CN102344648B - Conductive polymer-magnetic material composite absorbing material - Google Patents
Conductive polymer-magnetic material composite absorbing material Download PDFInfo
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- CN102344648B CN102344648B CN201010243099.XA CN201010243099A CN102344648B CN 102344648 B CN102344648 B CN 102344648B CN 201010243099 A CN201010243099 A CN 201010243099A CN 102344648 B CN102344648 B CN 102344648B
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Abstract
The invention, belonging to the technical field of absorbing material, relates to a conductive polymer-magnetic material composite absorbing material. The conductive polymer-magnetic material composite absorbing material comprises alfa-ferrite/poly(3,4-dioxo ethyl)thiophene (PEDOT) composite nanorods, epoxy resin or polyurethane and other organic binder, wherein, the alfa-ferrite/poly(3,4-dioxo ethyl)thiophene (PEDOT) composite nanorods account for 30-80 wt% of the conductive polymer-magnetic material composite absorbing material. The absorbing material disclosed herein has the outstanding advantages of thin coating, light weight, and strong electromagnetic wave absorbing property, especially having the wave absorption (reflectivity) of -35 dB on 5.5 GHz electromagnetic wave, and is a novel radar absorbing material which has an application prospect.
Description
Technical field
The invention belongs to the absorbing material technical field, particularly the compound absorbing material of conductive polymer-magnetic material.
Background technology
Absorbing material is can absorb to project its surperficial electromagnetic wave energy, and changes a class material of heat energy into by the loss of material.In recent years, along with the expansion to radar absorbing research and deeply, various novel wave-absorbing materials continue to bring out, and are intended to improve the existence, prominent anti-of stealthy weapon, especially the deep strike ability.Meeting that material (layer) is thin, the aspect such as (matter) light, (frequently) is wide, (absorbing property) strong, conductive polymers, as a kind of novel absorbing material, has good application prospect.
Conductive polymers is that a class has the process chemistry of pi-conjugated backbone or the polymer materials that electrochemical doping can conduct electricity.The electrical loss of utilizing it to have, can be used as absorbing material etc., caused people's concern, especially in order further to improve absorption intensity and to expand, absorbs frequency range, usually prepares the matrix material of conductive polymers and magneticsubstance as absorbing material.
CN03117132.X discloses the conductive polymers polyaniline and has been coated on magnetic particle Fe
3o
4, Fe
2o
3, Co
2o
3, NiO is upper, has electroconductibility and magnetic, provided the saturation magnetization value, but without the absorbing property data.CN98111335.X discloses electrochemical method and has prepared polypyrrole/ferrite/composite polypyrrole film, has electroconductibility and magnetic, provided electric conductivity, tensile strength, the saturation magnetization value of film, but it does not provide the absorbing property data yet.CN03121536.X and CN200410009428.9 disclose respectively Fe, Co, Ni powder and the electrically conductive polyaniline of soft magnetic metal particle Fe, Co, Ni upper coating polyaniline and 95% and organic binder bond blend as suction ripple and electromagnetic shielding material, preferably reach-17dB of reflectivity, be less than the 1.5GHz frequency range, shielding is higher than 50dB.Document Composites Science and Technology (2010,70,909-915) reported a-FeO (OH)/PPY mixture microwave absorbing property, be preferably-17dB.
Poly-(3,4 dioxoethyls) thiophene (PEDOT) is in conductive polymers family, there is high conductivity, low band gaps width, outstanding stability, the inventor discloses the PEDOT microballoon as absorbing material in CN200810112079.1, reflectivity is-21dB, PEDOT and magnetic composite as the absorbing material aspect there are no document and patent report.
Summary of the invention
The purpose of this invention is to provide a kind of function solenoid that has concurrently, coating is thinner, lighter weight, the very strong compound absorbing material of conductive polymer-magnetic material of absorption.
A further object of the present invention is to provide the a-ferrite (a-FeO (OH)) of the absorbing material compound for the preparation of conductive polymer-magnetic material/poly-(3,4-dioxoethyl) thiophene (PEDOT) composite nanorod and preparation method.
The compound absorbing material of conductive polymer-magnetic material of the present invention is by a-ferrite (a-FeO (OH))/poly-(3, the 4-dioxoethyl) organic binder bonds such as thiophene (PEDOT) composite nanorod and epoxy resin or urethane form, wherein the quality percentage composition in a-ferrite (a-FeO (OH))/poly-(3,4-dioxoethyl) thiophene (PEDOT) composite nanorod absorbing material compound at conductive polymer-magnetic material is 30～80%.
