CN102295913A - High frequency electromagnetic wave absorption graphene and triiron tetroxide nanomaterials and Method - Google Patents

High frequency electromagnetic wave absorption graphene and triiron tetroxide nanomaterials and Method Download PDF

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CN102295913A
CN102295913A CN2011101584800A CN201110158480A CN102295913A CN 102295913 A CN102295913 A CN 102295913A CN 2011101584800 A CN2011101584800 A CN 2011101584800A CN 201110158480 A CN201110158480 A CN 201110158480A CN 102295913 A CN102295913 A CN 102295913A
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graphene
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triiron tetroxide
high frequency
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朱春玲
欧阳秋云
王铁石
陈玉金
马杨
齐立红
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哈尔滨工程大学
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Abstract

本发明提供的是一种吸收高频电磁波的石墨烯与四氧化三铁纳米材料及制法。 The present invention provides a high frequency electromagnetic wave absorption graphene triiron tetroxide nanomaterials and methods of manufacture. 将0.08-0.12克石墨烯加入280-320毫升水中溶解,再向溶液中加入0.05-0.15克Fe(NO3)3·9H2O得到混合溶液,将混合溶液在50摄氏度水浴条件下搅拌两个小时,然后将获得的沉淀物离心分离出来,用乙醇和蒸馏水清洗几次,在真空的环境下干燥;将获得的产物在氩气下加热到350摄氏度退火处理2个小时,冷却到室温后,得到石墨烯与四氧化三铁纳米复合材料。 0.08-0.12 g of the graphene added 280-320 ml of water were dissolved, was added again 0.05 to 0.15 g of Fe (NO3) 3 · 9H2O to obtain a mixed solution, the mixed solution was stirred at 50 ° C water bath for two hours, then the obtained precipitate was centrifuged off, washed several times with ethanol and distilled water, dried in a vacuum environment; product obtained was heated to 350 ° C annealing for 2 hours under argon, cooled to room temperature, to obtain graphene and triiron tetroxide nanocomposite. 利用本发明的材料制备的薄膜,在其厚度为3-6毫米时,吸收强度均达到了-20dB以下,对频率为5.5GHz和7GHz左右的微波吸收强度分别都超过了-30dB。 Film prepared using the material of the present invention, when a thickness of 3-6 mm, the absorption intensity reached -20dB or less, and a frequency of about 5.5GHz 7GHz microwave absorption intensity are respectively more than -30dB. 并且其吸收频率宽度很大,用料更少,制作的薄膜材料材质更轻,更有利于工业化生产,应用也更广泛。 And its large absorption frequency width, with less material, making the material lighter film material, more suitable for industrial production, more extensive applications.

Description

吸收高频电磁波的石墨烯与四氧化三铁纳米材料及制法 High frequency electromagnetic wave absorption graphene and triiron tetroxide nanomaterials and Method

技术领域 FIELD

[0001] 本发明涉及一种对高频电磁波具有强吸收特性的纳米复合材料,本发明也涉及一种对高频电磁波具有强吸收特性的纳米复合材料的制备方法。 [0001] The present invention relates to a nanocomposite material having strong absorption characteristics to high frequency electromagnetic waves, the present invention also relates to a method for preparing a nanocomposite having strong absorption characteristics of high frequency electromagnetic waves.

背景技术 Background technique

[0002] 当今时代,随着电子技术的发展,电磁波也充满了世界的任何一个角落。 [0002] the present era, with the development of electronic technology, electromagnetic waves also full of any corner of the world. 电磁波对环境的影响也日益增大,在机场,飞机航班因电磁波干扰无法起飞,在医院电话会干扰电子设备而导致诊断仪器误诊。 The impact of electromagnetic waves on the environment is increasing, at the airport, airplane flights can not take off due to electromagnetic interference in hospitals may interfere with electronic devices and diagnostic instruments led to misdiagnosis. 因此,治理电磁波污染,寻找一种能抵挡并削弱电磁波辐射的材料已成为当今一大课题。 Therefore, electromagnetic pollution control, looking for a weakening of electromagnetic radiation and can withstand the material has become a major issue today.

