CN102936339A - Polypyrrole/ferrite/multi-wall carbon nanotube composite material preparation method - Google Patents
Polypyrrole/ferrite/multi-wall carbon nanotube composite material preparation method Download PDFInfo
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- CN102936339A CN102936339A CN2012103948632A CN201210394863A CN102936339A CN 102936339 A CN102936339 A CN 102936339A CN 2012103948632 A CN2012103948632 A CN 2012103948632A CN 201210394863 A CN201210394863 A CN 201210394863A CN 102936339 A CN102936339 A CN 102936339A
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Abstract
The present invention relates to a polypyrrole/ferrite/multi-wall carbon nanotube composite material preparation method, which comprises adopting a sol-gel method to prepare a BaFe12O19-Ni0.8Zn0.2Fe2O4 material, and then adopting an in situ polymerization method to prepare the polypyrrole/ferrite/multi-wall carbon nanotube composite material. According to the prepared polypyrrole/BaFe12O19-Ni0.8Zn0.2Fe2O4/multi-wall carbon nanotube composite material, polypyrrole, a carrier multi-wall carbon nanotube with characteristics of large specific surface area, good electrical conductivity, good dispersion and stable performance, and a hard magnetic and soft magnetic composite material BaFe12O19-Ni0.8Zn0.2Fe2O are compounded to increase a wave absorption performance of the material, wherein the polypyrrole adopted as the wave absorption material has advantages of low specific gravity, good compatibility and good electrical conductivity; and a chemical oxidation method is adopted to carry out polypyrrole in situ polymerization on the surface of the different amounts of the BaFe12O19-Ni0.8Zn0.2Fe2O4/multi-wall carbon nanotubes so as to achieve adjustable electromagnetic parameters, such that important significances are provided for widening of composite material microwave absorption frequency bands and preparation of novel wave absorption materials.
Description
Technical field
The invention belongs to the preparation method of ferrite composite wave-suction material, be specifically related to the preparation method of a kind of polypyrrole/ferrite/multi-wall carbon nano-tube composite material, be specially a kind of ferrite, conduction high polymer, carbon nano tube compound material---polypyrrole/BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4The preparation method of/multi-wall carbon nano-tube composite material.
Background technology
Microwave absorbing material has wide application background at commercial and military aspect.Development structure is stable, bandwidth, specific absorption are high, low density novel wave-absorbing material is the nowadays key point in electromagnetic absorption field.Normally used microwave absorbing material comprises ferrite, conduction high polymer, carbon nanomaterial etc.Ferrite such as Z 250, barium ferrite, although nickel-zinc ferrite etc. have higher saturation magnetization and magnetic loss, its density is large, dielectric loss is low, has greatly limited being widely used of it.Conduction high polymer such as polyaniline, polypyrrole, polyphenylacetylene etc. since being found, just because the structure of their uniquenesses, good electroconductibility, potential functionalization prospect and receiving much concern.Such as carbon nanotube and Graphene, high specific surface area is arranged in the carbon nanomaterial, special electronic conduction mode, satisfactory stability are the ideal choses of solid support material.Conduction high polymer and carbon nanomaterial are mainly the electrical loss material when being used for microwave absorbing, if can form electricity, magnetic loss shaped material with the magnetic particle compound, and obtain stable, efficient absorbing property.Document " " Applied surface science ", 259 (2012) pp.486-493 " has openly adopted situ aggregation method to synthesize PPy-BaFe
12O
19/ Ni
0.8Zn
0.2Fe
2O
4Nano composite material.By the analysis of vector network instrument, it is inhaled ripple and is lost in the I of 10.7GHz and reaches-21.5dB.
