CN103113580A - Preparation method of coaxial cable structure MWCNT/Fe3O4/ZnO/PANI microwave absorbant - Google Patents
Preparation method of coaxial cable structure MWCNT/Fe3O4/ZnO/PANI microwave absorbant Download PDFInfo
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Abstract
The invention provides a preparation method of a coaxial cable structure MWCNT/Fe3O4/ZnO/PANI microwave absorbant, and relates to a preparation method of a microwave absorbent, and the method is used for solving the problems that the wave absorption material prepared by adopting the existing method is limited into binary and ternary, and is bad in binding force with matrixes to cause poor wave absorption effect. The preparation method comprises the steps: I preparing an MWCNT/Fe3O4 nanomaterial; II preparing MWCNT/Fe3O4/ZnO composite powder; III preparing compound water solution; and IV preparing ammonium persulfate aqueous solution, then dropwise adding into the composite aqueous solution, performing constant-temperature reaction under the condition of 0-25 DEG C, then performing magnetic separation, collecting solid phase matters, and drying to obtain the coaxial cable structure MWCNT/Fe3O4/ZnO/PANI microwave absorbant, thereby completing the preparation method. The preparation method is applied in the field of microwave absorption materials.
Description
Technical field
The present invention relates to a kind of preparation method of microwave absorption.
Background technology
Due to the develop rapidly of science and technology in recent years, the high-tech electronic product is when improving the human lives, follow the electromagnetic radiation of its generation also human body health to be brought serious harm, the research aspect civilian also comes into one's own day by day so absorbing material is at visual broadcasting, electron device and microwave radiation protecting etc.In addition, along with the modern times are surveyed and the development of guidance technology, the weapon viability faces a severe test, and is the needs that adapt to modern war, and the suction wave technology that the reduction weaponry is found probability becomes rapidly the study hotspot of countries in the world.
Present microwave absorbing material can be divided into electrical loss type and magnetic loss type by loss mechanism.For electrical loss type absorbing material, electromagnetic energy mainly decays in the resistance of material and the loss of dielectric depolarization relaxation, and this absorbing material comprises conductive polymer polymkeric substance, graphite, silicon carbide etc.Magnetic loss type absorbing material comprises ferrite, iron carbonyl, polycrystalline iron fiber etc., and its wave-absorbing mechanism is mainly magnetic hysteresis loss and ferro resonance loss.But existing absorbing material is only limited to binary and ternary, and good not with basal body binding force, and wave-absorbing effect is difficult to reach application conditions.
Summary of the invention
The present invention will solve the absorbing material of existing method preparation owing to being only limited to binary and ternary, good not with basal body binding force, and cause the bad problem of wave-absorbing effect, a kind of preparation method of coaxial cable structure MWCNT/Fe3O4/ZnO/PANI microwave absorption is provided.