[0003] 随着纳米技术的发展,人们逐渐发现了众多纳米复合材料对电磁波的吸收有着良好的效果,比如四氧化三铁,作为一种磁性材料,纳米结构的四氧化三铁对一定频率范围的电磁波有着较好的吸收特性。 [0003] With the development of nanotechnology, many people gradually discovered nanocomposite has a good effect on the absorption of electromagnetic waves, such as triiron tetroxide, as a magnetic material, triiron tetroxide nanostructures on a range of frequencies the wave has a good absorption characteristics. 所以研究以四氧化三铁为基础的纳米复合材料用于微波的吸收屏蔽,引起了越来越多的国内外学者的关注。 So Absorption shield with four iron oxide-based nano-composite materials used in the microwave, causing more and more attention of domestic and foreign scholars. 然而由于现在已知的吸波材料仍存在着一些问题。 However, due to the absorbing material now known, there are still some problems.

[0004] 我们曾合成出具有良好微波吸收效果的四种复合纳米材料并已申请专利, 分别是四氧化三铁纳米颗粒(公开号CN101880065A)、四氧化三铁/氧化锡(公开号CN101586019)、四氧化三铁/氧化锌(公开号CN101767767A)以及四氧化三铁/铁/ 二氧化硅(公开号CN101514^2)。 [0004] We have synthesized four kinds having excellent microwave absorbing effect nanocomposite and patented, respectively, ferroferric oxide nanoparticles (Publication No. CN101880065A), ferroferric oxide / tin oxide (Publication No. CN101586019), triiron tetroxide / zinc oxide (Publication No. CN101767767A) and tri-iron tetroxide / iron / silicon dioxide (Publication No. CN101514 ^ 2). 但是以上材料都有着一定的不足,四氧化三铁纳米颗粒、四氧化三铁/氧化锡、四氧化三铁/氧化锌等具有较高的吸收强度和吸收频率带宽,但是它们需要较大的添加量,一般要大于40wt%。 However, the above materials have some disadvantages, ferroferric oxide nanoparticles, ferroferric oxide / tin oxide, tri-iron tetroxide / zinc oxide has a high absorption intensity and the absorption frequency bandwidth, but they require large add amount, typically greater than 40wt%. 添加量大,吸波体的重量会显著最大,限制了它们在某些领域的应用。 Amount added, the weight may be significantly absorber maximum limits their use in some areas. 因此,如何提高纳米复合吸波材料的吸收强度的同时,保证吸波体较轻是当前的主要技术难题之一。 Therefore, how to improve the absorption intensity nanocomposite absorbing materials while ensuring light absorber is one of the major technical problems.

发明内容 SUMMARY

[0005] 本发明的目的在于提供一种对高频电磁波具有强吸收特性的吸收高频电磁波具的石墨烯与四氧化三铁纳米复合材料。 [0005] The object of the present invention is to provide a high frequency electromagnetic wave absorption graphene having a strong absorption characteristic with triiron tetroxide Nanocomposites high frequency electromagnetic waves. 本发明的目的还在于提供一种操作简单、适合于工业化生产的吸收高频电磁波具的石墨烯与四氧化三铁纳米复合材料的制法。 Object of the present invention is to provide a simple, suitable for industrial production absorption graphene having high frequency electromagnetic wave with triiron tetroxide nano composite material manufacturing method.