But, the PPy-BaFe for preparing in the document
12O
19/ Ni
0.8Zn
0.2Fe
2O
4Has following deficiency: inhale ripple loss less (being that absorbing property is not good enough) at 8.2-12.4GHz, this is because the specific conductivity of matrix material is lower, electrical loss is less, and by adding 5% carbon nanotube, its suction ripple is lost in 8.9GHz and can reaches-25.46dB, has improved preferably its absorbing property.This is because the adding of carbon nanotube can increase the specific conductivity of matrix material, can form polaron when the main chain oxidation, and the position of polaron in molecule can displacement under the effect of electromagnetic field, thereby forms conductive current.Because the vibration of electromagnetic field forms eddy current at the conductive network of composite inner, electric energy conversion is that heat energy loses, thereby has increased electrical loss, has improved absorbing property.
Summary of the invention
The technical problem that solves
For fear of the deficiencies in the prior art part, the present invention proposes the preparation method of a kind of polypyrrole/ferrite/multi-wall carbon nano-tube composite material, at first adopts sol-gel method to prepare BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4Material adopts situ aggregation method to prepare polypyrrole/BaFe then
12O
19-Ni
0.8Zn
0.2Fe
2O
4/ multi-wall carbon nano-tube composite material.
Technical scheme
The preparation method of a kind of polypyrrole/ferrite/multi-wall carbon nano-tube composite material is characterized in that step is as follows:
Step 1 adopts sol-gel method to prepare BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4Ferrite powder: be the citric acid of 217:76:4:1:6 with mol ratio, iron nitrate, nickelous nitrate, zinc nitrate and nitrate of baryta are dissolved in the deionized water, and the room temperature lower magnetic force stirs; Then the ethylene glycol that with mol ratio is 2 times of citric acids joins in the solution, and regulates pH to 7 with quadrol; Under the magnetic agitation, gained solution is heated to 75-80 ℃, transpiring moisture is to gel formation; With gel dry 12-36h in 120-140 ℃ baking oven at first, be transferred to then that calcining obtains BaFe in the retort furnace
12O
19-Ni
0.8Zn
0.2Fe
2O
4Ferrite powder;
Step 2 pair multi-walled carbon nano-tubes is processed: multi-walled carbon nano-tubes at 550-650 ℃ of tubular type kiln roasting 2-2.5h, then is transferred in the mixed solution of sulfuric acid and nitric acid and reacts 4-5h; By centrifugal or filter to isolate multi-walled carbon nano-tubes after, with deionized water wash; At the dry 12-36h of 50-60 ℃ vacuum drying oven, obtain carboxylated multi-walled carbon nano-tubes at last, the sulfuric acid of described mixed solution and the volume ratio of nitric acid are 3:1;
Step 3 original position is synthesized polypyrrole/BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4/ multi-wall carbon nano-tube composite material: be pyrrole monomer, the BaFe of 2:1:0.05-3 with mass ratio
12O
19-Ni
0.8Zn
0.2Fe
2O
4Join in the deionized water with multi-walled carbon nano-tubes, after ultra-sonic dispersion is complete, add FeCl
36H
2The aqueous solution of O carries out oxypolymerization; Be transferred to 50-60 ℃ the dry 12-36h of vacuum drying oven behind the precipitation repetitive scrubbing that the gained mixed solution obtains after filtration, obtain polypyrrole/BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4/ multi-wall carbon nano-tube composite material; FeCl in the aqueous solution of described FeCl36H2O
36H
2O and pyrroles's mol ratio is 2.33:1.
Beneficial effect
The preparation method of a kind of polypyrrole/ferrite that the present invention proposes/multi-wall carbon nano-tube composite material, the polypyrrole/BaFe of preparation
12O
19-Ni
0.8Zn
0.2Fe
2O
4/ multi-wall carbon nano-tube composite material is with polypyrrole and the carrier multi-walled carbon nano-tubes with bigger serface, satisfactory electrical conductivity and dispersiveness and stable performance and hard, soft-magnetic composite material BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O is compound, to improve the absorbing property of material.Polypyrrole has the advantage of little, compatible good, the good conductivity of proportion as absorbing material.Adopt chemical oxidization method, at the BaFe of difference amount
12O
19-Ni
0.8Zn
0.2Fe
2O
4/ multi-walled carbon nano-tubes in situ Polymerization polypyrrole realizes that electromagnetic parameter is adjustable, for widen the Composite Microwave absorption band, the preparation novel wave-absorbing material significant.