A kind of coaxial cable structure MWCNT/Fe of the present invention
3O
4The preparation method of/ZnO/PANI microwave absorption carries out: one, respectively multi-walled carbon nano-tubes, ferric acetyl acetonade and triglycol are carried out ultra-sonic dispersion, then mix according to the following steps; Then be heated to boiling at nitrogen under as the protective atmosphere condition, after reaction 20～60min, carry out magnetic and separate, collect solid formation, drier, obtain MWCNT/Fe
3O
4Nano material; Wherein the mass ratio of multi-walled carbon nano-tubes and ferric acetyl acetonade is 1: (2～8), and multi-walled carbon nano-tubes and triglycol mass volume ratio are 1mg: (0.1mL～1mL);
Two, the MWCNT/Fe that respectively step 2 is obtained
3O
4Nano material, zinc acetate and triglycol carry out ultra-sonic dispersion, then mix, and then are heated to boiling at nitrogen under as the protective atmosphere condition, after reaction 20～60min, carry out magnetic and separate, and collect solid formation, drier, obtain MWCNT/Fe
3O
4/ ZnO composite granule; MWCNT/Fe wherein
3O
4The mass ratio of nano material and zinc acetate is 1: (2～8), MWCNT/Fe
3O
4The mass volume ratio of nano material and triglycol is 1mg: (0.1mL～1mL);
Three, with MWCNT/Fe
3O
4/ ZnO composite granule is dissolved in ultrapure water, ultra-sonic dispersion 10～20min then, then add aniline under the condition that stirs, and then stir 8～20min, obtain compound water solution; MWCNT/Fe wherein
3O
4The mass volume ratio of/ZnO composite granule and aniline is 1mg: (0.0001mL～0.002mL);
Four, taking ammonium persulphate is dissolved in ultrapure water, obtain ammonium persulfate aqueous solution, then be under the condition of 0.05-0.5mL/s in drop rate, ammonium persulfate aqueous solution is added drop-wise in compound water solution, isothermal reaction 2～10h under the condition of 0～25 ℃, then carry out magnetic and separate again, collects solid formation, carry out again drying, obtain coaxial cable structure MWCNT/Fe
3O
4/ ZnO/PANI microwave absorption is namely completed coaxial cable structure MWCNT/Fe
3O
4The preparation method of/ZnO/PANI microwave absorption; MWCNT/Fe wherein
3O
4/ ZnO composite granule and ammonium persulphate mass ratio are 1: (0.5～2); The mass volume ratio of ammonium persulphate and ultrapure water is (0.01g～0.04g): 1mL.
The present invention comprises following beneficial effect:
When absorbing material with dielectric materials and magneticsubstance nanoscale in conjunction with the time, can greatly improve the microwave absorbing property of material; In addition, in many interface systems, because the reinforcement of interfacial polarization effect also can improve the absorbing property of material greatly, the present invention is quaternary coupling system, and the more interfacial polarizations of component are stronger, can strengthen the microwave absorbing effect; The dispersed interface binding power of powder absorbing material and binding agent is bad, is one layer of polymeric at the outermost layer of coaxial cable structure, and interface junction is closed better.The coaxial cable structure MWCNT/Fe of the present invention's preparation
3O
4/ ZnO/PANI microwave absorption adopts multi-walled carbon nano-tubes as the innermost layer component, has good mechanical property, can guarantee the mechanical property of material; Then magneticsubstance Fe
3O
4Assemble in situ forms the coupling of dielectric and magnetic in carbon nano tube surface; Inferior skin carries out the ZnO involucrum to be processed, and makes semi-conductor ZnO shell can optimize interface structure and strengthens absorption; Outermost layer is dielectric loss absorbing material polyaniline (PANI), it is for conductive polymers and can make the combination at interface better, because the powder absorbing material will be dispersed in epoxy resin and use, polyaniline as outermost layer can with the good combination of epoxy resin, solve the powder absorbing material problem bad with binding agent dispersiveness interface binding power in the past.Four kinds of materials play a role separately and are coupled, and strengthen absorption of electromagnetic wave.
Description of drawings
Fig. 1 is the coaxial cable structure MWCNT/Fe of this test preparation
3O
4The TEM figure of/ZnO/PANI microwave absorption;
Fig. 2 is the coaxial cable structure MWCNT/Fe of this test preparation
3O
4The EDS of/ZnO/PANI microwave absorption can spectrogram.
