CN1300054C - Composite microwave absorbent of Nano carbon tube, and preparation method - Google Patents
Composite microwave absorbent of Nano carbon tube, and preparation method Download PDFInfo
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- CN1300054C CN1300054C CNB2004100509183A CN200410050918A CN1300054C CN 1300054 C CN1300054 C CN 1300054C CN B2004100509183 A CNB2004100509183 A CN B2004100509183A CN 200410050918 A CN200410050918 A CN 200410050918A CN 1300054 C CN1300054 C CN 1300054C
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- absorption agent
- carbon nanotube
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Abstract
The present invention relates to composite microwave absorbent of a nano carbon tube and a preparation method thereof. In the method, acetylene can be pyrolyzed with a simple device to prepare the composite microwave absorbent of a nano carbon tube of which the tube diameter can be controlled. The present invention has the characteristics of simple synthesis technology, high purity and low cost; a synthetic carbon nano tube has an outer diameter of 10 to 35 nm. The main components of the absorbent comprises the carbon nano tube, Fe2O3 and Al2O3, wherein the mass percents: the carbon nano tube is 75 to 90 percent, the Fe2 O3 is 5 to 11 percent, the Al2 O3 is 1 to 15 percent, and amorphous carbon granules is 1 to 5 percent. The appearance of the absorbent is black.
Description
Technical field
The present invention relates to a kind of carbon nanotube composite microwave absorption agent and preparation method thereof.
Background technology
Results reported is seen at present, absorbing material mainly contains: (1) conduction high polymer absorption agent, (2) metallic compound absorption agent. (3) Metal and Alloy absorption agent, (4) ceramic-like absorption agent. mainly contain SiC powder, SiC fiber, pure aluminium silicate etc., (5) nano wave-absorbing material.The nano material particular structure makes it have quantum size effect, small-size effect and surface interface effect.It is much bigger that the nano level super-fine powder is in surperficial atom number, increased the activity of nano material, thereby increased absorption of electromagnetic wave.The nanometer microwave absorption agent of research mainly contains following several types both at home and abroad: nano metal and alloy absorption agent, nano-oxide absorption agent, nano SiC absorption agent, nanometer ferrite absorption agent, nano-graphite absorption agent, nanoporous metal membrane, dielectric insulating film absorption agent, nanometer conductive polymer absorption agent, nano nitride absorption agent etc.There is following problem in above-mentioned absorption agent: the antioxidant property of metal powder absorption agent is relatively poor, causes the ageing resistance of coating to descend; Metallic compound absorption agent add-on needs a lot, causes coating overweight; The resistivity of ceramic-like absorption agent is higher again, compare with above-mentioned absorbing material, the advantage of carbon nanotube absorbing material is except it is nano material, being that also carbon nanotube is the chirality absorbing material. the advantage of chiral material is incident electromagnetic wave is not had mirror symmetry, can better realize electromagnetic diffuse scattering, reach by the reflection that reduces incident electromagnetic wave and absorb electromagnetic purpose.And it is low to frequency sensitivity, easily realizes wide band absorption.Carbon nanotube also has characteristics such as high-strength and high-modulus lightweight and Heat stability is good, so be a kind of ideal electromagnetic wave absorbent material.The another innovation of carbon nanotube composite microwave absorption agent of the present invention institute tool is: catalyst themselves is the nano-metal-oxide absorption agent simultaneously, and this catalyzer institute synthetic carbon nanotube composite microwave absorption agent has the absorption of electromagnetic wave performance advantage of nano-oxide absorption agent and carbon nanotube absorption agent simultaneously concurrently.
Summary of the invention
The purpose of this invention is to provide a kind of carbon nanotube composite microwave absorption agent and preparation method thereof.
Carbon nanotube composite microwave absorption agent of the present invention is to be main component with the carbon nanotube, contains Fe2O3, Al2O3 and decolorizing carbon particle; Wherein to account for mass percent be 75～90% to carbon nanotube, and it is 5～11% that Fe2O3 accounts for mass percent, and the shared mass percent of Al2O3 is that the shared mass percent of 1～15%. decolorizing carbon particle is 1～5%, and the carbon nanotube external diameter is distributed as 10～35nm.
