CN102965640B - Method for preparing carbon nano spiral electromagnetic wave absorbent coated by magnetic material - Google Patents

Method for preparing carbon nano spiral electromagnetic wave absorbent coated by magnetic material Download PDF

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CN102965640B
CN102965640B CN201210488870.9A CN201210488870A CN102965640B CN 102965640 B CN102965640 B CN 102965640B CN 201210488870 A CN201210488870 A CN 201210488870A CN 102965640 B CN102965640 B CN 102965640B
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CN102965640A (en
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覃勇
王桂振
高哲
陈朝秋
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Shanxi Institute of Coal Chemistry of CAS
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Abstract

The invention discloses a method for preparing a carbon nano spiral electromagnetic wave absorbent coated by a magnetic material. The method comprises the following steps of: pyrolyzing copper carboxylate at a high temperature to obtain copper nano particles, and carrying out a chemical vapor deposition reaction to obtain a carbon nano spiral by using the copper nano particles as a catalyst and acetylene as a carbon source; dispersing the carbon nano spiral on a quartz plate, putting the quartz plate into a reaction cavity of an atom layer deposition device and implementing the deposition of an Al2O3 protection film; directly implementing the deposition of a metal oxide Fe2O3 or NiO to the carbon nano spiral protected by an aluminum oxide film, reducing the carbon nano spiral product coated by Fe2O3 or NiO in a mixture atmosphere of H2 and N2, thereby obtaining a carbon nano spiral coated by a magnetic Fe3O4 or Ni coating. The method disclosed by the invention has the advantages of simple process and easiness for control.

Description

A kind of method preparing the coated carbon nanometer spiral radio-radar absorber of magneticsubstance
Technical field
The invention belongs to a kind of method preparing electromagnetic wave absorbent material, relate to one specifically and utilize ald (ALD) technology to prepare the method for magneticsubstance carbon coated nanometer spiral electromagnetic wave absorbent material.
Background technology
Carbon nanometer spiral is a kind of typical chiral material, and it has the plurality of advantages such as light weight, electroconductibility and good stability, is the good selection of design novel wave-absorbing material.But according to electromagnetic theory, good absorbing material must possess two main points, i.e. impedance matching and attenuation characteristic.Therefore, the material of two types is carried out multiple elements design, lowering economize on electricity magnetic parameter in the condition of mating as far as possible is improve the effective way absorbed.Carbon nanometer spiral has good electroconductibility, belongs to dielectric loss type material, has large quantity research to the absorbing property of carbon nanometer spiral, and achieves many achievements, is still paid attention to very much so far.But himself is substantially nonmagnetic, thus need and magneticsubstance compound, just can make it have the strong performance absorbed.Existing many investigators have carried out the research of magneticsubstance compound electric loss-type material, but carbon nanometer spiral size is little, chemically reactive is low and surface hole defect is many, traditional plating, electroless plating and sol-gel method are difficult to control effectively to coated quality and thickness, and complex process, step is many, does not obtain larger progress.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of technique simple, ald (ALD) technology that utilizes being easy to control prepares the method for the coated carbon nanometer spiral of magnetisable coating.
ALD is the thin film technique of a kind of advanced person, and can realize carrying out magneticsubstance to material surface coated, technique is simple, and thickness is even and highly controlled, and can realize ultra-thin coated, has outstanding advantage compared with traditional method.