Embodiment
Embodiment one: a kind of coaxial cable structure MWCNT/Fe of present embodiment
3O
4The preparation method of/ZnO/PANI microwave absorption carries out: one, respectively multi-walled carbon nano-tubes, ferric acetyl acetonade and triglycol are carried out ultra-sonic dispersion, then mix according to the following steps; Then be heated to boiling at nitrogen under as the protective atmosphere condition, after reaction 20～60min, carry out magnetic and separate, collect solid formation, drier, obtain MWCNT/Fe
3O
4Nano material; Wherein the mass ratio of multi-walled carbon nano-tubes and ferric acetyl acetonade is 1: (2～8), and multi-walled carbon nano-tubes and triglycol mass volume ratio are 1mg: (0.1mL～1mL);
Two, the MWCNT/Fe that respectively step 2 is obtained
3O
4Nano material, zinc acetate and triglycol carry out ultra-sonic dispersion, then mix, and then are heated to boiling at nitrogen under as the protective atmosphere condition, after reaction 20～60min, carry out magnetic and separate, and collect solid formation, drier, obtain MWCNT/Fe
3O
4/ ZnO composite granule; MWCNT/Fe wherein
3O
4The mass ratio of nano material and zinc acetate is 1: (2～8), MWCNT/Fe
3O
4The mass volume ratio of nano material and triglycol is 1mg: (0.1mL～1mL);
Three, with MWCNT/Fe
3O
4/ ZnO composite granule is dissolved in ultrapure water, ultra-sonic dispersion 10～20min then, then add aniline under the condition that stirs, and then stir 8～20min, obtain compound water solution; MWCNT/Fe wherein
3O
4The mass volume ratio of/ZnO composite granule and aniline is 1mg: (0.0001mL～0.002mL);
Four, taking ammonium persulphate is dissolved in ultrapure water, obtain ammonium persulfate aqueous solution, then be under the condition of 0.05-0.5mL/s in drop rate, ammonium persulfate aqueous solution is added drop-wise in compound water solution, isothermal reaction 2～10h under the condition of 0～25 ℃, then carry out magnetic and separate again, collects solid formation, carry out again drying, obtain coaxial cable structure MWCNT/Fe
3O
4/ ZnO/PANI microwave absorption is namely completed coaxial cable structure MWCNT/Fe
3O
4The preparation method of/ZnO/PANI microwave absorption; MWCNT/Fe wherein
3O
4/ ZnO composite granule and ammonium persulphate mass ratio are 1: (0.5～2); The mass volume ratio of ammonium persulphate and ultrapure water is (0.01g～0.04g): 1mL.
When absorbing material with dielectric materials and magneticsubstance nanoscale in conjunction with the time, can greatly improve the microwave absorbing property of material; In addition, in many interface systems, because the reinforcement of interfacial polarization effect also can improve the absorbing property of material greatly, present embodiment is quaternary coupling system, and the more interfacial polarizations of component are stronger, can strengthen the microwave absorbing effect; The dispersed interface binding power of powder absorbing material and binding agent is bad, is one layer of polymeric at the outermost layer of coaxial cable structure, and interface junction is closed better.The coaxial cable structure MWCNT/Fe of present embodiment preparation
3O
4/ ZnO/PANI microwave absorption adopts multi-walled carbon nano-tubes as the innermost layer component, has good mechanical property, can guarantee the mechanical property of material; Then magneticsubstance Fe
3O
4Assemble in situ forms the coupling of dielectric and magnetic in carbon nano tube surface; Inferior skin carries out the ZnO involucrum to be processed, and makes semi-conductor ZnO shell can optimize interface structure and strengthens absorption; Outermost layer is dielectric loss absorbing material polyaniline (PANI), it is for conductive polymers and can make the combination at interface better, because the powder absorbing material will be dispersed in epoxy resin and use, polyaniline as outermost layer can with the good combination of epoxy resin, solve the powder absorbing material problem bad with binding agent dispersiveness interface binding power in the past.Four kinds of materials play a role separately and are coupled together, and strengthen electromagnetic absorption.
Embodiment two: present embodiment is different from embodiment one is that multi-walled carbon nano-tubes diameter in step 1 is 30～60nm, and length is 5～25 μ m.Other steps and parameter are identical with embodiment one.
Embodiment three: that present embodiment is different from embodiment one or two is the MWCNT/Fe that step 1 obtains
3O
4Fe in nano material
3O
4The thickness of layer is 2～8nm.Other steps and parameter are identical with embodiment one or two.