The invention has the beneficial effects as follows: adopt situ aggregation method to prepare polypyrrole/BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4/ multi-walled carbon nano-tubes composite wave-suction material.But the polypyrrole well loaded is in multi-walled carbon nano-tubes and BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4The surface participates in microwave absorbing; Polypyrrole/BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4/ multi-walled carbon nano-tubes composite wave-suction material has good absorbing property.
Description of drawings
Fig. 1 is polypyrrole/BaFe among the embodiment 2
12O
19-Ni
0.8Zn
0.2Fe
2O
4/ multi-walled carbon nano-tubes XRD figure;
Polypyrrole/BaFe among Fig. 2 embodiment 2
12O
19-Ni
0.8Zn
0.2Fe
2O
4/ multi-walled carbon nano-tubes TEM figure
Polypyrrole/BaFe among Fig. 3 embodiment 2
12O
19-Ni
0.8Zn
0.2Fe
2O
4/ multi-walled carbon nano-tubes reflection loss curve.
Embodiment
Now in conjunction with the embodiments, the invention will be further described for accompanying drawing:
Embodiment 1:
(1) BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4Preparation:
(a) with mol ratio be the citric acid of 217:76:4:1:6, iron nitrate, nickelous nitrate, zinc nitrate, nitrate of baryta are dissolved in the deionized water, and the room temperature lower magnetic force stirs;
(b) be that the ethylene glycol of 2 times of citric acids joins in the solution with mol ratio, then regulate pH to 7 with quadrol;
(c) under the magnetic agitation, gained solution is heated to 75 ℃, transpiring moisture is to gel formation;
(d) with gel dry 24h in 120 ℃ baking oven at first, then be transferred to 400 ℃ retort furnace presintering 3h, at 1100 ℃ of lower calcining 2h, obtain BaFe at last
12O
19-Ni
0.8Zn
0.2Fe
2O
4Ferrite powder.
(2) multi-walled carbon nano-tubes is processed:
(a) with multi-walled carbon nano-tubes at first at 600 ℃ tubular type kiln roasting 2h;
(b) being transferred to sulfuric acid and nitric acid volume ratio is in the mixed solution of 3:1, and 60 ℃ are stirred 4h;
(c) centrifugation goes out precipitation, and is extremely neutral with deionized water wash;
(d) put that dry 24h. obtains carboxylated multi-walled carbon nano-tubes to 60 ℃ the baking oven.
(3) in-situ polymerization polypyrrole/BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4/ multi-wall carbon nano-tube composite material:
(a) BaFe of 1g
12O
19-Ni
0.8Zn
0.2Fe
2O
4Join in the 200ml deionized water ultra-sonic dispersion 1h with 2% multi-walled carbon nano-tubes;
(b) under 0 ℃, add the 2ml pyrrole monomer, ultrasonic 1h is uniformly dispersed;
(c) dropwise adding contains 18.2g FeCl
36H
2O (FeCl
36H
2O and pyrroles's mol ratio is 2.33:1) 100ml aqueous solution chlorination polymerization 12h, with the gained sedimentation and filtration, with behind deionized water and the ethanol repetitive scrubbing in 60 ℃ of vacuum drying ovens dry 24h, obtain polypyrrole/BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4/ multi-wall carbon nano-tube pipe powder.