Described a-ferrite (a-FeO (OH))/poly-(3,4-dioxoethyl) thiophene (PEDOT) composite nanorod is the monocrystalline feature, and its diameter is between 5nm～50nm, and specific conductivity is 1 * 10
-3～1 * 10
-1between S/cm, saturation magnetization is 15～60emu/g.
Described epoxy resin can be commercially available epoxy resin-based paint.
Described urethane can be commercially available polyurethane paint.
The preparation method of the absorbing material that conductive polymer-magnetic material of the present invention is compound is: by a-ferrite (a-FeO (OH))/poly-(3,4 dioxoethyls) thiophene (PEDOT) composite nanorod is dispersed in the organic binder bonds such as epoxy resin or urethane, obtain the compound absorbing material of described conductive polymer-magnetic material, wherein the quality percentage composition in a-ferrite (a-FeO (OH))/poly-(3,4-dioxoethyl) thiophene (PEDOT) composite nanorod absorbing material compound at conductive polymer-magnetic material is 30～80%.
Prepared by single stage method by the a-ferrite in the present invention (a-FeO (OH))/poly-(3,4 dioxoethyl) thiophene (PEDOT) composite nanorod, the method comprises the following steps:
1) the persulfate oxidation agent is joined in the deionized water in container, stirring and dissolving, obtaining volumetric molar concentration is 1 * 10
-4mol/L～1 * 10
-2the persulfate solution of mol/L, making the persulfate solution total amount is 100ml, under agitation condition, adds 3 of 0.1～1ml, 4-dioxoethyl thiophene; Under agitation condition, drip again ferric salt solution 10～30ml of 0.8mol/L, stir (being generally 10～15 minutes), drip again divalent iron salt solution 10～30ml of 0.8mol/L, stir (being generally 10～15 minutes), pass into rare gas element (as nitrogen) in solution, drip the ammoniacal liquor that the 10ml mass concentration is 25%; At room temperature continue stirring reaction (being generally about 2～8 hours), obtain the black emulsion that contains a-ferrite (a-FeO (OH))/poly-(3,4-dioxoethyl) thiophene (PEDOT) composite nanorod;
2) by step 1) obtain contain a-ferrite (a-FeO (OH))/poly-(3, the 4-dioxoethyl) black emulsion centrifugation in the whizzer of 8000～10000rpm (being generally 8～10 minutes) of thiophene (PEDOT) composite nanorod, remove unreacted reactant, supernatant liquid is outwelled, the black precipitate obtained again is dispersed in the mixed solvent of water that volume ratio is 1: 1 and ethanol washing and carries out centrifugation by above-mentioned centrifugal condition, the repeated centrifugation washing operation, until supernatant liquid is colourless, the black precipitate finally obtained is 80 ℃ of lower vacuum-dryings 24 hours in temperature, obtain black powder, above-mentioned black powder is the a-ferrite described in the present invention (a-FeO (OH))/poly-(3,4-dioxoethyl) thiophene (PEDOT) composite nanorod.
Described a-ferrite (a-FeO (OH))/poly-(3,4-dioxoethyl) thiophene (PEDOT) composite nanorod is the monocrystalline feature, and its diameter is between 5nm～50nm, and specific conductivity is 1 * 10
-3～1 * 10
-1between S/cm, saturation magnetization is 15～60emu/g.
Centrifuge speed during described centrifugation is 8000～10000rpm.
Described persulfate oxidation agent is ammonium persulphate, Potassium Persulphate, Sodium Persulfate or any mixture between them.
Described trivalent iron salt is iron nitrate, iron(ic) chloride or their mixture.
Described divalent iron salt is Iron nitrate, iron protochloride, ferrous sulfate or any mixture between them.
By conductive polymer-magnetic material of the present invention, compound absorbing material is coated on the aluminium sheet that the 3mm of 180mm * 180mm size is thick, and glue spread is 0.5kg/m
2～6kg/m
2, 2kg/m preferably
2～6kg/m
2, after coating, under 40～80 ℃, solidify dry; Test its performance, the compound absorbing material of conductive polymer-magnetic material of the present invention is on 2～18GHz frequency band at hertzian wave, has absorbing property, reach-35dB of maximum absorption of electromagnetic wave (reflectivity).
The present invention utilizes single stage method to prepare to have concurrently the a-ferrite (a-FeO (OH)) of electricity, magnetic function/poly-(3,4 dioxoethyl) thiophene (PEDOT) composite nanorod, using it as radar absorbing, is principal character of the present invention.It is thinner that absorbing material of the present invention has coating, and weight is lighter, the outstanding advantages that the rubber-ferrite performance is strong, and it is when the 5.5GHz frequency, and hertzian wave reaches maximum absorption (reflectivity)-35dB.
