CN105441029A - Ag@Fe3O4/reduced graphene oxide ternary composite wave absorbing material and preparation method thereof - Google Patents
Ag@Fe3O4/reduced graphene oxide ternary composite wave absorbing material and preparation method thereof Download PDFInfo
- Publication number
- CN105441029A CN105441029A CN201410439051.4A CN201410439051A CN105441029A CN 105441029 A CN105441029 A CN 105441029A CN 201410439051 A CN201410439051 A CN 201410439051A CN 105441029 A CN105441029 A CN 105441029A
- Authority
- CN
- China
- Prior art keywords
- absorbing material
- agfe
- redox graphene
- tri compound
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention discloses an Ag@Fe3O4/reduced graphene oxide ternary composite wave absorbing material and a preparation method thereof. The Ag@Fe3O4/reduced graphene oxide ternary composite wave absorbing material is prepared in a one-step manner through a solvothermal reaction with graphite oxide, iron nitrate nonahydrate and silver nitrate as a precursor. Ag@Fe3O4 composite nanoparticles prepared in the invention are directly loaded on reduced graphene oxide (RGO), and the Ag@Fe3O4 composite nanoparticles is a core-shell structure, and has a stable structure and good dispersion. The preparation method of the composite material has the advantages of simple process, low requirements on a device, high efficiency, short time, and overcoming of the disadvantages of tedious operation, high reaction temperature and uncontrollable structure commonly existing in present graphene composite material preparation methods. The Ag@Fe3O4/reduced graphene oxide ternary composite wave absorbing material has an excellent wave absorbing performance, and has a good application prospect in the field of wave absorbing materials.
Description
Technical field
The present invention relates to a kind of AgFe
3o
4/ redox graphene tri compound absorbing material and preparation method thereof, belongs to absorbing material technical field.
Background technology
Along with the fast development of electronic science and technology, following war has become the trial of strength of various new and high technology, electronic countermeasure and antielectronic countermeasures technique become the focus of information war, in order to improve the penetration ability of strategic weapon change system, strengthen existence and the fighting efficiency of militarization weapon, each main military country of the world is all in stealthyization of making great efforts its weaponry of development, therefore, stealthy technique has become one of important directions of World modernization military technique development, but, because configuration design is subject to the restriction of many working conditionss, the investigation and application of absorbing material has become the key breakthrough points of stealthy technique development.In addition, along with the high speed development of electronic technology, electronics, electric installation or other communication system spread all over the every field of the daily production of people, life already, while bringing great convenience to human lives, the environment that the electromagnetic radiation of generation is also depended on for existence to human health and the mankind causes serious threat.Moreover electromagnetic radiation also can cause space wave noise, thus disturb the normal work of the electronics in local area, cause equipment failure or industrial accident.Therefore, research and development absorbing material not only has important and far-reaching meaning to the development of Defence business, to improve human environment and the aspect such as industrial labor protection also has extremely important effect.
Graphene specific surface area is large, can adsorption particle, and there is good thermostability and chemical stability, be well suited for carrying out load nano particle as carrier, not only effectively can solve a nanoparticle dispersion difficult problem that is poor, that easily reunite, and people can be met on nanoscale, its stuctures and properties designed and optimize, thus prepare the graphene-based matrix material with specific composition, stuctures and properties, therefore Graphene composite wave-suction material becomes the study hotspot of Chinese scholars.
