CN103347377A - Method for preparing graphene/Co3O4 wave-absorbing material through hydrothermal method - Google Patents

Method for preparing graphene/Co3O4 wave-absorbing material through hydrothermal method Download PDF

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Publication number
CN103347377A
CN103347377A CN201310229708XA CN201310229708A CN103347377A CN 103347377 A CN103347377 A CN 103347377A CN 201310229708X A CN201310229708X A CN 201310229708XA CN 201310229708 A CN201310229708 A CN 201310229708A CN 103347377 A CN103347377 A CN 103347377A
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graphene
co3o4
wave
rgo
solution
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CN201310229708XA
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黄英
张伟
刘攀峰
赵丽岩
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Northwestern Polytechnical University
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Northwestern Polytechnical University
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Abstract

The invention provides a method for preparing a graphene/Co3O4 wave-absorbing material through a hydrothermal method. Graphene/Co3O4 nanometer materials and paraffin are mixed evenly, wherein the mass ratio of the graphene/Co3O4 nanometer materials to the paraffin is 1: 1. The mixed materials are pressed into an annular die which is 2.0mm in height, 7.0mm in outer diameter and 3.0mm in inner diameter to form a sample, the control thickness is 3.3mm, frequency is 13.8GHz, and the wave-absorbing performance can reach 43.7dB to the best. The graphene/Co3O4 nanocomposite is prepared according to the two-step method. The testing result shows that oxygen-containing functional groups of the graphite oxide in the RGO-Co3O4 nanometer materials are greatly reduced, GO is revivified to RGO, the formed Co3O4 nanometer particles are distributed on the surface of the RGO, and the grain diameter of each particle ranges from 5 nanometers to 15 nanometers.