Embodiment four: what present embodiment was different from one of embodiment one to three is that the speed that heats in step 1 and step 2 is 4 ℃/min.Other steps and parameter are identical with one of embodiment one to three.
Embodiment five: that present embodiment is different from one of embodiment one to four is the MWCNT/Fe that step 2 obtains
3O
4In/ZnO composite granule, the ZnO layer thickness is 1～7nm.Other steps and parameter are identical with one of embodiment one to four.
Embodiment six: that present embodiment is different from one of embodiment one to five is the coaxial cable structure MWCNT/Fe that step 4 obtains
3O
4In/ZnO/PANI microwave absorption, the PANI layer thickness is 5～30nm.Other steps and parameter are identical with one of embodiment one to five.
Embodiment seven: present embodiment is different from one of embodiment one to six is that magnetic in step 1, two and four is separated into and uses the absorption of superparamagnetic iron, then wash 2～3 times, dehydrated alcohol is washed 2～3 times again.Other steps and parameter are identical with one of embodiment one to six.
Embodiment eight: present embodiment is different from one of embodiment one to seven is that drying in step 1, two and four is for dry under the condition of 30 ℃～40 ℃.Other steps and parameter are identical with one of embodiment one to seven.
By following verification experimental verification beneficial effect of the present invention:
Test 1: a kind of coaxial cable structure MWCNT/Fe of the present invention
3O
4The preparation method of/ZnO/PANI microwave absorption carries out: one, respectively 100mg multi-walled carbon nano-tubes, 400mg ferric acetyl acetonade and 25mL triglycol are carried out ultra-sonic dispersion 10min, then mix according to the following steps; Then pass into N
2As protective atmosphere, be that 4 ℃/min is heated to boiling according to speed after 5min, after reaction 40min, carry out magnetic and separate, collect solid formation, drier under the condition of 30 ℃～40 ℃, obtain MWCNT/Fe
3O
4Nano material;
Two, the MWCNT/Fe that respectively the 100mg step 2 is obtained
3O
4Nano material, 400mg zinc acetate and 25mL triglycol carry out ultra-sonic dispersion 10min, then mix, more logical N
2As protective atmosphere, be that 4 ℃/min is heated to boiling according to speed after 5min, after reaction 40min, carry out magnetic and separate, collect solid formation, drier under the condition of 30 ℃～40 ℃, obtain MWCNT/Fe
3O
4/ ZnO composite granule;
Three, with 50mgMWCNT/Fe
3O
4/ ZnO composite granule is dissolved in the 25mL ultrapure water, ultra-sonic dispersion 15min then, then add 0.04mL aniline under the condition that stirs, and then stir 10min, obtain compound water solution;
Four, taking the 0.092g ammonium persulphate is dissolved in the 5mL ultrapure water, obtain ammonium persulfate aqueous solution, then in being added drop-wise to compound water solution under drop rate is the condition of 0.05-0.5mL/s, isothermal reaction 6h under the condition of 4 ℃ again, then carrying out magnetic separates, collect solid formation, drier under the condition of 30 ℃～40 ℃, obtain coaxial cable structure MWCNT/Fe
3O
4/ ZnO/PANI microwave absorption is namely completed coaxial cable structure MWCNT/Fe
3O
4The preparation method of/ZnO/PANI microwave absorption.
Fig. 1 is the coaxial cable structure MWCNT/Fe of this test preparation
3O
4The TEM figure of/ZnO/PANI microwave absorption, as can be seen from the figure the PANI covered effect is good, without the particle obscission.
Fig. 2 is the coaxial cable structure MWCNT/Fe of this test preparation
3O
4The EDS energy spectrogram of/ZnO/PANI microwave absorption, Fig. 2 ordinate zou photoelectron number is per second counting in unit energy, as can be seen from the figure, in sample, the content of nitrogen is up to 28.28%, and only have polyaniline to contain the nitrogen element in system, this has further proved by this kind method, can realize that polyaniline is to the coating of mixture.