Document " MengZongetal.MaterialsLetters111 (2013) 188-191 " discloses a kind of multistep wet chemistry method that adopts and prepares RGO/Fe
3o
4the method of/Ag matrix material, by FeCl
24H
2o and FeCl
36H
2o joins in the graphite oxide aqueous solution, drips the NaOH aqueous solution and regulates pH of mixed to be 11, heats 2h and forms black precipitate, black precipitate be dissolved in deionized water, add Silver Nitrate, then add NaBH at 80 DEG C
4the aqueous solution, stirs 2h at 80 DEG C, adopts Magneto separate, obtains black precipitate.Fe
3o
4with Ag nanoparticle with mixing form load on redox graphene lamella, the method described in the document mainly has the following disadvantages: preparation process is loaded down with trivial details, time consumption and energy consumption.Document " ErlongMaetal.Materialsletters91 (2013) 209-212 " discloses one and prepares Fe
3o
4the method of/RGO, by Fe
3+, reduction-oxidation graphite ultrasonic dissolution wiring solution-forming in ethylene glycol, add two kinds of Surfactant SDSs (SDS) and Sodium dodecylbenzene sulfonate (SDBS) again, mixture stirs 1h at 60 DEG C, the NaOH aqueous solution is added in mixed solution, continue to stir 2h, be 7 by the mixture deionized water wash obtained to pH, put into 60 DEG C of dry 12h of loft drier, obtained powder is placed in tube furnace, 450 DEG C are heated in argon shield, 2h is kept to be cooled to 350 DEG C, pass into hydrogen and argon gas gas mixture keeps 30min, the powder obtained is Fe
3o
4/ RGO matrix material, through electromagnetic performance test, when this thickness of composite material is 2mm, in 14.3-18GHz reflection loss lower than-10dB, reaches maximum absorption for-22.2dB when 17.3GHz.This preparation method has the following disadvantages: need to add tensio-active agent, need high-temperature calcination, needs to use hydrogen to reduce, and preparation time is long, and preparation process is complicated, time consumption and energy consumption, and absorbing property is not good enough.
Summary of the invention
The object of the present invention is to provide a kind of AgFe
3o
4/ redox graphene tri compound absorbing material and preparation method thereof, this matrix material not only has the features such as quality is light, absorption is strong, bandwidth, and preparation process is simple.
The present invention is achieved through the following technical solutions:
A kind of AgFe
3o
4/ redox graphene tri compound absorbing material, has the AgFe of nucleocapsid structure
3o
4nanometer particle load forms described composite wave-suction material on redox graphene, wherein, and AgFe
3o
4in nanoparticle, Ag is core, Fe
3o
4for shell.
A kind of AgFe
3o
4the preparation method of/redox graphene tri compound absorbing material, its step is as follows:
(1) graphite oxide, Fe(NO3)39H2O and Silver Nitrate are formed dispersion liquid by ultrasonic disperse in ethylene glycol, then add anhydrous sodium acetate, stir and make it fully dissolve formation mixed solution;
(2) mixed solution is proceeded to reactor, adopt solvent-thermal method to prepare AgFe
3o
4/ redox graphene tri compound absorbing material.
The mass ratio of the graphite oxide described in step (1) and ethylene glycol is 1:892, the mass ratio of graphite oxide and Fe(NO3)39H2O is 1:(24.24 ~ 40.40), the mol ratio of Fe(NO3)39H2O and Silver Nitrate is 1:(0.15 ~ 0.6), the mol ratio of Fe(NO3)39H2O and anhydrous sodium acetate is 1:(7.5 ~ 10).
Solvent thermal reaction temperature described in step (2) is 180 ~ 220 DEG C, and the solvent thermal reaction time is 6 ~ 10h.
Compared with prior art, the present invention has following beneficial effect:
1, the present invention has prepared AgFe by a simple step solvent-thermal method
3o
4/ redox graphene tri compound absorbing material, AgFe
3o
4the direct load of core-shell structure nanometer particle on Graphene, without the need to adding tensio-active agent, without the need to inert atmosphere protections such as nitrogen.
2, preparation process of the present invention is simple, and preparation condition easily realizes, and conveniently accomplishes scale production.