The accompanying drawing explanation
Fig. 1. the SEM photo of the a-ferrite (a-FeO (OH)) of the embodiment of the present invention 1 preparation/poly-(3,4-dioxoethyl) thiophene (PEDOT) composite nanorod.
Embodiment
Embodiment 1
1) the ammonium persulphate oxygenant is joined in the deionized water in container, stirring and dissolving, obtaining volumetric molar concentration is 1.0 * 10
-4the ammonium persulfate solution of mol/L, making the ammonium persulfate solution total amount is 100ml, under agitation condition, adds 3 of 0.1ml, 4-dioxoethyl thiophene stirs 10 minutes; And under agitation condition, then drip the liquor ferri trichloridi 10ml of 0.8mol/L, stir about 10 minutes, drip again the ferrous sulfate aqueous solution 30ml of 0.8mol/L, stir about 10 minutes, in solution, pass into nitrogen, drip the ammoniacal liquor that the 10ml mass concentration is 25%; At room temperature continue stirring reaction 4 hours, obtain the black emulsion that contains a-ferrite (a-FeO (OH))/poly-(3,4-dioxoethyl) thiophene (PEDOT) composite nanorod;
2) by step 1) obtain contain a-ferrite/poly-(3, the 4-dioxoethyl) the black emulsion of thiofuran composite nanorod centrifugation 8～10 minutes in 8000～10000rpm whizzer, remove unreacted reactant, supernatant liquid is outwelled, the black precipitate obtained again is dispersed in the mixed solvent of water that volume ratio is 1: 1 and ethanol washing and carries out centrifugation by above-mentioned centrifugal condition, the repeated centrifugation washing operation, until supernatant liquid is colourless, the black precipitate finally obtained is 80 ℃ of lower vacuum-dryings 24 hours in temperature, obtains black powder; Above-mentioned black powder is the a-ferrite described in the present invention (a-FeO (OH))/poly-(3,4-dioxoethyl) thiophene (PEDOT) composite nanorod.This composite nanorod is the monocrystalline feature, and its diameter is the 10nm left and right, and specific conductivity is 5.0 * 10
-3s/cm, saturation magnetization 56emu/g.
3) by step 2) in the a-ferrite (a-FeO (OH))/poly-(3 that obtains, 4 dioxoethyls) thiophene (PEDOT) composite nanorod is evenly dispersed in polyurethane paint, obtain the compound absorbing material of conductive polymer-magnetic material, a-ferrite (a-FeO (OH))/poly-(3 wherein, 4 dioxoethyls) mass percentage concentration in thiophene (PEDOT) the composite nanorod absorbing material compound at conductive polymer-magnetic material is 80%, it is coated on the aluminium sheet that the 3mm of 180mm * 180mm size is thick, and glue spread is 2.0kg/m
2, solidify drying after coating under 40 ℃, the about 1.5mm of thickness, wherein hertzian wave is at maximum absorption 14.8GHz place, and can reach-27dB of reflectivity, show excellent absorbing property.
Embodiment 2
1) the potassium persulfate oxidation agent is joined in the deionized water in container, stirring and dissolving, obtaining volumetric molar concentration is 5.0 * 10
-3the potassium persulfate solution of mo1/L, making the potassium persulfate solution total amount is 100ml, under agitation condition, adds 3 of 0.5ml, 4-dioxoethyl thiophene stirs 10 minutes; And under agitation condition, then drip the iron nitrate solution 20ml of 0.8mol/L, and stir about 15 minutes, then drip the ferrous chloride aqueous solution 20ml of 0.8mol/L, stir about 10 minutes, pass into nitrogen in solution, drip the ammoniacal liquor that the 10ml mass concentration is 25%; At room temperature continue stirring reaction 2 hours, obtain the black emulsion that contains a-ferrite (a-FeO (OH))/poly-(3,4-dioxoethyl) thiophene (PEDOT) composite nanorod;
2) by step 1) obtain contain a-ferrite/poly-(3, the 4-dioxoethyl) the black emulsion of thiofuran composite nanorod is according to embodiment 1 step 2) technical scheme implement, obtain a-ferrite (a-FeO (OH))/poly-(3,4-dioxoethyl) thiophene (PEDOT) composite nanorod.This composite nanorod is the monocrystalline feature, and its diameter is the 30nm left and right, and specific conductivity is 3.2 * 10
-2s/cm, saturation magnetization is 36emu/g.