[0006] 本发明的目的是这样实现的: [0006] The object of the present invention is implemented as follows:

[0007] 本发明的吸收高频电磁波具的石墨烯与四氧化三铁纳米复合材料是:先将0. 08-0. 12克石墨烯加入观0-320毫升水中形成溶液,再向溶液中加入0. 05-0. 15克Fe (NO3) 3 ·9Η20得到混合液,将混合溶液在50摄氏度下搅拌两个小时,然后将沉淀物分离出来,用乙醇和蒸馏水清洗,在真空的环境下干燥;在氩气下加热到350摄氏度退火处理2个小时所得到的石墨烯与四氧化三铁纳米复合材料。 [0007] Graphene has high frequency electromagnetic wave absorber of the present invention and Fe3O4 nanocomposite is: first graphene 0. 08-012 g of 0-320 ml of water was added to form a solution concept, the solution again was added 0. 05-0. 15 g Fe (NO3) 3 · 9Η20 obtained mixed solution, the mixed solution was stirred for two hours at 50 ° C, then the precipitate is separated out, washed with ethanol and distilled water, in a vacuum environment drying; heated to 350 ° C annealing treatment graphene 2 hours and the resulting Fe3O4 nanocomposite under argon.

[0008] 本发明的吸收高频电磁波的石墨烯与四氧化三铁纳米复合材料的制法为: [0008] The high frequency electromagnetic wave absorption graphene and Fe3O4 nanocomposite production method according to the present invention are:

[0009] (1)将乙醇和金属钠同时加入高压釜中,在220摄氏度下反应72小时,然后将所得的产物在空气中灼烧,最后将生产的产物用蒸馏水和乙醇清洗,得到石墨烯;[0010] (2)将0. 08-0. 12克石墨烯加入观0_320毫升水中溶解,再向溶液中加入0. 05-0. 15克狗(而3)3 ·9Η20得到混合溶液,将混合溶液在50摄氏度水浴条件下搅拌两个小时,然后将获得的沉淀物离心分离出来,用乙醇和蒸馏水清洗几次,在真空的环境下干燥; [0009] (1) metallic sodium and ethanol simultaneously added to the autoclave, reacted at 220 ° C for 72 hours and the resulting product was calcined in air to produce the final product was washed with distilled water and ethanol, to obtain graphene ;.. [0010] (2) 0.5 g of the graphene 08-012 View dissolved 0_320 ml of water was added, again the solution was added 0.5 05-015 Zerglings (and 3) 3 · 9Η20 obtain a mixed solution, the mixed solution was stirred at 50 ° C water bath for two hours, then separating the precipitate obtained was centrifuged out, washed several times with ethanol and distilled water, dried in a vacuum environment;

[0011] (3)将步骤⑵获得的产物在氩气下加热到350摄氏度退火处理2个小时,冷却到室温后,得到石墨烯与四氧化三铁纳米复合材料。 [0011] (3) The product of step ⑵ was heated under argon to 350 ° C annealing treatment 2 hours, cooled to room temperature, to obtain graphene triiron tetroxide nanocomposite.

[0012] 用本发明的石墨烯/四氧化三铁纳米复合材料制备20wt%石墨烯/四氧化三铁-石蜡复合薄膜材料,利用T/R同轴传输线测试其电磁参数。 [0012] The present invention graphene / triiron tetroxide prepared 20wt% graphene / triiron tetroxide nanocomposite - Paraffin composite film, using a T / R test electromagnetic coaxial transmission line parameters. 最后利用电磁传输线理论计算不同薄膜厚度的电磁波反射率。 Finally, the electromagnetic wave reflectance is calculated using an electromagnetic film thickness of different transmission line theory.