Description

A kind of Hydrothermal Preparation Graphene/Co 3O 4The method of absorbing material
Technical field
The present invention relates to the extraordinary material of a kind of absorbing property, relate to the good Graphene/Co of a kind of absorbing property of a kind of Hydrothermal Preparation 3O 4Material.
Background technology
Graphene be a kind of have the bi-dimensional cellular nanostructure, by single carbon atom closely rearrange new carbon, it has bigger specific area, good conductivity, mechanical stability and thermal stability, therefore all is widely used at aspects such as electronic equipment, capacitor, compound enhancings.
We have prepared Graphene/Co with two-step method 3O 4(RGO-Co 3O 4) nano material and be applied to inhale the ripple application facet first.Utilize XRD, TEM is, and prepared nano material characterizes, and we are expected to possess application prospect widely at super capacitor material, electrode material and absorbing material etc. at the nano composite material of preparation.
Chinese invention patent---application number is that CN102702929A relates to " a kind of chiral polyaniline antiradar coatings and preparation method ".The antiradar coatings absorbing property that makes with this method is not very outstanding, and about coating thickness 2mm, the 8-18GHz average reflectance is-10.124dB.
Summary of the invention
For fear of the deficiencies in the prior art part, the present invention proposes the good Graphene/Co of a kind of absorbing property of a kind of Hydrothermal Preparation 3O 4Material has prepared Graphene/Co with two step method 3O 4(RGO-Co 3O 4) nano composite material.
Technical scheme
A kind of Hydrothermal Preparation Graphene/Co 3O 4The method of absorbing material is characterized in that step is as follows:
Step 1:0.1g Graphene adds ultrasonic 2h in the 100ml water, and adding 10ml concentration is 140g/L CoCl 26H 2The O aqueous solution and 10ml concentration are to pour in the teflon-lined autoclave after the 94g/L NaOH aqueous solution stirs 2h;
Step 2: add the 4ml mass fraction in the autoclave and be 30% H 2O 2, and be placed in 160 ℃ of baking ovens and react 24h, the product with gained after the room temperature cooling spends deionised water for several times and is made into 100ml solution;
Step 3: be that 80% hydrazine hydrate solution adds above-mentioned solution with the 0.2ml mass fraction, in 95 ℃ behind the reaction 12h with ethanol and deionized water washing for several times, then with products therefrom in vacuum drying chamber 60 ℃ place 24h, namely obtain required Graphene/Co 3O 4Nano composite material;
Above-mentioned addition is a requirement of preparation.
Supersonic frequency control is at 45HZ in the described step 1, and ultrasonic time length is uniformly dispersed it.
Beneficial effect
A kind of Graphene/Co that the present invention proposes 3O 4The preparation method of nano wave-absorbing material is with Graphene/Co 3O 4Nano material is evenly mixed (mass ratio 1:1) with paraffin, and be pressed in the ring mould (high 2.0mm, external diameter 7.0mm, internal diameter 3.0mm) and make sample, control thickness 3.3mm, frequency 13.8GHz, absorbing property preferably reach-43.7dB.Prepared Graphene/Co with two step method of the present invention 3O 4(RGO-Co 3O 4) nano composite material, testing result shows: RGO-Co 3O 4The oxygen-containing functional group quantity of graphite oxide in the nano material (GO) significantly reduces, and GO has been reduced into Graphene (RGO); The Co that forms 3O 4Nano particle is distributed in the RGO surface, and its particle diameter is between 5-15nm.
Description of drawings
Fig. 1: the flow chart of the inventive method;
Fig. 2: Graphene/Co 3O 4The XRD spectra of nano wave-absorbing material;
Fig. 3: Graphene/Co 3O 4The TEM figure of nano wave-absorbing material;
Fig. 4: Graphene/Co 3O 4The absorbing property of nano wave-absorbing material.
Embodiment
Now in conjunction with the embodiments, accompanying drawing is further described the present invention:
1., the 0.1g Graphene adds ultrasonic 2h in the 100ml water embodiment 1:, adding 10ml concentration is 140g/LCoCl 26H 2The O aqueous solution and 10ml concentration are to pour in the teflon-lined autoclave after the 94g/L NaOH aqueous solution stirs 2h; 2., adding the 4ml mass fraction in the autoclave is 30% H 2O 2, and be placed in 160 ℃ of baking ovens and react 24h, the product with gained after the room temperature cooling spends deionised water for several times and is made into 100ml solution; 3., be that 80% hydrazine hydrate solution adds above-mentioned solution with the 0.1ml mass fraction, in 95 ℃ behind the reaction 12h with ethanol and deionized water washing for several times, then with products therefrom in vacuum drying chamber 60 ℃ place 24h, namely obtain required Graphene/Co 3O 4Nano composite material.
1., the 0.1g Graphene adds ultrasonic 2h in the 100ml water embodiment 2:, adding 10ml concentration is 140g/LCoCl 26H 2The O aqueous solution and 10ml concentration are to pour in the teflon-lined autoclave after the 94g/L NaOH aqueous solution stirs 2h; 2., adding the 4ml mass fraction in the autoclave is 30% H 2O 2, and be placed in 160 ℃ of baking ovens and react 24h, the product with gained after the room temperature cooling spends deionised water for several times and is made into 100ml solution; 3., be that 80% hydrazine hydrate solution adds above-mentioned solution with the 0.2ml mass fraction, in 95 ℃ behind the reaction 12h with ethanol and deionized water washing for several times, then with products therefrom in vacuum drying chamber 60 ℃ place 24h, namely obtain required Graphene/Co 3O 4Nano composite material.
1., the 0.1g Graphene adds ultrasonic 2h in the 100ml water embodiment 3:, adding 10ml concentration is 140g/LCoCl 26H 2The O aqueous solution and 10ml concentration are to pour in the teflon-lined autoclave after the 94g/L NaOH aqueous solution stirs 2h; 2., adding the 4ml mass fraction in the autoclave is 30% H 2O 2, and be placed in 160 ℃ of baking ovens and react 24h, the product with gained after the room temperature cooling spends deionised water for several times and is made into 100ml solution; 3., be that 80% hydrazine hydrate solution adds above-mentioned solution with the 0.2ml mass fraction, in 95 ℃ behind the reaction 24h with ethanol and deionized water washing for several times, then with products therefrom in vacuum drying chamber 60 ℃ place 24h, namely obtain required Graphene/Co 3O 4Nano composite material.

Claims (1)