3, the AgFe for preparing of the present invention
3o
4/ redox graphene tri compound absorbing material quality is light, wave absorbing efficiency is high, bandwidth, when thickness of composite material is 2mm, reflection loss reaches 3.1GHz lower than the frequency range of-10dB, reach maximum absorption-40.05dB when 11.9GHz, thickness of composite material is 1.5-5.0mm, and reflection loss reaches about 13.5GHz lower than the frequency range of-10dB, thickness of composite material is 4.0mm, when 4.5mm, 5.0mm, there is absorption peak at high and low frequency.
Accompanying drawing explanation
Fig. 1 is AgFe prepared by embodiment 1
3o
4/ redox graphene tri compound absorbing material XRD figure.
Fig. 2 is AgFe prepared by embodiment 1
3o
4/ redox graphene tri compound absorbing material TEM schemes.
Fig. 3 is AgFe prepared by embodiment 1
3o
4the absorbing property figure of/redox graphene tri compound absorbing material.
Embodiment
In conjunction with the embodiments, accompanying drawing is described further the present invention:
Embodiment 1
Be 1:892 by the mass ratio of graphite oxide and ethylene glycol, the mass ratio of graphite oxide and Fe(NO3)39H2O is 1:32.32, the mol ratio of Fe(NO3)39H2O and Silver Nitrate is 1:0.3, Fe(NO3)39H2O and anhydrous sodium acetate mol ratio be 1:8.75, take 0.05g graphite oxide, 1.616g Fe(NO3)39H2O and 0.2038g Silver Nitrate are dispersed in 40mL ethylene glycol by ultrasonic 1h and form dispersion liquid, then 2.87g anhydrous sodium acetate is added, stirring makes it fully dissolve formation mixed solution, pour in teflon-lined autoclave, be placed in 200 DEG C of baking oven reaction 8h, to be cooled to after room temperature by precipitation ethanol and deionized water wash for several times, then products therefrom is dry in vacuum drying oven, namely AgFe is obtained
3o
4/ redox graphene tri compound absorbing material.The AgFe prepared as can be seen from Figure 1
3o
4/ redox graphene tri compound absorbing material is without the existence of other impurity phase.As can be seen from Figure 2 at the loaded Ag Fe of redox graphene surface uniform
3o
4nanoparticle, and Ag and Fe
3o
4present obvious nucleocapsid structure.Powdered product in embodiment 1 is mixed at 80 DEG C with solid paraffin, internal diameter 3.04mm is pressed in particular manufacturing craft, external diameter 7.0mm, thickness is at the coaxial sample of 2 ~ 4mm, by vector network analyzer (Agilent, N5244A) test its absorbing property, test frequency is 2 ~ 18GHz.Fig. 3 is AgFe prepared by embodiment 1
3o
4the absorbing property of/redox graphene tri compound absorbing material.When thickness of composite material is 2mm, reflection loss reaches 3.1GHz lower than the frequency range of-10dB, maximum absorption-40.05dB is reached when 11.9GHz, thickness of composite material is 1.5-5.0mm, reflection loss reaches about 13.5GHz lower than the frequency range of-10dB, and thickness of composite material is 4.0mm, 4.5mm, during 5.0mm, there is absorption peak at high and low frequency.
Embodiment 2
Be 1:892 by the mass ratio of graphite oxide and ethylene glycol, the mass ratio of graphite oxide and Fe(NO3)39H2O is 1:24.24, the mol ratio of Fe(NO3)39H2O and Silver Nitrate is 1:0.15, Fe(NO3)39H2O and anhydrous sodium acetate mol ratio be 1:7.5, take 0.05g graphite oxide, 1.212g Fe(NO3)39H2O and 0.0764g Silver Nitrate are dispersed in 40mL ethylene glycol by ultrasonic 1h and form dispersion liquid, then 2.46g anhydrous sodium acetate is added, stirring makes it fully dissolve formation mixed solution, pour in teflon-lined autoclave, be placed in 180 DEG C of baking oven reaction 10h, to be cooled to after room temperature by precipitation ethanol and deionized water wash for several times, then products therefrom is dry in vacuum drying oven, namely AgFe3O4/ redox graphene tri compound absorbing material is obtained.