The technical solution adopted in the present invention is:
(1) copper carboxylate salt is obtained copper nano-particle through high temperature pyrolysis, using copper nano-particle as catalyzer, acetylene is as carbon source, carbon nanometer spiral is obtained by chemical vapour deposition reaction, concrete preparation method is shown in Ph D dissertation: the growth pattern of spiral carbon nanofiber controls and growth mechanism research, author: Qin Yong, tutor: Cui Zuolin;
(2) the carbon nanometer spiral that step (1) obtains is scattered on quartz plate, puts into the reaction chamber of atomic layer deposition apparatus, carry out Al 2o 3the deposition of protective membrane;
The ALD deposition parameter of setting is:
Temperature of reaction 150-300 oC;
Reaction source: adopt Al (CH 3) 3and H 2o is precursor, Al (CH 3) 3and H 2o source temperature is room temperature;
Carrier gas: the high pure nitrogen of 10-50 sccm;
Single cycle pulse, to feel suffocated and purge time: first carry out H 2the O burst length is 0.1-0.5 s, and BHT is 5-7 s, and purge time is 10-15 s; Then Al (CH is carried out 3) 3burst length is 0.01-0.5 s, and BHT is 5-7 s, and purge time is 10-15 s;
(3) the carbon nanometer spiral of step (2) after aluminum oxide film protection is directly carried out metal oxide Fe 2o 3or the deposition of NiO, the ALD deposition parameter of setting is:
Deposition Fe 2o 3time:
Temperature of reaction: Fe 2o 3depositing temperature is 220-300 oC;
Reaction source: Fe 2o 3adopt ferrocene (Fe (Cp) 2) and O 3for precursor, Fe (Cp) 2source temperature is 120-150 oC, O 3source temperature is room temperature;
Carrier gas: the high pure nitrogen of 10-50 sccm;
Single cycle pulse, to feel suffocated and purge time: first carry out O 3burst length is 0.1-0.5 s, and BHT is 3-5 s, and purge time is 14-18 s; Then Fe (Cp) is carried out 2burst length is 2-5 s, and BHT is 5-7 s, and purge time is 14-18 s;
During deposition NiO:
Temperature of reaction: NiO depositing temperature is 150-180 oC;
Reaction source: NiO adopts nickelocene (Ni (Cp) 2) and O 3for precursor, Ni (Cp) 2source temperature is 60-80 oC, O 3source temperature is room temperature;
Carrier gas: the high pure nitrogen of 10-50 sccm;
Single cycle pulse, to feel suffocated and purge time: first carry out O 3pulse is 0.1-0.5 s, and feel suffocated 3-5 s, and purge time is 20-25 s; Then Ni (Cp) is carried out 2pulse is 8-10 s, and BHT is 1-3 s, and purge time is 20-25 s;
(4) by coated Fe that step (3) obtains 2o 3or the carbon nanometer spiral product after NiO is at H 2the H of content to be volume ratio be 5-10% 2with N 2high temperature reduction in mixed atmosphere, namely obtains the Fe of magnetic 3o 4or the carbon nanometer spiral that Ni coating is coated.
In the technical program, Fe 2o 3each cycling deposition thickness is each cycling deposition thickness of 0.09-0.11, NiO is 0.18-0.2.By step (3) to Fe 2o 3or the single cycle pulse of NiO, to feel suffocated and purge repeatedly repeats, the thickness of magnetic coating layer can be controlled.
Compared with prior art tool of the present invention has the following advantages:
1, it is coated that the technique for atomic layer deposition that the present invention adopts can realize the magneticsubstance of nano level uniform, controllable on carbon nanometer spiral surface, can the electromagnetic parameter of very effective adjustment material, thus realize impedance matching, obtains efficient absorbing material.Prepared magnetisable coating carbon coated nanometer spiral has important actual application value in electromagnetic absorption field.
2, in the present invention, Fe is worked as 2o 3when cycle index is 2400, assimilation effect is better, and loss is absorbed as-10 ~-28.5dB at 10.5-14.0GHz.Nickel oxide circulate 800 times time, loss is absorbed as-10 ~-11.7dB at 10.5-15.3GHz.
3, technique is simple.
Accompanying drawing explanation
Fig. 1 is embodiment 1 is the Fe that deposition 600 circulates 2o 3the Fe obtained after reduction 3o 4/ Al 2o 3the TEM photo of/CNC, Fig. 2 is embodiment 1 is reflection loss and frequency variation curve.
Fig. 3 is embodiment 2 is the Fe that deposition 1200 circulates 2o 3the Fe obtained after reduction 3o 4/ Al 2o 3the TEM photo of/CNC, Fig. 4 is embodiment 2 is reflection loss and frequency variation curve.