The coaxial cable structure MWCNT/Fe of this test preparation
3O
4/ ZnO/PANI microwave absorption adopts multi-walled carbon nano-tubes as the innermost layer component, has good mechanical property, can guarantee the mechanical property of material; Then magneticsubstance Fe
3O
4Assemble in situ forms the coupling of dielectric and magnetic in carbon nano tube surface; Inferior skin carries out the ZnO involucrum to be processed, and makes semi-conductor ZnO shell can optimize interface structure and strengthens absorption; Outermost layer is dielectric loss absorbing material polyaniline (PANI), it is for conductive polymers and can make the combination at interface better, because the powder absorbing material will be dispersed in epoxy resin and use, polyaniline as outermost layer can with the good combination of epoxy resin, solve the powder absorbing material problem bad with binding agent dispersiveness interface binding power in the past.Four kinds of materials play a role separately and are coupled together, and strengthen electromagnetic absorption.
Claims (8)
1. coaxial cable structure MWCNT/Fe
3O
4The preparation method of/ZnO/PANI microwave absorption is characterized in that coaxial cable structure MWCNT/Fe
3O
4The preparation method of/ZnO/PANI microwave absorption carries out according to the following steps: one, respectively multi-walled carbon nano-tubes, ferric acetyl acetonade and triglycol are carried out ultra-sonic dispersion, then mix; Then be heated to boiling at nitrogen under as the protective atmosphere condition, after reaction 20～60min, carry out magnetic and separate, collect solid formation, drier, obtain MWCNT/Fe
3O
4Nano material; Wherein the mass ratio of multi-walled carbon nano-tubes and ferric acetyl acetonade is 1: (2～8), and multi-walled carbon nano-tubes and triglycol mass volume ratio are 1mg: (0.1mL～1mL);
Two, the MWCNT/Fe that respectively step 2 is obtained
3O
4Nano material, zinc acetate and triglycol carry out ultra-sonic dispersion, then mix, and then are heated to boiling at nitrogen under as the protective atmosphere condition, after reaction 20～60min, carry out magnetic and separate, and collect solid formation, drier, obtain MWCNT/Fe
3O
4/ ZnO composite granule; MWCNT/Fe wherein
3O
4The mass ratio of nano material and zinc acetate is 1: (2～8), MWCNT/Fe
3O
4The mass volume ratio of nano material and triglycol is 1mg: (0.1mL～1mL);
Three, with MWCNT/Fe
3O
4/ ZnO composite granule is dissolved in ultrapure water, ultra-sonic dispersion 10～20min then, then add aniline under the condition that stirs, and then stir 8～20min, obtain compound water solution; MWCNT/Fe wherein
3O
4The mass volume ratio of/ZnO composite granule and aniline is 1mg: (0.0001mL～0.002mL);
Four, taking ammonium persulphate is dissolved in ultrapure water, obtain ammonium persulfate aqueous solution, then be under the condition of 0.05-0.5mL/s in drop rate, ammonium persulfate aqueous solution is added drop-wise in compound water solution, isothermal reaction 2～10h under the condition of 0～25 ℃, then carry out magnetic and separate again, collects solid formation, carry out again drying, obtain coaxial cable structure MWCNT/Fe
3O
4/ ZnO/PANI microwave absorption is namely completed coaxial cable structure MWCNT/Fe
3O
4The preparation method of/ZnO/PANI microwave absorption; MWCNT/Fe wherein
3O
4/ ZnO composite granule and ammonium persulphate mass ratio are 1: (0.5～2); The mass volume ratio of ammonium persulphate and ultrapure water is (0.01g～0.04g): 1mL.
2. a kind of coaxial cable structure MWCNT/Fe according to claim 1
3O
4The preparation method of/ZnO/PANI microwave absorption is characterized in that the multi-walled carbon nano-tubes diameter in step 1 is 30～60nm, and length is 5～25 μ m.