Embodiment 3
Be 1:892 by the mass ratio of graphite oxide and ethylene glycol, the mass ratio of graphite oxide and Fe(NO3)39H2O is 1:40.40, the mol ratio of Fe(NO3)39H2O and Silver Nitrate is 1:0.6, Fe(NO3)39H2O and anhydrous sodium acetate mol ratio be 1:0.6, take 0.05g graphite oxide, 2.02g Fe(NO3)39H2O and 0., 5096g Silver Nitrate is dispersed in 40mL ethylene glycol by ultrasonic 1h and forms dispersion liquid, then 3.28g anhydrous sodium acetate is added, stirring makes it fully dissolve formation mixed solution, pour in teflon-lined autoclave, be placed in 220 DEG C of baking oven reaction 6h, be cooled to room temperature and will precipitate rear ethanol and deionized water wash several, then products therefrom is dry in vacuum drying oven, namely AgFe3O4/ redox graphene tri compound absorbing material is obtained.
Claims (7)
1. an AgFe
3o
4/ redox graphene tri compound absorbing material, is characterized in that, has the AgFe of nucleocapsid structure
3o
4nanometer particle load forms described composite wave-suction material on redox graphene, wherein, and AgFe
3o
4in nanoparticle, Ag is core, Fe
3o
4for shell.
2. AgFe according to claim 1
3o
4/ redox graphene tri compound absorbing material, is characterized in that, described absorbing material is prepared by the following method:
(1) graphite oxide, Fe(NO3)39H2O and Silver Nitrate are formed dispersion liquid by ultrasonic disperse in ethylene glycol, then add anhydrous sodium acetate, stir and make it fully dissolve formation mixed solution;
(2) mixed solution is proceeded to reactor, adopt solvent-thermal method to prepare AgFe
3o
4/ redox graphene tri compound absorbing material.
3. AgFe according to claim 2
3o
4/ redox graphene tri compound absorbing material, it is characterized in that, in step (1), the mass ratio of graphite oxide and ethylene glycol is 1:892, the mass ratio of graphite oxide and Fe(NO3)39H2O is 1:(24.24 ~ 40.40), the mol ratio of Fe(NO3)39H2O and Silver Nitrate is 1:(0.15 ~ 0.6), the mol ratio of Fe(NO3)39H2O and anhydrous sodium acetate is 1:(7.5 ~ 10).
4. AgFe according to claim 2
3o
4/ redox graphene tri compound absorbing material, is characterized in that, the solvent thermal reaction temperature described in step (2) is 180 ~ 220 DEG C, and the solvent thermal reaction time is 6 ~ 10h.
5. an AgFe
3o
4the preparation method of/redox graphene tri compound absorbing material, is characterized in that, comprise the steps:
(1) graphite oxide, Fe(NO3)39H2O and Silver Nitrate are formed dispersion liquid by ultrasonic disperse in ethylene glycol, then add anhydrous sodium acetate, stir and make it fully dissolve formation mixed solution;
(2) mixed solution is proceeded to reactor, adopt solvent-thermal method to prepare AgFe
3o
4/ redox graphene tri compound absorbing material.
6. AgFe according to claim 5
3o
4the preparation method of/redox graphene tri compound absorbing material, it is characterized in that, in step (1), the mass ratio of graphite oxide and ethylene glycol is 1:892, the mass ratio of graphite oxide and Fe(NO3)39H2O is 1:(24.24 ~ 40.40), the mol ratio of Fe(NO3)39H2O and Silver Nitrate is 1:(0.15 ~ 0.6), the mol ratio of Fe(NO3)39H2O and anhydrous sodium acetate is 1:(7.5 ~ 10).