Product among the embodiment 1 is mixed take mass ratio as 2:5 with paraffin, be pressed into the rectangle of 22.86mm * 10.16mm with mould, adopt vector network analyzer at its electromagnetic parameter of 8.2GHz-12.4GHz scope build-in test: magnetic permeability real part (μ '), magnetic permeability imaginary part (μ "), real part of permittivity (ε '), imaginary part of dielectric constant (ε ").By complex permeability μ
r=μ '-j μ ", complex permittivity ε
r=ε '-j ε ", and formula
Finally simulate the reflectivity R (dB) of sample.Record product at the reflection loss of 8.8-10.3GHz less than-10dB, be up under the 9GHz-20.6dB.
Embodiment 2:
(1) BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4Preparation:
(a) with mol ratio be the citric acid of 217:76:4:1:6, iron nitrate, nickelous nitrate, zinc nitrate, nitrate of baryta are dissolved in the deionized water, and the room temperature lower magnetic force stirs;
(b) be that the ethylene glycol of 2 times of citric acids joins in the solution with mol ratio, then regulate pH to 7 with quadrol;
(c) under the magnetic agitation, gained solution is heated to 75 ℃, transpiring moisture is to gel formation;
(d) with gel dry 24h in 120 ℃ baking oven at first, then be transferred to 400 ℃ retort furnace presintering 3h, at 1100 ℃ of lower calcining 2h, obtain BaFe at last
12O
19-Ni
0.8Zn
0.2Fe
2O
4Ferrite powder.
(2) multi-walled carbon nano-tubes is processed:
(a) with multi-walled carbon nano-tubes at first at 600 ℃ tubular type kiln roasting 2h;
(b) being transferred to sulfuric acid and nitric acid volume ratio is in the mixed solution of 3:1, and 60 ℃ are stirred 4h;
(c) centrifugation goes out precipitation, and is extremely neutral with deionized water wash;
(d) put that dry 24h. obtains carboxylated multi-walled carbon nano-tubes to 60 ℃ the baking oven.
(3) in-situ polymerization polypyrrole/BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4/ multi-wall carbon nano-tube composite material:
(a) BaFe of 1g
12O
19-Ni
0.8Zn
0.2Fe
2O
4Join in the 200ml deionized water ultra-sonic dispersion 1h with 5% multi-walled carbon nano-tubes;
(b) under 0 ℃, add the 2ml pyrrole monomer, ultrasonic 1h is uniformly dispersed;
(c) dropwise adding contains 18.2g FeCl
36H
2O (FeCl
36H
2O and pyrroles's mol ratio is 2.33:1) 100ml aqueous solution chlorination polymerization 12h, with the gained sedimentation and filtration, with behind deionized water and the ethanol repetitive scrubbing in 60 ℃ of vacuum drying ovens dry 24h, obtain polypyrrole/BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4/ multi-wall carbon nano-tube pipe powder.
Product among the embodiment 2 is mixed take mass ratio as 2:5 with paraffin, be pressed into the rectangle of 22.86mm * 10.16mm with mould, adopt vector network analyzer at its electromagnetic parameter of 8.2GHz-12.4GHz scope build-in test: magnetic permeability real part (μ '), magnetic permeability imaginary part (μ "), real part of permittivity (ε '), imaginary part of dielectric constant (ε ").By complex permeability μ
r=μ '-j μ ", complex permittivity ε
r=ε '-j ε ", and formula
Finally simulate the reflectivity R (dB) of sample.Record product at the reflection loss of 8.5-10.3GHz less than-10dB, be up under the 8.9GHz-25.46dB.
Embodiment 3:
(1) BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4Preparation:
(a) with mol ratio be the citric acid of 217:76:4:1:6, iron nitrate, nickelous nitrate, zinc nitrate, nitrate of baryta are dissolved in the deionized water, and the room temperature lower magnetic force stirs;
(b) be that the ethylene glycol of 2 times of citric acids joins in the solution with mol ratio, then regulate pH to 7 with quadrol;
(c) under the magnetic agitation, gained solution is heated to 75 ℃, transpiring moisture is to gel formation;
(d) with gel dry 24h in 120 ℃ baking oven at first, then be transferred to 400 ℃ retort furnace presintering 3h, at 1100 ℃ of lower calcining 2h, obtain BaFe at last
12O
19-Ni
0.8Zn
0.2Fe
2O
4Ferrite powder.