The preparation technology of carbon nanotube composite microwave absorption agent has following steps:
(1) nitric acid molysite and the aluminum nitrate salt that takes by weighing suitable proportion dissolves in distilled water, add an amount of organic acid, after stirring, adding ammoniacal liquor regulator solution pH value is 7, solution is dried down at 120 ℃, to add 95% ethanol in the solid matter that obtain behind the complete drying, products therefrom is used to prepare carbon nanotube composite microwave absorption agent as catalyzer after the ignition;
(2) adopt the horizontal pipe stove, at first on catalyzer, feed the air in the nitrogen eliminating reaction unit, heat up then, feeding flow when unit temp rises to about 873K is the hydrogen of 50sccm, continues to heat up, when rising to 1000K, unit temp feeds acetylene, the acetylene flow is 100sccm, reacts to stop heating after 30 minutes, and gas is switched to nitrogen, under nitrogen atmosphere, lower the temperature, collect product and obtain carbon nanotube composite microwave absorption agent.
Embodiment
It below is the example of preparation carbon nanotube composite microwave absorption agent.
Embodiment 1:
Take by weighing the nitric acid molysite and the aluminum nitrate salt (nFe of suitable proportion
+ 3: nAl
+ 3=1: 5) in distilled water, dissolve, add an amount of organic acid, after stirring, adding ammoniacal liquor regulator solution pH value is 7, solution is dried down at 120 ℃, 95% ethanol detonator will be added in the solid matter that obtain behind the complete drying, products therefrom is 1: 5 catalyzer for the Fe/Al mol ratio after the ignition. the quartz boat that this catalyzer of 1g (the Fe/Al mol ratio is 1: 5) will be housed is put into reaction chamber, feed and feed hydrogen when nitrogen is heated to 873K again, hydrogen flowing quantity is a 50sccm acetylene, when unit temp rises to 1000K, feed acetylene, regulating the acetylene flow is 100sccm, under 1000K, stop heating behind the reaction 0.5h, gas is switched to nitrogen, feed nitrogen, obtain carbon nanotube composite microwave absorption agent until the device cool to room temperature.To account for mass percent be 75% to carbon nanotube in the composite microwave absorption agent, and it is 5% that Fe2O3 accounts for mass percent, and the shared mass percent of Al2O3 is that the shared mass percent of 15%. decolorizing carbon particles is 5%.
Embodiment 2:
Take by weighing the nitric acid molysite and the aluminum nitrate salt (nFe of suitable proportion
+ 3: nAl
+ 3=1: 2) in distilled water, dissolve, add an amount of organic acid, after stirring, adding ammoniacal liquor regulator solution pH value is 7, solution is dried down at 120 ℃, 95% ethanol detonator will be added in the solid matter that obtain behind the complete drying, products therefrom is 1: 2 catalyzer for the Fe/Al mol ratio after the ignition. the quartz boat that this catalyzer of 1g (the Fe/Al mol ratio is 1: 2) will be housed is put into reaction chamber, feed and feed hydrogen when nitrogen is heated to 873K again, hydrogen flowing quantity is a 50sccm acetylene, when unit temp rises to 1000K, feed acetylene, regulating the acetylene flow is 100sccm, under 1000K, stop heating behind the reaction 0.5h, gas is switched to nitrogen, feed nitrogen, obtain carbon nanotube composite microwave absorption agent until the device cool to room temperature.To account for mass percent be 76% to carbon nanotube in the composite microwave absorption agent, and it is 8% that Fe2O3 accounts for mass percent, and the shared mass percent of Al2O3 is that the shared mass percent of 12%. decolorizing carbon particles is 4%.
Embodiment 3:
Take by weighing the nitric acid molysite and the aluminum nitrate salt (nFe of suitable proportion
+ 3: nAl
+ 3=1: 1) in distilled water, dissolve, add an amount of organic acid, after stirring, adding ammoniacal liquor regulator solution pH value is 7, solution is dried down at 120 ℃, to add 95% ethanol detonator in the solid matter that obtain behind the complete drying, products therefrom is 1: 1 catalyzer for the Fe/Al mol ratio after the ignition.The quartz boat that this catalyzer of 1g (the Fe/Al mol ratio is 1: 1) will be housed is put into reaction chamber, feed and feed hydrogen when nitrogen is heated to 873K again, hydrogen flowing quantity is a 50sccm acetylene, when unit temp rises to 1000K, feed acetylene, regulating the acetylene flow is 100sccm, under 1000K, stop heating behind the reaction 0.5h, gas is switched to nitrogen, feed nitrogen, obtain carbon nanotube composite microwave absorption agent until the device cool to room temperature.To account for mass percent be 80% to carbon nanotube in the composite microwave absorption agent, and it is 11% that Fe2O3 accounts for mass percent, and the shared mass percent of Al2O3 is that the shared mass percent of 6%. decolorizing carbon particles is 3%.