Fig. 5 is embodiment 3 is the Fe that deposition 2400 circulates 2o 3the Fe obtained after reduction 3o 4/ Al 2o 3the TEM photo of/CNC, Fig. 6 is embodiment 3 is reflection loss and frequency variation curve.
Fig. 7 is embodiment 4 is the Ni/Al obtained after the Ni reduction of deposition 400 circulation 2o 3the TEM photo of/CNC, Fig. 8 is embodiment 4 is reflection loss and frequency variation curve.
Fig. 9 is embodiment 5 is the Ni/Al obtained after the Ni reduction of deposition 800 circulation 2o 3the TEM photo of/CNC, Figure 10 is embodiment 5 is reflection loss and frequency variation curve.
Embodiment
Embodiment 1
By cupric tartrate presoma in 250oC pyrolysis, obtain the copper nano-particle of about 50 nm, pass into acetylene gas, at 250oC catalyzing acetylene, synthesis spiral nano-fibre.By spiral nano-fibre thermal treatment 1 hour in 900oC rare gas element, obtain having uniform spiral structure, the carbon nanometer spiral of direct 100nm.Be distributed on quartz plate by carbon nanometer spiral, be transferred to the reaction chamber of atomic layer deposition apparatus after drying, the ALD deposition parameter of setting is:
Temperature of reaction 150 oC; Reaction source: adopt Al (CH 3) 3and H 2o is precursor, and the two temperature is room temperature; Carrier gas: the high pure nitrogen of 10 sccm; Single cycle pulse, to feel suffocated and purge time: first H 2o pulse is 0.1 s, and BHT is 5 s, and purge time is 10 s; Then Al (CH 3) 3pulse is 0.015 s, and BHT is 5 s, and purge time is 10 s; Carry out the Al of 100 circulations continuously 2o 3the deposition of protective membrane.
Then Fe is carried out 2o 3deposition, setup parameter is:
Temperature of reaction is 220 oC; Reaction source: ferrocene (Fe (Cp) 2) and O 3; Fe (Cp) 2source temperature is 120 oC; O 3source temperature is room temperature; Carrier gas: the high pure nitrogen of 50 sccm; Single cycle pulse, to feel suffocated and purge time: first carry out O 3pulse is 0.5 s, and BHT is 3 s, and purge time is 14 s; Then Fe (Cp) is carried out 2pulse is 5 s, and BHT is 5 s, and purge time is 14 s; Carry out the Fe of 600 circulations continuously 2o 3deposition, the product obtained is at H 2: N 2for in the atmosphere of 5:95, namely 450oC reductase 12 hour obtains Fe 3o 4coated carbon nanometer spiral.
Can find out from electromicroscopic photograph, the Al of carbon fiber surface is evenly coated 12 nm 2o 3with the Fe of 6 nm 3o 4, product and paraffin 1:3 are mixed with magnet ring sample (internal diameter: 3.04 mm, external diameter: 7.00 mm), its absorbing property is studied with vector network analyzer test electromagnetic parameter, result shows, when thickness is 2 mm, the reflectivity of product is-10.0 ~-10.7 dB at 8.1-9.2 GHz.
Embodiment 2
By cupric tartrate presoma in 250oC pyrolysis, obtain the copper nano-particle of about 50 nm, pass into acetylene gas, at 250oC catalyzing acetylene, synthesis spiral nano-fibre.By spiral fiber thermal treatment 1 hour in 900oC rare gas element, obtain having uniform spiral structure, the carbon nanometer spiral of direct 100nm.Be distributed on quartz plate by carbon nanometer spiral, be transferred to the reaction chamber of atomic layer deposition apparatus after drying, the ALD deposition parameter of setting is:
Temperature of reaction 200 oC; Reaction source: adopt Al (CH 3) 3and H 2o is precursor, and precursor temperature is room temperature; Carrier gas: the high pure nitrogen of 30 sccm; Single cycle pulse, to feel suffocated and purge time: first carry out H 2o pulse is 0.3 s, and BHT is 6 s, and purge time is 12 s; Then Al (CH is carried out 3) 3pulse is 0.1 s, and BHT is 6 s, and purge time is 12 s; Carry out the Al of 100 circulations continuously 2o 3the deposition of protective membrane.