(2) multi-walled carbon nano-tubes is processed:
(a) with multi-walled carbon nano-tubes at first at 600 ℃ tubular type kiln roasting 2h;
(b) being transferred to sulfuric acid and nitric acid volume ratio is in the mixed solution of 3:1, and 60 ℃ are stirred 4h;
(c) centrifugation goes out precipitation, and is extremely neutral with deionized water wash;
(d) put that dry 24h. obtains carboxylated multi-walled carbon nano-tubes to 60 ℃ the baking oven.
(3) in-situ polymerization polypyrrole/BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4/ multi-wall carbon nano-tube composite material:
(a) BaFe of 1g
12O
19-Ni
0.8Zn
0.2Fe
2O
4Join in the 200ml deionized water ultra-sonic dispersion 1h with 10% multi-walled carbon nano-tubes;
(b) under 0 ℃, add the 2ml pyrrole monomer, ultrasonic 1h is uniformly dispersed;
(c) dropwise adding contains 18.2g FeCl
36H
2O (FeCl
36H
2O and pyrroles's mol ratio is 2.33:1) 100ml aqueous solution chlorination polymerization 12h, with the gained sedimentation and filtration, with behind deionized water and the ethanol repetitive scrubbing in 60 ℃ of vacuum drying ovens dry 24h, obtain polypyrrole/BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4/ multi-wall carbon nano-tube pipe powder.
Product among the embodiment 3 is mixed take mass ratio as 2:5 with paraffin, be pressed into the rectangle of 22.86mm * 10.16mm with mould, adopt vector network analyzer at its electromagnetic parameter of 8.2GHz-12.4GHz scope build-in test: magnetic permeability real part (μ '), magnetic permeability imaginary part (μ "), real part of permittivity (ε '), imaginary part of dielectric constant (ε ").By complex permeability μ
r=μ '-j μ ", complex permittivity ε
r=ε '-j ε ", and formula
Finally simulate the reflectivity R (dB) of sample.Record product at the reflection loss of 10.7-11.3GHz less than-10dB, be up under the 10.8GHz-23.9dB.
Case study on implementation 4:
(1) BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4Preparation:
(a) with mol ratio be the citric acid of 217:76:4:1:6, iron nitrate, nickelous nitrate, zinc nitrate, nitrate of baryta are dissolved in the deionized water, and the room temperature lower magnetic force stirs;
(b) be that the ethylene glycol of 2 times of citric acids joins in the solution with mol ratio, then regulate pH to 7 with quadrol;
(c) under the magnetic agitation, gained solution is heated to 75 ℃, transpiring moisture is to gel formation;
(d) with gel dry 24h in 120 ℃ baking oven at first, then be transferred to 400 ℃ retort furnace presintering 3h, at 1100 ℃ of lower calcining 2h, obtain BaFe at last
12O
19-Ni
0.8Zn
0.2Fe
2O
4Ferrite powder.
(2) multi-walled carbon nano-tubes is processed:
(a) with multi-walled carbon nano-tubes at first at 600 ℃ tubular type kiln roasting 2h;
(b) being transferred to sulfuric acid and nitric acid volume ratio is in the mixed solution of 3:1, and 60 ℃ are stirred 4h;
(c) centrifugation goes out precipitation, and is extremely neutral with deionized water wash;
(d) put dry 24h to 60 ℃ the baking oven, obtain carboxylated multi-walled carbon nano-tubes.
