CN104401980A - Hydrothermal preparation method of Fe2O3-SnO2/graphene ternary composite nano-material - Google Patents

Hydrothermal preparation method of Fe2O3-SnO2/graphene ternary composite nano-material Download PDF

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CN104401980A
CN104401980A CN201410614928.9A CN201410614928A CN104401980A CN 104401980 A CN104401980 A CN 104401980A CN 201410614928 A CN201410614928 A CN 201410614928A CN 104401980 A CN104401980 A CN 104401980A
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graphene
composite nano
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CN104401980B (en
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张海娇
谭英杰
李立昂
朱学栋
徐静
焦正
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University of Shanghai for Science and Technology
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Abstract

The invention relates to a hydrothermal preparation method of a Fe2O3-SnO2/graphene ternary composite nano-material. The graphene ternary composite nano-material with a stable structure is prepared through the one-step hydrothermal method with graphene, iron chloride and stannous chloride as raw materials. A TEM spectrum shows that the prepared composite nano-material is formed by self-assembling sheet iron oxide nano-particles and two-dimensional graphene nano-sheets in a sheet-sheet combination mode, and the combination mode improves the structural stability of a graphene and metal oxide composite nano-material. More importantly, the graphene composite nano-material prepared through the method has potential application prospects in the fields of environment, energy and the like.