3) by step 2) in the a-ferrite (a-FeO (OH))/poly-(3 that obtains, 4 dioxoethyls) thiophene (PEDOT) composite nanorod is evenly dispersed in epoxy resin-based paint, obtain the compound absorbing material of conductive polymer-magnetic material, a-ferrite (a-FeO (OH))/poly-(3 wherein, 4 dioxoethyls) mass percentage concentration in thiophene (PEDOT) the composite nanorod absorbing material compound at conductive polymer-magnetic material is 50%, it is coated on the aluminium sheet that the 3mm of 180mm * 180mm size is thick, and glue spread is 3.6kg/m
2, solidify drying after coating under 60 ℃, the about 3mm of thickness, wherein hertzian wave is at maximum absorption 7.2GHz place, and can reach-30dB of reflectivity, show excellent absorbing property.
Embodiment 3
1) the Sodium Persulfate oxygenant is joined in the deionized water in container, stirring and dissolving, obtaining volumetric molar concentration is 1.0 * 10
-2the Sodium Persulfate solution of mol/L, making Sodium Persulfate solution total amount is 100ml, under agitation condition, adds 3 of 1.0ml, 4-dioxoethyl thiophene,, stir 10 minutes; And under agitation condition, then drip the iron nitrate solution 30ml of 0.8mol/L, and stir about 15 minutes, then drip the ferrous nitrate aqueous solution 10ml of 0.8mol/L, stir about 15 minutes, pass into nitrogen in solution, drip the ammoniacal liquor that the 10ml mass concentration is 25%; At room temperature continue stirring reaction 8 hours, obtain the black emulsion that contains a-ferrite (a-FeO (OH))/poly-(3,4-dioxoethyl) thiophene (PEDOT) composite nanorod;
2) by step 1) obtain contain a-ferrite/poly-(3, the 4-dioxoethyl) the black emulsion of thiofuran composite nanorod is according to embodiment 1 step 2) technical scheme implement, obtain a-ferrite (a-FeO (OH))/poly-(3,4-dioxoethyl) thiophene (PEDOT) composite nanorod.This composite nanorod is the monocrystalline feature, and its diameter is the 43nm left and right, and specific conductivity is 9.8 * 10
-2s/cm, saturation magnetization is 23emu/g.
3) by step 2) in the a-ferrite (a-FeO (OH))/poly-(3 that obtains, the 4-dioxoethyl) thiophene (PEDOT) composite nanorod is evenly dispersed in epoxy resin-based paint, obtain the compound absorbing material of conductive polymer-magnetic material, a-ferrite (a-FeO (OH))/poly-(3 wherein, the 4-dioxoethyl) mass percentage concentration in thiophene (PEDOT) the composite nanorod absorbing material compound at conductive polymer-magnetic material is 30%, it is coated on the aluminium sheet that the 3mm of 180mm * 180mm size is thick, and glue spread is 4.5kg/m
2, solidify drying after coating under 70 ℃, the about 4mm of thickness, wherein at hertzian wave maximum absorption 5.5GHz place, can reach-35dB of reflectivity, show excellent absorbing property.
Embodiment 4
1) Sodium Persulfate, ammonium persulphate and potassium persulfate oxidation agent are joined in the deionized water in container, stirring and dissolving, the volumetric molar concentration that obtains Sodium Persulfate is 2.0 * 10
-3the volumetric molar concentration of mol/L, ammonium persulphate is 5.0 * 10
-3the volumetric molar concentration of mol/L, Potassium Persulphate is 5.0 * 10
-4the persulphate mixing solutions of mol/L, making persulphate mixing solutions total amount is 100ml, under agitation condition, adds 3 of 0.6ml, 4-dioxoethyl thiophene stirs 10 minutes; And under agitation condition, drip respectively again iron nitrate solution and each 10ml of ferric chloride Solution that concentration is all 0.8mol/L, stir about 15 minutes, drip respectively again each 10ml of the aqueous solution of Iron nitrate, iron protochloride and ferrous sulfate that concentration is all 0.8mol/L, stir about 15 minutes, pass into nitrogen in solution, drip the ammoniacal liquor that the 10ml mass concentration is 25%; At room temperature continue stirring reaction 6 hours, obtain the black emulsion that contains a-ferrite (a-FeO (OH))/poly-(3,4-dioxoethyl) thiophene (PEDOT) composite nanorod;
2) by step 1) obtain contain a-ferrite/poly-(3, the 4-dioxoethyl) the black emulsion of thiofuran composite nanorod is according to embodiment 1 step 2) technical scheme implement, obtain a-ferrite (a-FeO (OH))/poly-(3,4-dioxoethyl) thiophene (PEDOT) composite nanorod.This composite nanorod is the monocrystalline feature, and its diameter is the 30nm left and right, and specific conductivity is 4.2 * 10
-2s/cm, saturation magnetization is 50emu/g.