(3) in-situ polymerization polypyrrole/BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4/ multi-wall carbon nano-tube composite material:
(a) BaFe of 1g
12O
19-Ni
0.8Zn
0.2Fe
2O
4Join in the 200ml deionized water ultra-sonic dispersion 1h with 20% multi-walled carbon nano-tubes;
(b) under 0 ℃, add the 2ml pyrrole monomer, ultrasonic 1h is uniformly dispersed;
(c) dropwise adding contains 18.2g FeCl
36H
2O (FeCl
36H
2O and pyrroles's mol ratio is 2.33:1) 100ml aqueous solution chlorination polymerization 12h, with the gained sedimentation and filtration, with behind deionized water and the ethanol repetitive scrubbing in 60 ℃ vacuum drying oven dry 24h, obtain polypyrrole/BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4/ multi-wall carbon nano-tube pipe powder.
Product among the embodiment 4 is mixed take mass ratio as 2:5 with paraffin, be pressed into the rectangle of 22.86mm * 10.16mm with mould, adopt vector network analyzer at its electromagnetic parameter of 8.2GHz-12.4GHz scope build-in test: magnetic permeability real part (μ '), magnetic permeability imaginary part (μ "), real part of permittivity (ε '), imaginary part of dielectric constant (ε ").By complex permeability μ
r=μ '-j μ ", complex permittivity ε
r=ε '-j ε ", and formula
Finally simulate the reflectivity R (dB) of sample.Record product at the reflection loss of 11.2-11.7GHz less than-10dB, be up under the 11.3GHz-22.5dB.
Case study on implementation 5:
(1) BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4Preparation:
(a) with mol ratio be the citric acid of 217:76:4:1:6, iron nitrate, nickelous nitrate, zinc nitrate, nitrate of baryta are dissolved in the deionized water, and the room temperature lower magnetic force stirs;
(b) be that the ethylene glycol of 2 times of citric acids joins in the solution with mol ratio, then regulate pH to 7 with quadrol;
(c) under the magnetic agitation, gained solution is heated to 75 ℃, transpiring moisture is to gel formation;
(d) with gel dry 24h in 120 ℃ baking oven at first, then be transferred to 400 ℃ retort furnace presintering 3h, at 1100 ℃ of lower calcining 2h, obtain BaFe at last
12O
19-Ni
0.8Zn
0.2Fe
2O
4Ferrite powder.
(2) multi-walled carbon nano-tubes is processed:
(a) with multi-walled carbon nano-tubes at first at 600 ℃ tubular type kiln roasting 2h;
(b) being transferred to sulfuric acid and nitric acid volume ratio is in the mixed solution of 3:1, and 60 ℃ are stirred 4h;
(c) centrifugation goes out precipitation, and is extremely neutral with deionized water wash;
(d) put dry 24h to 60 ℃ the baking oven, obtain carboxylated multi-walled carbon nano-tubes.
(3) in-situ polymerization polypyrrole/BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4/ multi-wall carbon nano-tube composite material:
(a) BaFe of 1g
12O
19-Ni
0.8Zn
0.2Fe
2O
4Join in the 200ml deionized water ultra-sonic dispersion 1h with 30% multi-walled carbon nano-tubes;
(b) under 0 ℃, add the 2ml pyrrole monomer, ultrasonic 1h is uniformly dispersed;
(c) dropwise adding contains 18.2g FeCl
36H
2O (FeCl
36H
2O and pyrroles's mol ratio is 2.33:1) 100ml aqueous solution chlorination polymerization 12h, with the gained sedimentation and filtration, with behind deionized water and the ethanol repetitive scrubbing in 60 ℃ vacuum drying oven dry 24h, obtain polypyrrole/BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4/ multi-wall carbon nano-tube pipe powder.
Product among the embodiment 5 is mixed take mass ratio as 2:5 with paraffin, be pressed into the rectangle of 22.86mm * 10.16mm with mould, adopt vector network analyzer at its electromagnetic parameter of 8.2GHz-12.4GHz scope build-in test: magnetic permeability real part (μ '), magnetic permeability imaginary part (μ "), real part of permittivity (ε '), imaginary part of dielectric constant (ε ").By complex permeability μ
r=μ '-j μ ", complex permittivity ε
r=ε '-j ε ", and formula
Finally simulate the reflectivity R (dB) of sample.Record product at the reflection loss of 11.2-11.7GHz less than-10dB, be up under the 11.3GHz-28dB.