7. AgFe according to claim 5
3o
4the preparation method of/redox graphene tri compound absorbing material, is characterized in that, the solvent thermal reaction temperature described in step (2) is 180 ~ 220 DEG C, and the solvent thermal reaction time is 6 ~ 10h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410439051.4A CN105441029A (en) | 2014-08-29 | 2014-08-29 | Ag@Fe3O4/reduced graphene oxide ternary composite wave absorbing material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410439051.4A CN105441029A (en) | 2014-08-29 | 2014-08-29 | Ag@Fe3O4/reduced graphene oxide ternary composite wave absorbing material and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105441029A true CN105441029A (en) | 2016-03-30 |
Family
ID=55551686
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410439051.4A Pending CN105441029A (en) | 2014-08-29 | 2014-08-29 | Ag@Fe3O4/reduced graphene oxide ternary composite wave absorbing material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105441029A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107008456A (en) * | 2017-05-12 | 2017-08-04 | 河南师范大学 | A kind of biological assisted synthesizing method with bacteriostasis property photochemical catalyst |
| CN108097950A (en) * | 2017-12-25 | 2018-06-01 | 浙江理工大学 | A kind of nucleocapsid Ag@Fe3O4Complex microsphere, preparation method and applications |
| CN109569648A (en) * | 2018-10-25 | 2019-04-05 | 湖北省晴川生态工程技术有限公司 | A kind of method of ferrous acid silver nano material catalysis organic wastewater treatment through persulfate |
| CN109802127A (en) * | 2019-03-25 | 2019-05-24 | 东北大学 | A kind of preparation method of Ag doping ferriferrous oxide nano composite material |
| JP2019178039A (en) * | 2018-03-30 | 2019-10-17 | 学校法人関西学院 | Method for producing oxygen gas |
| CN113451783A (en) * | 2021-06-18 | 2021-09-28 | 西安交通大学 | Phase-change controllable composite wave absorber and preparation and performance regulation and control method thereof |
| CN113881869A (en) * | 2021-09-29 | 2022-01-04 | 西安热工研究院有限公司 | Silver nanowire and ferroferric oxide composite wave-absorbing material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103074619A (en) * | 2013-02-06 | 2013-05-01 | 上海应用技术学院 | Graphene oxide-silver compound particle and preparation method thereof |
| CN103305185A (en) * | 2013-06-08 | 2013-09-18 | 西北工业大学 | Method for preparing reduced-oxidized graphene/Fe3O4/Ag nano composite wave-absorbing material |
-
2014
- 2014-08-29 CN CN201410439051.4A patent/CN105441029A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103074619A (en) * | 2013-02-06 | 2013-05-01 | 上海应用技术学院 | Graphene oxide-silver compound particle and preparation method thereof |
| CN103305185A (en) * | 2013-06-08 | 2013-09-18 | 西北工业大学 | Method for preparing reduced-oxidized graphene/Fe3O4/Ag nano composite wave-absorbing material |
Non-Patent Citations (1)
| Title |
|---|
| 杨俊松等: "水热体系中四氧化三铁与氧化石墨烯复合纳米颗粒的合成", 《硅酸盐通报》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107008456A (en) * | 2017-05-12 | 2017-08-04 | 河南师范大学 | A kind of biological assisted synthesizing method with bacteriostasis property photochemical catalyst |
| CN107008456B (en) * | 2017-05-12 | 2020-03-31 | 河南师范大学 | Biologically-assisted synthesis method of photocatalyst with antibacterial performance |
| CN108097950A (en) * | 2017-12-25 | 2018-06-01 | 浙江理工大学 | A kind of nucleocapsid Ag@Fe3O4Complex microsphere, preparation method and applications |
| JP2019178039A (en) * | 2018-03-30 | 2019-10-17 | 学校法人関西学院 | Method for producing oxygen gas |
| JP7045665B2 (en) | 2018-03-30 | 2022-04-01 | 学校法人関西学院 | Oxygen gas manufacturing method |
| CN109569648A (en) * | 2018-10-25 | 2019-04-05 | 湖北省晴川生态工程技术有限公司 | A kind of method of ferrous acid silver nano material catalysis organic wastewater treatment through persulfate |
