromagnetic absorption material of embodiment and comparative example is carried out Electronic Speculum to sweep
It retouches, result is as depicted in figs. 1 and 2, and Fig. 1 is the scanning electron microscope (SEM) photograph of 3 gained composite electromagnetic absorption material of the embodiment of the present invention,
Fig. 2 is the scanning electron microscope (SEM) photograph of polythiophene trepanning microballoon obtained by comparative example；Referring to Figures 1 and 2, present invention gained composite electromagnetic is inhaled
It receives in material, on the bismuth nitrate surface of modified, easily slowly polymerization obtains the sheet polythiophene nanometer sheet of high molecular weight to thiophene, and
Polythiophene trepanning microballoon is mostly spherical obtained by comparative example, and electromagnetic wave receiving area bigger of the present invention is can be seen that from structure,
Higher is lost in reflection of electromagnetic wave, and electromaganic wave absorbing property is more preferable.
It is anti-that polythiophene trepanning microballoon obtained by 3 gained composite electromagnetic absorption material of embodiment and comparative example is subjected to electromagnetic wave
Loss detection is penetrated, result is as shown in Figure 3 and Figure 4, and Fig. 3 is the electricity of 3 gained composite electromagnetic absorption material of the embodiment of the present invention
Magnetic wave reflection loss curve, Fig. 4 are the reflection of electromagnetic wave damage curve of polythiophene trepanning microballoon obtained by comparative example；With reference to Fig. 3 and
Fig. 4, present invention gained composite electromagnetic absorption material increase effectively electromagnetic wave receiving area, are opened than polythiophene obtained by comparative example
Hole microballoon is lost with higher reflection of electromagnetic wave.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (13)
1. a kind of preparation method of composite electromagnetic absorption material, which is characterized in that include the following steps：
S1, bismuth nitrate is added in ethylene glycol and is stirred, then recrystallized, washed, being dried to obtain surface has hydroxyl modified
Bismuth nitrate；
S2, surface is had hydroxyl modified bismuth nitrate be added valine aqueous solution in once disperseed, add thiophene monomer
Twice dispersing is carried out, is then stirred, ammonium persulfate aqueous solution is added dropwise in whipping process, be then allowed to stand to obtain mixed material；
S3, it after filtering mixed material, washs, vacuum drying obtains composite electromagnetic absorption material.
2. the preparation method of composite electromagnetic absorption material according to claim 1, which is characterized in that in S1, bismuth nitrate and
The mass volume ratio (g/mL) of ethylene glycol is 20~100：1000.
3. the preparation method of composite electromagnetic absorption material according to claim 1, which is characterized in that in S1, stirring when
Between be 24~72h.
4. the preparation method of composite electromagnetic absorption material according to claim 1, which is characterized in that in S1, the speed of stirring
Degree is 100~300rpm.
5. the preparation method of composite electromagnetic absorption material according to claim 1, which is characterized in that in S2, bismuth nitrate, thiophene
The mass ratio of thiophene monomer, valine and ammonium persulfate is 1：1.6~4.8：0.4~1.2：2.4~5.8.
6. the preparation method of composite electromagnetic absorption material according to claim 1, which is characterized in that in S2, using ultrasound
Disperseed, the time of primary dispersion and twice dispersing is 0.8~1.2h.
7. the preparation method of composite electromagnetic absorption material according to claim 1, which is characterized in that in S2, the speed of stirring
Degree is 45~55rpm.
8. the preparation method of composite electromagnetic absorption material according to claim 1, which is characterized in that in S2, ammonium persulfate
The rate of addition of aqueous solution is 1~2.5 drop/s.
9. the preparation method of composite electromagnetic absorption material according to claim 1, which is characterized in that in S2, ammonium persulfate
It is 20~30 DEG C that the temperature of solution system is maintained during the dropwise addition of aqueous solution.
10. the preparation method of composite electromagnetic absorption material according to claim 1, which is characterized in that in S2, time of repose
For 23~25h.
11. the preparation method of composite electromagnetic absorption material according to claim 1, which is characterized in that in S3, vacuum drying
Temperature be 58~62 DEG C, the vacuum drying time be 23~25h.
12. the preparation method of composite electromagnetic absorption material according to claim 1, which is characterized in that in S3, the tool of washing
Gymnastics is made as follows：Obtained solid material will be filtered uses distilled water and absolute ethyl alcohol to wash to filtrate in colourless successively.
13. a kind of preparation method of the composite electromagnetic absorption material as described in claim any one of 1-12 is prepared compound
Electromagnetic wave absorbent material.
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| CN101585959A (en) * | 2008-05-21 | 2009-11-25 | 中国科学院理化技术研究所 | Conductive polymer wave-absorbing material |
| CN102634169A (en) * | 2011-02-15 | 2012-08-15 | 中国科学院理化技术研究所 | Magnetic material and conductive polymer composite wave-absorbing material and preparation method thereof |
| CN104031357A (en) * | 2014-05-26 | 2014-09-10 | 中国科学院理化技术研究所 | Conductive polymer wave-absorbing material with double-shell structure and preparation method thereof |
| CN104592514A (en) * | 2015-01-07 | 2015-05-06 | 合肥师范学院 | Preparation method of polypyrrole/carbon fiber composite electromagnetic wave absorbing material |
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| JP6546717B2 (en) * | 2012-09-20 | 2019-07-17 | Jsr株式会社 | Electromagnetic wave absorbing composition and electromagnetic wave absorber |
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| CN104031357A (en) * | 2014-05-26 | 2014-09-10 | 中国科学院理化技术研究所 | Conductive polymer wave-absorbing material with double-shell structure and preparation method thereof |
| CN104592514A (en) * | 2015-01-07 | 2015-05-06 | 合肥师范学院 | Preparation method of polypyrrole/carbon fiber composite electromagnetic wave absorbing material |
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| 《高分子热电材料研究进展》;赵敬红，胡楠，赵丽娟，李权;《塑料工业》;20140831;第42卷(第8期);全文 * |
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