By the test result of above embodiment as can be known, 5% multi-wall carbon nano-tube composite material has excellent absorbing property than other ratios., be up under the 8.9GHz-25.46dB less than-10dB at the reflection loss of 8.5-10.3GHz, illustrate polypyrrole //BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4/ multi-walled carbon nano-tubes can be used for the stealth material field.Fig. 1 is the XRD figure of embodiment 2, has clearly show the crystal face of each material among the figure.Fig. 2 is embodiment 2TEM figure, shows polypyrrole and BaFe among the figure
12O
19-Ni
0.8Zn
0.2Fe
2O
4In-situ polymerization has formed polypyrrole/BaFe on the multi-wall carbon nano-tube tube-surface
12O
19-Ni
0.8Zn
0.2Fe
2O
4/ multi-walled carbon nano-tubes microwave absorbing system.
Claims (1)
1. the preparation method of polypyrrole/ferrite/multi-wall carbon nano-tube composite material is characterized in that step is as follows:
Step 1 adopts sol-gel method to prepare BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4Ferrite powder: be the citric acid of 217:76:4:1:6 with mol ratio, iron nitrate, nickelous nitrate, zinc nitrate and nitrate of baryta are dissolved in the deionized water, and the room temperature lower magnetic force stirs; Then the ethylene glycol that with mol ratio is 2 times of citric acids joins in the solution, and regulates pH to 7 with quadrol; Under the magnetic agitation, gained solution is heated to 75-80 ℃, transpiring moisture is to gel formation; With gel dry 12-36h in 120-140 ℃ baking oven at first, be transferred to then that calcining obtains BaFe in the retort furnace
12O
19-Ni
0.8Zn
0.2Fe
2O
4Ferrite powder;
Step 2 pair multi-walled carbon nano-tubes is processed: multi-walled carbon nano-tubes at 550-650 ℃ of tubular type kiln roasting 2-2.5h, then is transferred in the mixed solution of sulfuric acid and nitric acid and reacts 4-5h; By centrifugal or filter to isolate multi-walled carbon nano-tubes after, with deionized water wash; At the dry 12-36h of 50-60 ℃ vacuum drying oven, obtain carboxylated multi-walled carbon nano-tubes at last, the sulfuric acid of described mixed solution and the volume ratio of nitric acid are 3:1;
Step 3 original position is synthesized polypyrrole/BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4/ multi-wall carbon nano-tube composite material: be pyrrole monomer, the BaFe of 2:1:0.05-3 with mass ratio
12O
19-Ni
0.8Zn
0.2Fe
2O
4Join in the deionized water with multi-walled carbon nano-tubes, after ultra-sonic dispersion is complete, add FeCl
36H
2The aqueous solution of O carries out oxypolymerization; Be transferred to 50-60 ℃ the dry 12-36h of vacuum drying oven behind the precipitation repetitive scrubbing that the gained mixed solution obtains after filtration, obtain polypyrrole/BaFe
12O
19-Ni
0.8Zn
0.2Fe
2O
4/ multi-wall carbon nano-tube composite material; FeCl in the aqueous solution of described FeCl36H2O
36H
2O and pyrroles's mol ratio is 2.33:1.