[0013] 本发明提供了一种对高频电磁波具有强吸收特性的石墨烯/四氧化三铁纳米复合材料的制备方法。 [0013] The present invention provides a method of preparing iron having a strong absorption characteristic of the graphene / tetroxide nanocomposite of high frequency electromagnetic waves. 利用石墨烯/四氧化三铁纳米复合材料制备的薄膜,在其厚度为3-6 毫米时,吸收强度均达到了-20dB以下,对频率为5. 5GHz和7GHz左右的微波吸收强度分别都超过了-30dB。 Using the graphene / tetroxide composite film prepared iron nm at a thickness of 3-6 mm, the absorption intensity reached -20dB or less, and a frequency of about 5. 5GHz 7GHz microwave absorption intensity are exceeded the -30dB. 并且其吸收频率宽度很大,大于_15dB吸收的频率范围达到了7GHz,兼具了四氧化三铁纳米颗粒、四氧化三铁/氧化锡、四氧化三铁/氧化锌等具有较高的吸收强度和四氧化三铁/铁/二氧化硅吸收的频率带宽较宽的优点。 Large absorption width and frequency, the frequency range larger than the absorbent _15dB 7GHz reached, both the iron tetroxide nanoparticles, ferroferric oxide / tin oxide, tri-iron tetroxide / zinc oxide having a high absorption wide frequency bandwidth and strength advantages triiron tetraoxide / iron / silicon dioxide absorption.

[0014] 本发明的另一个与以往微波吸收材料不同的优点是制备薄膜所需的材料比重很小,薄膜材料中石墨烯/四氧化三铁材料比例仅为20wt%,所以用料更少,制作的薄膜材料材质更轻,更有利于工业化生产,应用也更广泛。 [0014] Another of the present invention different from the conventional advantages of microwave absorbing material is required for preparation of the film material very small proportion of film material graphene / triiron tetroxide material ratio is only 20wt%, so less material, production of film material lighter materials, more conducive to industrial production, applications and more widely.

附图说明 BRIEF DESCRIPTION

[0015] 图1为石墨烯/四氧化三铁纳米复合材料的透射电镜图。 [0015] FIG. 1 is a graphene / TEM FIG composite nano-iron tetroxide.

[0016] 图2为石墨烯/四氧化三铁纳米复合材料的XRD图谱。 [0016] FIG. 2 is a graphene / triiron tetroxide XRD patterns of nano composites.

[0017] 图3为含20wt%石墨烯/四氧化三铁-石蜡复合物在不同厚度下的电磁波反射率。 [0017] FIG. 3 is alkylene containing 20wt% graphite / triiron tetroxide - Paraffin composite wave reflectivity at different thicknesses.

具体实施方式 Detailed ways

[0018] 下面举例对本发明做更详细地描述: [0018] The following examples of the present invention is described in more detail:

[0019] 本发明中的石墨烯可以采用文献(Nat.NanOteChnO1.2009,4,30)上的方法合成。 The method of the literature (Nat.NanOteChnO1.2009,4,30) Synthesis of graphene [0019] The present invention may be employed. 简单的说,就是将一定量的乙醇和金属钠同时加入高压釜中,在220摄氏度下反应72小时。 Simply put, is to a certain amount of ethanol and sodium metal simultaneously added to the autoclave, reacted at 220 ° C for 72 hours. 然后将所得的产物在空气中灼烧,最后将生产的产物用蒸馏水和乙醇清洗几次,便获得了石墨炼。 The resulting product was fired in air, the final products produced and washed several times with distilled water and ethanol, then mixing graphite obtained.

[0020] 实施例1 : [0020] Example 1:

[0021] (1)取一个500毫升容量的烧杯,加入280-320毫升水,然后加入0. 08-0. 12克石墨烯并且搅拌使其溶解分散,再向溶液中加入0. 05克!^e (NO3) 3 ·9Η20,并将获得的混合溶液在50摄氏度水浴条件下搅拌反应两个小时。 [0021] (1) takes a 500 ml volume beaker, 280-320 ml of water was added, followed by addition of 0. 08-0. 12 g graphene dispersion and stirred to dissolve, was added again 0.05 g! ^ e (NO3) 3 · 9Η20, and the reaction of the mixed solution was stirred for two hours at 50 ° C water bath. 反应结束后,冷却到室温并将获得的溶液中的沉淀物离心分离出来,用乙醇和蒸馏水清洗几次,在真空的环境下干燥。 After the reaction was cooled to room temperature and the precipitate was centrifuged out of the solution obtained, washed several times with ethanol and distilled water, dried in a vacuum environment.