Then Fe is carried out 2o 3deposition, setup parameter is:
Temperature of reaction is 260 oC; Reaction source: ferrocene (Fe (Cp) 2) and O 3; Fe (Cp) 2source temperature is 135 oC; O 3source temperature is room temperature; Carrier gas: the high pure nitrogen of 50 sccm; Single cycle pulse, to feel suffocated and purge time: first carry out O 3pulse is 0.3 s, and BHT is 4 s, and purge time is 16 s; Then Fe (Cp) is carried out 2pulse is 4 s, and BHT is 6 s, and purge time is 16 s; Carry out the Fe of 1200 circulations continuously 2o 3deposition, the product obtained is at H 2: N 2for in the atmosphere of 10:90, namely 450oC reductase 12 hour obtains Fe 3o 4coated carbon nanometer spiral.
Can find out from electromicroscopic photograph, the Al of carbon fiber surface is evenly coated 12 nm 2o 3with the Fe of 12 nm 3o 4, product and paraffin 1:3 are mixed with magnet ring sample (internal diameter: 3.04 mm, external diameter: 7.00 mm), its absorbing property is studied with vector network analyzer test electromagnetic parameter, result shows, when thickness is 2 mm, the reflectivity of product is-10.0 ~-18.4 dB at 9.6-12.4 GHz.
Embodiment 3
By cupric tartrate presoma in 250oC pyrolysis, obtain the copper nano-particle of about 50 nm, pass into acetylene gas, at 250oC catalyzing acetylene, synthesis spiral nano-fibre.By spiral fiber thermal treatment 1 hour in 900oC rare gas element, obtain having uniform spiral structure, the carbon nanometer spiral of direct 100nm.Be distributed on quartz plate by carbon nanometer spiral, be transferred to the reaction chamber of atomic layer deposition apparatus after drying, the ALD deposition parameter of setting is:
Temperature of reaction 250 oC; Reaction source: adopt Al (CH 3) 3and H 2o is precursor, and precursor temperature is room temperature; Carrier gas: the high pure nitrogen of 50 sccm; Single cycle pulse, to feel suffocated and purge time: first carry out H 2o pulse is 0.5 s, and BHT is 7 s, and purge time is 15 s; Then Al (CH is carried out 3) 3pulse is 0.4 s, and BHT is 7 s, and purge time is 15 s; Carry out the Al of 100 circulations continuously 2o 3the deposition of protective membrane.
Then Fe is carried out 2o 3deposition, setup parameter is:
Temperature of reaction is 300 oC; Reaction source: ferrocene (Fe (Cp) 2) and O 3; Fe (Cp) 2source temperature is 150 oC; O 3source temperature is room temperature; Carrier gas: the high pure nitrogen of 50 sccm; Single cycle pulse, to feel suffocated and purge time: first carry out O 3pulse is 0.1 s, and BHT is 5 s, and purge time is 18 s; Then Fe (Cp) is carried out 2pulse is 2 s, and BHT is 7 s, and purge time is 18 s; Carry out the Fe of 2400 circulations continuously 2o 3deposition, the product obtained is at H 2: N 2for in the atmosphere of 5:95, namely 450oC reductase 12 hour obtains Fe 3o 4coated carbon nanometer spiral.
Can find out from electromicroscopic photograph, the Al of carbon fiber surface is evenly coated 12 nm 2o 3with the Fe of 24 nm 3o 4, product and paraffin 1:3 are mixed with magnet ring sample (internal diameter: 3.04 mm, external diameter: 7.00 mm), its absorbing property is studied with vector network analyzer test electromagnetic parameter, result shows, when thickness is 2 mm, the reflectivity of product is-10.0 ~-28.4 dB at 10.5-14.0 GHz.