1. Hydrothermal Preparation Graphene/Co 3O 4The method of absorbing material is characterized in that step is as follows:
Step 1:0.1g Graphene adds ultrasonic 2h in the 100ml water, and adding 10ml concentration is 140g/L CoCl 26H 2The O aqueous solution and 10ml concentration are to pour in the teflon-lined autoclave after the 94g/L NaOH aqueous solution stirs 2h;
Step 2: add the 4ml mass fraction in the autoclave and be 30% H 2O 2, and be placed in 160 ℃ of baking ovens and react 24h, the product with gained after the room temperature cooling spends deionised water for several times and is made into 100ml solution;
Step 3: be that 80% hydrazine hydrate solution adds above-mentioned solution with the 0.2ml mass fraction, in 95 ℃ behind the reaction 12h with ethanol and deionized water washing for several times, then with products therefrom in vacuum drying chamber 60 ℃ place 24h, namely obtain required Graphene/Co 3O 4Nano composite material;
Above-mentioned addition is a requirement of preparation.
CN201310229708XA 2013-06-08 2013-06-08 Method for preparing graphene/Co3O4 wave-absorbing material through hydrothermal method Pending CN103347377A (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104263317A (en) * 2014-09-26 2015-01-07 厦门大学 Method for synthesizing cobalt oxide/graphene composite wave-absorbing material
CN104673185A (en) * 2014-07-21 2015-06-03 西北工业大学 Method for preparing reduced graphene oxide/CoFe2O4/Ag composite wave-absorbing material
CN105632787A (en) * 2016-01-20 2016-06-01 安徽大学 Preparation method of cobaltosic oxide/graphene nano composite electrode material for super capacitor
CN105670560A (en) * 2016-01-08 2016-06-15 北京科技大学 Preparation method of nano-cobalt oxide/graphene composite wave-absorbing coating
CN106211728A (en) * 2016-07-10 2016-12-07 上海大学 A kind of graphene coated Fe3o4the composite wave-suction material preparation method of nano-particle
CN104252970B (en) * 2014-10-17 2017-01-04 武汉理工大学 Three-dimensional net structure Co3O4-Graphene@nickel cobalt double-hydroxide composite and its preparation method and application
CN107333460A (en) * 2017-06-30 2017-11-07 河北大学 A kind of preparation method of graphene-based metal composite absorbing material
CN107949266A (en) * 2017-12-27 2018-04-20 山东大学 A kind of three-dimensional porous flower-like structure cobalt/carbon nano composite electromagnetic wave absorption material and preparation method thereof
CN113068390A (en) * 2021-03-31 2021-07-02 燕山大学 Two-dimensional magnetic Fe3GeTe2Composite material of nanosheet and graphene nanosheet as well as preparation method and application of composite material
CN114105088A (en) * 2021-11-17 2022-03-01 哈尔滨工业大学(威海) Preparation method of graphite nanosheet composite cobaltosic oxide multilayer special-shaped hollow wave absorber

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CN101550003A (en) * 2009-04-22 2009-10-07 湖南大学 Nano-graphite alkenyl composite wave-absorbing material and method of preparing the same

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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104673185A (en) * 2014-07-21 2015-06-03 西北工业大学 Method for preparing reduced graphene oxide/CoFe2O4/Ag composite wave-absorbing material
CN104263317B (en) * 2014-09-26 2016-03-09 厦门大学 The synthetic method of a kind of cobalt oxide/Graphene composite wave-suction material
CN104263317A (en) * 2014-09-26 2015-01-07 厦门大学 Method for synthesizing cobalt oxide/graphene composite wave-absorbing material
CN104252970B (en) * 2014-10-17 2017-01-04 武汉理工大学 Three-dimensional net structure Co3O4-Graphene@nickel cobalt double-hydroxide composite and its preparation method and application
CN105670560A (en) * 2016-01-08 2016-06-15 北京科技大学 Preparation method of nano-cobalt oxide/graphene composite wave-absorbing coating
CN105632787A (en) * 2016-01-20 2016-06-01 安徽大学 Preparation method of cobaltosic oxide/graphene nano composite electrode material for super capacitor
CN106211728A (en) * 2016-07-10 2016-12-07 上海大学 A kind of graphene coated Fe3o4the composite wave-suction material preparation method of nano-particle
CN106211728B (en) * 2016-07-10 2019-04-02 上海大学 A kind of graphene coated Fe3O4The composite wave-suction material preparation method of nano particle
CN107333460A (en) * 2017-06-30 2017-11-07 河北大学 A kind of preparation method of graphene-based metal composite absorbing material
CN107949266A (en) * 2017-12-27 2018-04-20 山东大学 A kind of three-dimensional porous flower-like structure cobalt/carbon nano composite electromagnetic wave absorption material and preparation method thereof
CN107949266B (en) * 2017-12-27 2019-01-11 山东大学 A kind of three-dimensional porous flower-like structure cobalt/carbon nano composite electromagnetic wave absorption material and preparation method thereof
CN113068390A (en) * 2021-03-31 2021-07-02 燕山大学 Two-dimensional magnetic Fe3GeTe2Composite material of nanosheet and graphene nanosheet as well as preparation method and application of composite material
CN113068390B (en) * 2021-03-31 2022-07-01 燕山大学 Two-dimensional magnetic Fe3GeTe2Composite material of nanosheet and graphene nanosheet as well as preparation method and application thereof
CN114105088A (en) * 2021-11-17 2022-03-01 哈尔滨工业大学(威海) Preparation method of graphite nanosheet composite cobaltosic oxide multilayer special-shaped hollow wave absorber
CN114105088B (en) * 2021-11-17 2023-09-22 哈尔滨工业大学(威海) Preparation method of graphite nano-sheet composite cobaltosic oxide multi-layer special-shaped hollow wave absorber

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Application publication date: 20131009