[0022] (2)将获得的产物在氩气环境下加热到350摄氏度退火处理2个小时。 [0022] (2) The product obtained was heated under argon atmosphere to 350 ° C annealing for 2 hours. 冷却到室温后,石墨烯/四氧化三铁纳米复合材料便由上面的过程制得。 After cooling to room temperature, the graphene / triiron tetroxide nanocomposites obtained by the above process will be made.

[0023] 实施例2 : [0023] Example 2:

[0024] (1)取一个500毫升容量的烧杯,加入280-320毫升水,然后加入0. 08-0. 12克石墨烯并且搅拌使其溶解分散,再向溶液中加入0. 1克!^e(NO3)3 · 9H20,并将获得的混合溶液在50摄氏度水浴条件下搅拌反应两个小时。 [0024] (1) takes a 500 ml volume beaker, 280-320 ml of water was added, followed by addition of 0. 08-0. 12 g graphene dispersion and stirred to dissolve, was added again 0.1 g! ^ e (NO3) 3 · 9H20, and the reaction of the mixed solution was stirred for two hours at 50 ° C water bath. 反应结束后,冷却到室温并将获得的溶液中的沉淀物离心分离出来,用乙醇和蒸馏水清洗几次,在真空的环境下干燥。 After the reaction was cooled to room temperature and the precipitate was centrifuged out of the solution obtained, washed several times with ethanol and distilled water, dried in a vacuum environment.

[0025] (2)将获得的产物在氩气环境下加热到350摄氏度退火处理2个小时。 [0025] (2) The product obtained was heated under argon atmosphere to 350 ° C annealing for 2 hours. 冷却到室温后,石墨烯/四氧化三铁纳米复合材料便由上面的过程制得。 After cooling to room temperature, the graphene / triiron tetroxide nanocomposites obtained by the above process will be made.

[0026] 实施例3 : [0026] Example 3:

[0027] (1)取一个500毫升容量的烧杯,加入280-320毫升水,然后加入0. 08-0. 12克石墨烯并且搅拌使其溶解分散,再向溶液中加入0. 15克!^e (NO3) 3 ·9Η20,并将获得的混合溶液在50摄氏度水浴条件下搅拌反应两个小时。 [0027] (1) takes a 500 ml volume beaker, 280-320 ml of water was added, followed by addition of 0. 08-0. 12 g graphene dispersion and stirred to dissolve, was added again 0.15 g! ^ e (NO3) 3 · 9Η20, and the reaction of the mixed solution was stirred for two hours at 50 ° C water bath. 反应结束后,冷却到室温并将获得的溶液中的沉淀物离心分离出来,用乙醇和蒸馏水清洗几次,在真空的环境下干燥。 After the reaction was cooled to room temperature and the precipitate was centrifuged out of the solution obtained, washed several times with ethanol and distilled water, dried in a vacuum environment.

[0028] (2)将获得的产物在氩气环境下加热到350摄氏度退火处理2个小时。 [0028] (2) The product obtained was heated under argon atmosphere to 350 ° C annealing for 2 hours. 冷却到室温后,石墨烯/四氧化三铁纳米复合材料便由上面的过程制得。 After cooling to room temperature, the graphene / triiron tetroxide nanocomposites obtained by the above process will be made.

Claims (3)