Embodiment 4
By cupric tartrate presoma in 250 oC pyrolysis, obtain the copper nano-particle of about 50 nm, pass into acetylene gas, at 250 oC catalyzing acetylenes, synthesis spiral nano-fibre.By spiral fiber thermal treatment 1 hour in 900 oC rare gas elementes, obtain having uniform spiral structure, the carbon nanometer spiral of direct 100 nm.Be distributed on quartz plate by carbon nanometer spiral, be transferred to the reaction chamber of atomic layer deposition apparatus after drying, the ALD deposition parameter of setting is:
Temperature of reaction 300 oC; Reaction source: adopt Al (CH 3) 3and H 2o is precursor, and precursor temperature is room temperature; Carrier gas: the high pure nitrogen of 20 sccm; Single cycle pulse, to feel suffocated and purge time: first H 2o pulse is 0.2 s, and BHT is 6 s, and purge time is 10 s; Then Al (CH 3) 3pulse is 0.015 s, and BHT is 6 s, and purge time is 10 s; Carry out the Al of 100 circulations continuously 2o 3the deposition of protective membrane.
Then the deposition of NiO is carried out,
Setup parameter is: temperature of reaction is 150 oC; Reaction source: nickelocene (Ni (Cp) 2) and O 3; Ni (Cp) 2source temperature is 80 oC; O 3source temperature is room temperature; Carrier gas: the high pure nitrogen of 50 sccm; Single cycle pulse, to feel suffocated and purge time: first carry out O 3pulse is 0.1 s, and BHT is 3s, and purge time is 20 s; Then Ni (Cp) is carried out 2pulse is 8 s, and BHT is 1s, and purge time is 20 s; Carry out the NiO deposition of 400 circulations continuously, the product obtained is at H 2: N 2for namely 450oC reductase 12 in the atmosphere of 5:95 hour obtains the coated carbon nanometer spiral of Ni film of nanoparticles.
Can find out from electromicroscopic photograph, the Al of carbon fiber surface is evenly coated 12 nm 2o 3film and median size are the Ni particle membrane of 4.7 nm, product and paraffin 1:3 are mixed with magnet ring sample (internal diameter: 3.04 mm, external diameter: 7.00 mm), its absorbing property is studied with vector network analyzer test electromagnetic parameter, result shows, when thickness is 1.5 mm, the reflectivity of product is-10.0 ~-11.4 dB at 11.9-14.7 GHz.
Embodiment 5
By cupric tartrate presoma in 250oC pyrolysis, obtain the copper nano-particle of about 50nm, pass into acetylene gas, at 250oC catalyzing acetylene, synthesis spiral nano-fibre.By spiral fiber thermal treatment 1 hour in 900oC rare gas element, obtain having uniform spiral structure, the carbon nanometer spiral of direct 100nm.Be distributed on quartz plate by carbon nanometer spiral, be transferred to the reaction chamber of atomic layer deposition apparatus after drying, the ALD deposition parameter of setting is:
Temperature of reaction 300 oC; Reaction source: adopt Al (CH 3) 3and H 2o is precursor, and precursor temperature is room temperature; Carrier gas: the high pure nitrogen of 20 sccm; Single cycle pulse, to feel suffocated and purge time: first carry out H 2o pulse is 0.2 s, and BHT is 6 s, and purge time is 10 s; Then Al (CH 3) 3pulse is 0.02 s, and BHT is 6 s, and purge time is 10 s; Carry out the Al of 100 circulations continuously 2o 3the deposition of protective membrane.
Then the deposition of NiO is carried out,
Setup parameter is: temperature of reaction is 180 oC; Reaction source: nickelocene (Ni (Cp) 2) and O 3; Ni (Cp) 2source temperature is 80 oC; O 3source temperature is room temperature; Carrier gas: the high pure nitrogen of 50 sccm; Single cycle pulse, to feel suffocated and purge time: first carry out O 3pulse is 0.1 s, and BHT is 5 s, and purge time is 24 s; Then Ni (Cp) is carried out 2pulse is 10 s, and BHT is 1s, and purge time is 24 s; Carry out the NiO deposition of 800 circulations continuously, the product obtained is at H 2: N 2for namely 450oC reductase 12 in the atmosphere of 10:90 hour obtains the coated carbon nanometer spiral of Ni film of nanoparticles.