3) by step 2) in the a-ferrite (a-FeO (OH))/poly-(3 that obtains, the 4-dioxoethyl) thiophene (PEDOT) composite nanorod is evenly dispersed in the Polyurethane paint, obtain the compound absorbing material of conductive polymer-magnetic material, a-ferrite (a-FeO (OH))/poly-(3 wherein, the 4-dioxoethyl) mass percentage concentration in thiophene (PEDOT) the composite nanorod absorbing material compound at conductive polymer-magnetic material is 80%, it is coated on the aluminium sheet that the 3mm of 180mm * 180mm size is thick, and glue spread is 6.0kg/m
2, solidify drying after coating under 80 ℃, the about 4mm of thickness, wherein at hertzian wave maximum absorption 6.0GHz place, can reach-32dB of reflectivity, show excellent absorbing property.
Claims (6)
1. the absorbing material that conductive polymer-magnetic material is compound, it is characterized in that: the compound absorbing material of described conductive polymer-magnetic material is by α-FeO (OH)/poly-(3, the 4-dioxoethyl) thiofuran composite nanorod and epoxy resin or urethane organic binder bond form, wherein the quality percentage composition in α-FeO (OH)/poly-(3,4-dioxoethyl) thiofuran composite nanorod absorbing material compound at conductive polymer-magnetic material is 30～80%.
2. the compound absorbing material of conductive polymer-magnetic material according to claim 1, it is characterized in that: described α-FeO (OH)/poly-(3, the 4-dioxoethyl) thiofuran composite nanorod is the monocrystalline feature, and its diameter is between 5nm～50nm, and specific conductivity is 1 * 10
-3～1 * 10
-1between S/cm, saturation magnetization is 15～60emu/g.
3. the compound absorbing material of conductive polymer-magnetic material according to claim 1, it is characterized in that: the compound absorbing material of described conductive polymer-magnetic material is on 2～18GHz frequency band at hertzian wave, there is absorbing property, reach-35dB of hertzian wave maximum absorption.
4. the compound absorbing material of conductive polymer-magnetic material according to claim 1 and 2 is characterized in that: described α-FeO (OH)/poly-(3,4 dioxoethyl) thiofuran composite nanorod is prepared by following methods:
1) the persulfate oxidation agent is joined in the deionized water in container, stirring and dissolving, obtaining volumetric molar concentration is 1 * 10
-4mol/L～1 * 10
-2the persulfate solution of mol/L, making the persulfate solution total amount is 100ml, under agitation condition, add 3 of 0.1～1ml, divalent iron salt solution 10～30ml of 4-dioxoethyl thiophene, the ferric salt solution 10～30ml that drips 0.8mol/L and dropping 0.8mol/L, stir, in solution, pass into rare gas element, drip the ammoniacal liquor that the 10ml mass concentration is 25%; At room temperature continue stirring reaction, obtain the black emulsion that contains α-FeO (OH)/poly-(3,4-dioxoethyl) thiofuran composite nanorod;
2) by step 1) obtain contain α-FeO (OH)/poly-(3, the 4-dioxoethyl) black emulsion centrifugation in whizzer of thiofuran composite nanorod, remove unreacted reactant, supernatant liquid is outwelled, the black precipitate obtained is dispersed in washing centrifugation in the mixed solvent of water that volume ratio is 1: 1 and ethanol again, the repeated centrifugation washing operation, until supernatant liquid is colourless, the black precipitate finally obtained is 80 ℃ of lower vacuum-dryings in temperature, obtains black powder; Be described α-FeO (OH)/poly-(3,4-dioxoethyl) thiofuran composite nanorod;
Described trivalent iron salt is iron nitrate, iron(ic) chloride or their mixture;
Described divalent iron salt is Iron nitrate, iron protochloride, ferrous sulfate or any mixture between them.
5. the compound absorbing material of conductive polymer-magnetic material according to claim 4, it is characterized in that: centrifuge speed during described centrifugation is 8000～10000rpm.
6. the compound absorbing material of conductive polymer-magnetic material according to claim 4, it is characterized in that: described persulfate oxidation agent is ammonium persulphate, Potassium Persulphate, Sodium Persulfate or any mixture between them.
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| CN101186745A (en) * | 2007-11-09 | 2008-05-28 | 华南理工大学 | Method for preparing polythiophene-metal oxide nano composite material |
| 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 |
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| CN101186745A (en) * | 2007-11-09 | 2008-05-28 | 华南理工大学 | Method for preparing polythiophene-metal oxide nano composite material |
| 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 |
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