1. 一种吸收高频电磁波具的石墨烯与四氧化三铁纳米材料,其特征是:是先将0. 08-0. 12克石墨烯加入观0-320毫升水中形成溶液,再向溶液中加入0. 05-0. 15克Fe (NO3) 3 ·9Η20得到混合液,将混合溶液在50摄氏度下搅拌两个小时,然后将沉淀物分离出来,用乙醇和蒸馏水清洗,在真空的环境下干燥;在氩气下加热到350摄氏度退火处理2个小时所得到的石墨烯与四氧化三铁纳米复合材料。 Graphene nano-iron tetroxide An absorbent material with a high frequency electromagnetic wave, characterized in that: a first graphene 0. 08-012 g of 0-320 ml of water was added to form a solution concept, solution again. was added 0. 05-0. 15 g Fe (NO3) 3 · 9Η20 obtained mixed solution, the mixed solution was stirred for two hours at 50 ° C, then the precipitate is separated out, washed with ethanol and distilled water, in a vacuum environment dried; heated to 350 ° C annealing treatment graphene 2 hours and the resulting Fe3O4 nanocomposite under argon.
2. 一种吸收高频电磁波的石墨烯与四氧化三铁纳米材料的制法,其特征是:(1)将0. 08-0. 12克石墨烯加入观0-320毫升水中溶解,再向溶液中加入0. 05-0. 15克Fe (NO3) 3 ·9Η20得到混合溶液,将混合溶液在50摄氏度水浴条件下搅拌两个小时,然后将获得的沉淀物离心分离出来,用乙醇和蒸馏水清洗几次,在真空的环境下干燥;(2)将步骤(1)获得的产物在氩气下加热到350摄氏度退火处理2个小时,冷却到室温后,得到石墨烯与四氧化三铁纳米复合材料。 A high frequency electromagnetic wave absorption graphene and triiron tetroxide nanomaterial production method, characterized in that: (1) 0.5 g of the graphene 08-012 0-320 ml of water was added to dissolve View, then was added 0. 05-0. 15 g Fe (NO3) 3 · 9Η20 solution to obtain a mixed solution, the mixed solution was stirred at 50 ° C water bath for two hours, then separating the precipitate obtained by centrifugation, washed with ethanol and washed several times with distilled water, and dried in a vacuum environment; product (2) in step (1) was heated to 350 ° C annealing for 2 hours under argon, cooled to room temperature, to obtain graphene triiron tetroxide nanocomposites.
3.根据权利要求2所述的吸收高频电磁波的石墨烯与四氧化三铁纳米材料的制法,其特征是所述的石墨烯是采用如下方法制备的:将乙醇和金属钠同时加入高压釜中,在220 摄氏度下反应72小时,然后将所得的产物在空气中灼烧,最后将生产的产物用蒸馏水和乙醇清洗,得到石墨烯。 The high frequency electromagnetic wave absorption graphene and triiron tetroxide nanomaterial production method according to claim 2, wherein the graphene is prepared by the following method: Ethanol added simultaneously and high-pressure sodium metal kettle, for 72 hours at 220 ° C, and the resulting product was calcined in air to produce the final product was washed with distilled water and ethanol, to obtain graphene.
CN2011101584800A 2011-06-14 2011-06-14 High frequency electromagnetic wave absorption graphene and triiron tetroxide nanomaterials and Method CN102295913A (en)

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CN102553593A (en) * 2012-01-10 2012-07-11 常州大学 Method for preparing magnetic nanometer ferroferric oxide-graphene composite catalyst
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CN103540291B (en) * 2013-08-09 2015-05-13 牡丹江师范学院 Layered three-dimensional graphene/gamma-ferric oxide ferromagnetic nanosheet array and synthetic method thereof
CN104084575A (en) * 2014-06-30 2014-10-08 北京师范大学 Cubic phase cobalt/graphene composite material, preparation method and microwave absorbing property
CN104084575B (en) * 2014-06-30 2016-03-23 北京师范大学 Emission in Cubic cobalt/graphene composite material, preparation method and absorbing property
CN104117683A (en) * 2014-07-01 2014-10-29 北京师范大学 Hexagonal phase nickel-cobalt alloy nanocluster-graphene composite material and preparation method and application thereof
CN104043840A (en) * 2014-07-01 2014-09-17 北京师范大学 Cubic-phase cobalt-nickel alloy nano-cluster-graphene composite material and manufacturing method and purpose thereof
CN104043840B (en) * 2014-07-01 2016-03-23 北京师范大学 Emission in Cubic cobalt-nickel alloy nano-cluster-graphene composite material, Preparation Method And The Use
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