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Cited By (12)
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CN103113580A (en) * | 2013-03-12 | 2013-05-22 | 哈尔滨工业大学 | Preparation method of coaxial cable structure MWCNT/Fe3O4/ZnO/PANI microwave absorbant |
CN103122066A (en) * | 2013-02-27 | 2013-05-29 | 南昌航空大学 | Preparation method of SDBS (sodium dodecyl benzene sulfonate) modified manganese-copper-cobalt ferrite filled carbon nanotube-polypyrrole composite wave absorbing material |
CN103450683A (en) * | 2013-08-28 | 2013-12-18 | 西北工业大学 | Preparation method of polypyrrole/BaFe12O19-Ni0.8Zn0.2Fe2O4/graphene nano wave-absorbing material |
CN104190385A (en) * | 2014-08-29 | 2014-12-10 | 湖南大学 | Polypyrrole/Fe3O4/graphene composite material, and preparation method and application thereof |
CN104608430A (en) * | 2015-01-12 | 2015-05-13 | 冯丹 | Wave-absorbing composite material |
CN104744895A (en) * | 2014-09-24 | 2015-07-01 | 郑州大学 | Conductive polymer and halloysite nanotube composite wave-absorbing material and preparation method thereof |
CN106495228A (en) * | 2016-10-17 | 2017-03-15 | 王道远 | Nano combined alkaline earth permanent magnetism powder body and preparation method thereof |
CN106905743A (en) * | 2017-03-02 | 2017-06-30 | 中国石油大学(北京) | Graphene/carbon nano-tube/iron containing compoundses/polymer coating type absorbing material |
CN110204713A (en) * | 2019-06-18 | 2019-09-06 | 合肥工业大学 | A kind of design method of the composite material with polypyrrole and manganese-zinc ferrite preparation with negative dielectric properties |
CN111551597A (en) * | 2020-05-29 | 2020-08-18 | 西安工程大学 | Polypyrrole composite electromagnetic wave absorbing material, preparation method and application |
CN113214481A (en) * | 2021-04-23 | 2021-08-06 | 陕西科技大学 | Preparation method of nickel ferrite-polypyrrole composite material with negative dielectric constant |
CN116496096A (en) * | 2023-06-20 | 2023-07-28 | 西南交通大学 | Method for enhancing wave absorbing performance of soft magnetic/hard magnetic composite ferrite |
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CN103113580A (en) * | 2013-03-12 | 2013-05-22 | 哈尔滨工业大学 | Preparation method of coaxial cable structure MWCNT/Fe3O4/ZnO/PANI microwave absorbant |
CN103450683A (en) * | 2013-08-28 | 2013-12-18 | 西北工业大学 | Preparation method of polypyrrole/BaFe12O19-Ni0.8Zn0.2Fe2O4/graphene nano wave-absorbing material |
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CN106495228A (en) * | 2016-10-17 | 2017-03-15 | 王道远 | Nano combined alkaline earth permanent magnetism powder body and preparation method thereof |
CN106905743A (en) * | 2017-03-02 | 2017-06-30 | 中国石油大学(北京) | Graphene/carbon nano-tube/iron containing compoundses/polymer coating type absorbing material |
CN106905743B (en) * | 2017-03-02 | 2020-05-22 | 中国石油大学(北京) | Graphene/carbon nanotube/iron-containing compound/polymer coating type wave-absorbing material |
CN110204713A (en) * | 2019-06-18 | 2019-09-06 | 合肥工业大学 | A kind of design method of the composite material with polypyrrole and manganese-zinc ferrite preparation with negative dielectric properties |
CN111551597A (en) * | 2020-05-29 | 2020-08-18 | 西安工程大学 | Polypyrrole composite electromagnetic wave absorbing material, preparation method and application |
CN113214481A (en) * | 2021-04-23 | 2021-08-06 | 陕西科技大学 | Preparation method of nickel ferrite-polypyrrole composite material with negative dielectric constant |
CN116496096A (en) * | 2023-06-20 | 2023-07-28 | 西南交通大学 | Method for enhancing wave absorbing performance of soft magnetic/hard magnetic composite ferrite |
CN116496096B (en) * | 2023-06-20 | 2023-09-01 | 西南交通大学 | Method for enhancing wave absorbing performance of soft magnetic/hard magnetic composite ferrite |
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