3. a kind of coaxial cable structure MWCNT/Fe according to claim 1
3O
4The preparation method of/ZnO/PANI microwave absorption is characterized in that the MWCNT/Fe that step 1 obtains
3O
4Fe in nano material
3O
4The thickness of layer is 2～8nm.
4. a kind of coaxial cable structure MWCNT/Fe according to claim 1
3O
4The preparation method of/ZnO/PANI microwave absorption is characterized in that the speed that heats in step 1 and step 2 is 4 ℃/min.
5. a kind of coaxial cable structure MWCNT/Fe according to claim 1
3O
4The preparation method of/ZnO/PANI microwave absorption is characterized in that the MWCNT/Fe that step 2 obtains
3O
4In/ZnO composite granule, the ZnO layer thickness is 1～7nm.
6. a kind of coaxial cable structure MWCNT/Fe according to claim 1
3O
4The preparation method of/ZnO/PANI microwave absorption is characterized in that the coaxial cable structure MWCNT/Fe that step 4 obtains
3O
4In/ZnO/PANI microwave absorption, the PANI layer thickness is 5～30nm.
7. a kind of coaxial cable structure MWCNT/Fe according to claim 1
3O
4The preparation method of/ZnO/PANI microwave absorption is characterized in that magnetic in step 1, two and four is separated into to use the absorption of superparamagnetic iron, then wash 2～3 times, dehydrated alcohol is washed 2～3 times again.
8. a kind of coaxial cable structure MWCNT/Fe according to claim 1
3O
4The preparation method of/ZnO/PANI microwave absorption is characterized in that the drying in step 1, two and four is drying under the condition of 30 ℃～40 ℃.
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| CN103342980A (en) * | 2013-06-26 | 2013-10-09 | 哈尔滨工业大学 | Preparation method for MWCNT/Fe3O4/PANI/Au multilayer wrapped nanotube |
| CN105273689A (en) * | 2014-07-18 | 2016-01-27 | 广东工业大学 | Novel multi-element structure composite conductive filling material |
| WO2018157400A1 (en) * | 2017-03-03 | 2018-09-07 | 深圳市佩成科技有限责任公司 | Preparation method for pani/fe3o4/mwcnts-paraffin composite material |
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| CN110724493A (en) * | 2019-09-29 | 2020-01-24 | 安徽理工大学 | Multi-walled carbon nanotube/ferroferric oxide/nano oxide hybrid wave-absorbing material and preparation method thereof |
| CN114801381A (en) * | 2022-03-29 | 2022-07-29 | 四川盈乐威科技有限公司 | Multilayer wave-absorbing material and preparation method thereof |
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| CN103342980A (en) * | 2013-06-26 | 2013-10-09 | 哈尔滨工业大学 | Preparation method for MWCNT/Fe3O4/PANI/Au multilayer wrapped nanotube |
| CN105273689A (en) * | 2014-07-18 | 2016-01-27 | 广东工业大学 | Novel multi-element structure composite conductive filling material |
| WO2018157400A1 (en) * | 2017-03-03 | 2018-09-07 | 深圳市佩成科技有限责任公司 | Preparation method for pani/fe3o4/mwcnts-paraffin composite material |
| WO2018157399A1 (en) * | 2017-03-03 | 2018-09-07 | 深圳市佩成科技有限责任公司 | Preparation method for fe3o4/mwcnts-paraffin composite material |
| CN110724493A (en) * | 2019-09-29 | 2020-01-24 | 安徽理工大学 | Multi-walled carbon nanotube/ferroferric oxide/nano oxide hybrid wave-absorbing material and preparation method thereof |
| CN110724493B (en) * | 2019-09-29 | 2022-11-18 | 安徽理工大学 | Multi-walled carbon nanotube/ferroferric oxide/nano oxide hybrid wave-absorbing material and preparation method thereof |
| CN114801381A (en) * | 2022-03-29 | 2022-07-29 | 四川盈乐威科技有限公司 | Multilayer wave-absorbing material and preparation method thereof |
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