Can find out from electromicroscopic photograph, the Al of carbon fiber surface is evenly coated 12 nm 2o 3film and median size are the Ni particle membrane of 8.9 nm, product and paraffin 1:3 are mixed with magnet ring sample (internal diameter: 3.04 mm, external diameter: 7.00 mm), its absorbing property is studied with vector network analyzer test electromagnetic parameter, result shows, when thickness is 1.5 mm, the reflectivity of product is-10.0 ~-14.7 dB at 11.7-15.3 GHz.

Claims (3)

1. prepare a method for the coated carbon nanometer spiral radio-radar absorber of magneticsubstance, it is characterized in that comprising the steps:
(1) copper carboxylate salt is obtained copper nano-particle through high temperature pyrolysis, using copper nano-particle as catalyzer, acetylene, as carbon source, obtains carbon nanometer spiral by chemical vapour deposition reaction;
(2) the carbon nanometer spiral that step (1) obtains is scattered on quartz plate, puts into the reaction chamber of atomic layer deposition apparatus, carry out Al 2o 3the deposition of protective membrane;
The ALD deposition parameter of setting is:
Temperature of reaction 150-300 DEG C;
Reaction source: adopt Al (CH 3) 3and H 2o is precursor, Al (CH 3) 3and H 2o source temperature is room temperature;
Carrier gas: the high pure nitrogen of 10-50 sccm;
Single cycle pulse, to feel suffocated and purge time: first carry out H 2the O burst length is 0.1-0.5 s, and BHT is 5-7 s, and purge time is 10-15 s; Then Al (CH is carried out 3) 3burst length is 0.01-0.5 s, and BHT is 5-7 s, and purge time is 10-15 s;
(3) the carbon nanometer spiral of step (2) after aluminum oxide film protection is directly carried out metal oxide Fe 2o 3or the deposition of NiO, the ALD deposition parameter of setting is:
Deposition Fe 2o 3time:
Temperature of reaction: Fe 2o 3depositing temperature is 220-300 DEG C;
Reaction source: Fe 2o 3adopt ferrocene (Fe (Cp) 2) and O 3for precursor, Fe (Cp) 2source temperature is 120-150 DEG C, O 3source temperature is room temperature;
Carrier gas: the high pure nitrogen of 10-50 sccm;
Single cycle pulse, to feel suffocated and purge time: first carry out O 3burst length is 0.1-0.5 s, and BHT is 3-5 s, and purge time is 14-18 s; Then Fe (Cp) is carried out 2burst length is 2-5 s, and BHT is 5-7 s, and purge time is 14-18 s;
During deposition NiO:
Temperature of reaction: NiO depositing temperature is 150-180 DEG C;
Reaction source: NiO adopts nickelocene (Ni (Cp) 2) and O 3for precursor, Ni (Cp) 2source temperature is 60-80 DEG C, O 3source temperature is room temperature;
Carrier gas: the high pure nitrogen of 10-50 sccm;
Single cycle pulse, to feel suffocated and purge time: first carry out O 3pulse is 0.1-0.5 s, and feel suffocated 3-5 s, and purge time is 20-25 s; Then Ni (Cp) is carried out 2pulse is 8-10 s, and BHT is 1-3 s, and purge time is 20-25 s;
(4) by coated Fe that step (3) obtains 2o 3or the carbon nanometer spiral product after NiO is at H 2the H of content to be volume ratio be 5-10% 2with N 2high temperature reduction in mixed atmosphere, namely obtains the Fe of magnetic 3o 4or the carbon nanometer spiral that Ni coating is coated.
2. a kind of method preparing the coated carbon nanometer spiral radio-radar absorber of magneticsubstance as claimed in claim 1, is characterized in that by step (3) Fe 2o 3or the single cycle pulse of NiO, to feel suffocated and purge repeatedly repeats, the thickness of magnetic coating layer can be controlled.
3. a kind of method preparing the coated carbon nanometer spiral radio-radar absorber of magneticsubstance as claimed in claim 2, is characterized in that described Fe 2o 3each single loop growth thickness is each single loop growth thickness of 0.09-0.11, NiO is 0.18-0.2.
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