Embodiment 4:
Take by weighing the nitric acid molysite and the aluminum nitrate salt (nFe of suitable proportion
+ 3: nAl
+ 3=2: 1) in distilled water, dissolve, add an amount of organic acid, after stirring, adding ammoniacal liquor regulator solution pH value is 7, solution is dried down at 120 ℃, 95% ethanol detonator will be added in the solid matter that obtain behind the complete drying, products therefrom is 2.: 1 catalyzer for the Fe/Al mol ratio after the ignition. the quartz boat that this catalyzer of 1.0g (the Fe/Al mol ratio is 2: 1) will be housed is put into reaction chamber, feed and feed hydrogen when nitrogen is heated to 873K again, hydrogen flowing quantity is a 50sccm acetylene, when unit temp rises to 1000K, feed acetylene, regulating the acetylene flow is 100sccm, under 1000K, stop heating behind the reaction 0.5h, gas is switched to nitrogen, feed nitrogen, obtain carbon nanotube composite microwave absorption agent until the device cool to room temperature.To account for mass percent be 82% to carbon nanotube in the composite microwave absorption agent, and it is 11% that Fe2O3 accounts for mass percent, and the shared mass percent of Al2O3 is that the shared mass percent of 5%. decolorizing carbon particles is 2%.
Embodiment 5:
Take by weighing the nitric acid molysite and the aluminum nitrate salt (nFe of suitable proportion
+ 3: nAl
+ 3=5: 1) in distilled water, dissolve, add an amount of organic acid, after stirring, adding ammoniacal liquor regulator solution pH value is 7, solution is dried down at 120 ℃, to add 95% ethanol detonator in the solid matter that obtain behind the complete drying, products therefrom is 39: 1 catalyzer for the Fe/Al mol ratio after the ignition.The quartz boat that this catalyzer of 1.0g (the Fe/Al mol ratio is 5: 1) will be housed is put into reaction chamber, feed and feed hydrogen when nitrogen is heated to 873K again, hydrogen flowing quantity is a 50sccm acetylene, when unit temp rises to 1000K, feed acetylene, regulating the acetylene flow is 100sccm, under 1000K, stop heating behind the reaction 0.5h, gas is switched to nitrogen, feed nitrogen, obtain carbon nanotube composite microwave absorption agent until the device cool to room temperature.To account for mass percent be 90% to carbon nanotube in the composite microwave absorption agent, and it is 8% that Fe2O3 accounts for mass percent, and the shared mass percent of Al2O3 is that the shared mass percent of 1%. decolorizing carbon particles is 1%.
Claims (1)
1. carbon nanotube composite microwave absorption agent is characterized in that: described carbon nanotube composite microwave absorption agent is to be main component with the carbon nanotube, contains Fe
2O
3, Al
2O
3With the decolorizing carbon particle; Wherein to account for mass percent be 75～90% to carbon nanotube, Fe
2O
3Accounting for mass percent is 5～11%, Al
2O
3Shared mass percent is 1～15%, and the shared mass percent of decolorizing carbon particle is 1～5%, and the carbon nanotube external diameter is distributed as 10～35nm.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2004100509183A CN1300054C (en) | 2004-07-30 | 2004-07-30 | Composite microwave absorbent of Nano carbon tube, and preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100509183A CN1300054C (en) | 2004-07-30 | 2004-07-30 | Composite microwave absorbent of Nano carbon tube, and preparation method |
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| Publication Number | Publication Date |
|---|---|
| CN1727306A CN1727306A (en) | 2006-02-01 |
| CN1300054C true CN1300054C (en) | 2007-02-14 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102101371A (en) * | 2010-10-29 | 2011-06-22 | 清华大学 | Method for bonding objects |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108516815A (en) * | 2018-05-03 | 2018-09-11 | 佛山九陌科技信息咨询有限公司 | A kind of preparation method of Electromagnetic heating type microwave absorbing material |
| CN115414937B (en) * | 2022-08-17 | 2024-04-16 | 华东理工大学 | Catalyst for preparing carbon nano tube by microwave catalytic pyrolysis of waste plastics and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1514684A (en) * | 2003-06-27 | 2004-07-21 | 中国科学院上海硅酸盐研究所 | Carbon nano-pipe/ceramic composite material possessing microwave absorption function and its preparation method |
-
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1514684A (en) * | 2003-06-27 | 2004-07-21 | 中国科学院上海硅酸盐研究所 | Carbon nano-pipe/ceramic composite material possessing microwave absorption function and its preparation method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102101371A (en) * | 2010-10-29 | 2011-06-22 | 清华大学 | Method for bonding objects |
| CN102101371B (en) * | 2010-10-29 | 2014-04-23 | 清华大学 | Method for bonding objects |
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| CN1727306A (en) | 2006-02-01 |
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