| CN109569648B (en) * | 2018-10-25 | 2021-05-18 | 湖北省晴川生态工程技术有限公司 | Method for treating organic wastewater by catalyzing persulfate through silver ferrite nano material |
| CN109802127A (en) * | 2019-03-25 | 2019-05-24 | 东北大学 | A kind of preparation method of Ag doping ferriferrous oxide nano composite material |
| CN113451783A (en) * | 2021-06-18 | 2021-09-28 | 西安交通大学 | Phase-change controllable composite wave absorber and preparation and performance regulation and control method thereof |
| CN113881869A (en) * | 2021-09-29 | 2022-01-04 | 西安热工研究院有限公司 | Silver nanowire and ferroferric oxide composite wave-absorbing material and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105441029A (en) | Ag@Fe3O4/reduced graphene oxide ternary composite wave absorbing material and preparation method thereof | |
| CN103305185B (en) | Method for preparing reduced-oxidized graphene/Fe3O4/Ag nano composite wave-absorbing material | |
| CN101475157B (en) | Preparation of lithium iron phosphate nano composite microsphere | |
| Wang et al. | Sulfur-polypyrrole/graphene multi-composites as cathode for lithium-sulfur battery | |
| CN107585758A (en) | A kind of graphene aerogel and its preparation method and application | |
| CN103173189A (en) | Method for preparing reduced graphene oxide/ferroferric oxide nano-grade wave-absorbing materials | |
| CN102842710A (en) | Preparation method of Co3O4/graphene nanocomposite material | |
| CN109678193B (en) | Preparation method of nano cerium oxide particles | |
| CN105338799A (en) | Nanocomposite made of magnetic-metal-doped multiwalled carbon nanotubes/tin dioxide | |
| Zhang et al. | Porous α-Fe2O3 nanoparticles encapsulated within reduced graphene oxide as superior anode for lithium-ion battery | |
| Zhang et al. | MoS2 coated hollow carbon spheres for anodes of lithium ion batteries | |
| CN105295832A (en) | Preparation method for reduced graphene oxide/Ni-Co ternary composite wave-absorbing material | |
| CN103450843A (en) | Preparation method of reduction-oxidation graphene/ferroferric oxide composite wave-absorbing hydrogel having three-dimensional structure | |
| CN108862366B (en) | Flake Cu2-xApplication of S nanocrystal as microwave absorbent and preparation method thereof | |
| CN105018029A (en) | Metallic nickel/graphene composite wave-absorbing material and preparation method thereof | |
| CN104403275A (en) | Modified grapheme/thermosetting resin composite material and preparation method thereof | |
| CN113697863B (en) | Ferroferric oxide/carbon nanosheet composite material with excellent electromagnetic wave absorption performance and preparation method and application thereof | |
| Lai et al. | Enhanced high-rate capability of the CN-doped TiO2 as anode material for lithium-ion battery | |
| CN103107313B (en) | Tin-based oxide/graphene composite material,preparation method and application thereof | |
| CN105293565A (en) | Preparing method for light-color doping nanometer electro-conductive zinc oxide powder | |
| CN109585831A (en) | A kind of composite material and preparation method and application of sandwich type structural | |
| CN105923625A (en) | Method for preparing single-oxide uniformly-loaded graphene quantum dots | |
| CN104004496A (en) | Preparation method of reduced graphene oxide/nickel oxide composite wave absorbing material | |
| CN103613759B (en) | A kind of MoO 3the preparation method of/polyaniline co-axial nano heterojunction | |
| Li et al. | Electrospun FeCo nanoparticles encapsulated in N-doped carbon nanofibers as self-supporting flexible anodes for lithium-ion batteries |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20160330 |