Description

Fe 2o 3-SnO 2the hydrothermal preparing process of/Graphene tri compound nano material
Technical field
The present invention relates to a kind of Sn 2+the Fe of guiding 2o 3-SnO 2the hydrothermal preparing process of/Graphene tri compound nano material.
Background technology
Graphene is sp 2 the two dimensional crystal material that the carbon atom of hydridization is interconnected to form, because of the excellent specific property such as carrier mobility, light transmission that it has larger specific surface area, cellular void structure, good heat conductivility, superpower conductivity, high physical strength, superelevation, just get more and more people's extensive concerning since Late Cambrian from 2004.In addition, as the nano level two-dimensional material of one, Graphene or well composite material carrier.Discoverer professor Geim of Graphene also once pointed out, Graphene the most direct Application Areas in future is exactly graphene composite material.In these matrix materials, with the most extensive with the compound research of metal oxide.Mainly because this type of matrix material is while the part excellent properties of maintenance Graphene own, also achieve the effective efficiency of Graphene, impart the new character of material and function, expanded it and further applied.
At present, along with deepening continuously of studying graphene composite material, also grow with each passing day about the report of Graphene as base load metal oxide nano-material.People can realize load is different on graphene nanometer sheet metal oxide nano-material (as Fe by different physico-chemical processes 2o 3, SnO 2, Fe 3o 4, Co 3o 4, ZnO 2, MnO 2, TiO 2deng).This binary graphene composite material can be good at playing Graphene and the respective performance of the metal oxide both of load on graphene nanometer sheet, and multi-field application can be realized by synergistic effect between the two, as battery, catalysis, energy storage, biological medicine etc., illustrate potential application prospect.Wherein, iron oxide nano material relies on that it is with low cost, environmental friendliness and the advantage such as resistance to corrosion is strong, shows one's talent, and be widely used in multiple fields in numerous metal oxide materials.
Summary of the invention
The object of the present invention is to provide a kind of Fe 2o 3-SnO 2the hydrothermal preparing process of/Graphene tri compound nano material, is characterized in that this composite nano materials achieves Graphene and is combined with the blade of matrix material: with sheet Graphene for substrate, above the similar rectangle sheet Fe of load 2o 3nanoparticle, SnO 2nanoparticle is dispersed in Fe with the form of fine particle 2o 3around nanoparticle, thus form constitutionally stable Fe 2o 3-SnO 2/ Graphene tri compound nano material.
For achieving the above object, the present invention adopts following technical scheme:
A. redox graphene is dissolved in deionized water, is mixed with the suspension liquid of 0.20 ~ 0.30 wt%;
The stannous chloride solution of to be b. the ferric chloride Solution of 0.12 mol/L and concentration by concentration be 0.07 mol/L joins in 28 ~ 42 mL step a gained suspension liquids successively, and supersound process 20 min, obtains mixing solutions; Wherein in mixed solution, the mass ratio of Graphene, iron(ic) chloride and tin protochloride is 1:0.16 ~ 0.35:0.1 ~ 0.26;
C. by step b gained mixing solutions at 180 DEG C of Water Under thermal response 1 ~ 24 h; Product is taken out, through the step such as centrifugal, washing, oven dry of routine, obtains Fe 2o 3-SnO 2/ Graphene tri compound nano material.
In technological process of the present invention, a small amount of Sn 2+add and can induce sheet Fe 2o 3the formation of nanoparticle, thus the mode that can be combined by blade with the Graphene of two dimension carries out effective compound.Compared with other, this mode is more firm, is more conducive to improving the resistance to overturning of matrix material in performance test.In addition, Sn 2+not only serve Fe 2o 3the pattern guide effect of nanoparticle, and unnecessary Sn 2+can graphenic surface be adsorbed on and by hydrothermal final load on graphene nanometer sheet surface, thus can successfully realize single stage method and prepare Fe 2o 3-SnO 2/ Graphene tri compound nano material.
Compared with prior art, the technology of the present invention has following remarkable advantage:
The inventive method has easy and simple to handle, and reaction conditions is gentle, and abundant raw material is easy to get, with low cost, productive rate advantages of higher.By the Graphene trielement composite material that this legal system is standby, pattern is homogeneous, Stability Analysis of Structures, can play the excellent specific property of each component in matrix material simultaneously, have broad application prospects in the field such as lithium ion battery, organic pollutant removal.
Accompanying drawing explanation
Fig. 1 is gained Fe in the embodiment of the present invention 1 2o 3-SnO 2the TEM picture of/Graphene tri compound nano material.
Fig. 2 is gained Fe in the embodiment of the present invention 1 2o 3-SnO 2the XRD spectra of/Graphene tri compound nano material.
Fig. 3 is gained Fe in the embodiment of the present invention 1 2o 3-SnO 2the Raman spectrogram of/Graphene tri compound nano material.
Fig. 4 is gained Fe in the embodiment of the present invention 4 2o 3the TEM picture of/Graphene binary composite nano material.
Embodiment
All embodiments all operate by the operation steps of technique scheme.The preparation method of graphene oxide used in the present invention refers to j. Am. Chem.Soc., 2008,130,5856-5857.
Embodiment 1
A. first Graphene is produced by existing known technology: first use Potassium Persulphate (K 2s 2o 8) and Vanadium Pentoxide in FLAKES (P 2o 5) etc. material Graphene is carried out pre-oxidation treatment in the vitriol oil.Use potassium permanganate (KMnO in concentrated sulfuric acid at low temperatures again 4) graphite is carried out fully oxidized.Finally carry out aftertreatment with dilute hydrochloric acid solution and can obtain graphene oxide (GO).With the graphene oxide of above-mentioned preparation for presoma, single-layer graphene nanometer sheet (rGO) can be prepared by pyrolysis reduction method;
B. accurately taking 0.05 g rGO with electronic balance is dissolved in 35 g deionized waters, ultrasonic 2 h, to prepare the rGO suspension liquid of stable homogeneous;
C. 600 μ l ferric chloride Solution (FeCl are accurately pipetted 36H 2o, 0.12 mol/L) and 450 μ l stannous chloride solution (SnCl 22H 2o, 0.07 mol/L) join above-mentioned rGO suspension liquid, after stirring for some time, supersound process 20 min;
D. above-mentioned mixing solutions is poured in band teflon-lined 150 ml autoclave, under 180 DEG C of conditions, react 24 h;
E., after having reacted, product is taken out from reactor, with deionized water and ethanol repetitive scrubbing, centrifugal after, dry at product 60 DEG C, obtain Fe prepared by the present invention 2o 3-SnO 2/ Graphene tri compound nano material.
The sample of gained is carried out physical property sign, and its partial results as shown in drawings.The gained matrix material Fe of tile that has been the graphene nanometer sheet area load of accordion 2o 3nanoparticle (250 nm × 95 about nm); In addition, its surface also attached to the extra small SnO of about 5 ~ 10 nm 2nanoparticle.
Embodiment 2: preparation process and the step of the present embodiment are substantially the same manner as Example 1, and difference is step C:
Accurately pipette 2 ml ferric chloride Solution (FeCl 36H 2o, 0.12 mol/L) and 1.5 ml stannous chloride solution (SnCl 22H 2o, 0.07 mol/L) join above-mentioned rGO suspension liquid.
Acquired results and embodiment 1 different, when increasing the consumption of source of iron and Xi Yuan by a certain percentage, the Fe of graphenic surface load 2o 3the pattern of nanoparticle has larger change, starts the Fe occurring strip 2o 3nanoparticle, and can not well be combined with graphene film due to this structure, reduce the stability of matrix material, after supersound process, have part Fe 2o 3nanoparticle obscission.
Embodiment 3: preparation process and the step of the present embodiment are substantially the same manner as Example 1, and difference is step C:
Accurately pipette 600 μ l ferric chloride Solution (FeCl 36H 2o, 0.12 mol/L) and 1.5 ml stannous chloride solution (SnCl 22H 2o, 0.07 mol/L) join above-mentioned rGO suspension liquid.
Acquired results and embodiment 1 have bigger difference.In obtained Graphene trielement composite material, the Fe of graphenic surface load 2o 3nanoparticle is long gradually, and the SnO of load on graphenic surface 2nanoparticle is showed increased also.
Comparative example
The preparation process of the present embodiment is identical with embodiment 1 with step, and difference is step C:
Accurately pipette 600 μ l ferric chloride Solution (FeCl 36H 2o, 0.12 mol/L) join above-mentioned rGO suspension liquid, do not add any Xi Yuan.
Acquired results is obviously different from embodiment 1.In obtained Graphene trielement composite material, the Fe of graphenic surface load 2o 3nanoparticle does not have the pattern of stable homogeneous, but occurs that larger particles shape is stacking, the graphene composite material after supersound process, the Fe of its graphenic surface 2o 3nanoparticle has partial exfoliation, and the Fe of the irregular pattern of particulate state is described 2o 3nanoparticle is combined instability with graphene nanometer sheet, describes a small amount of Sn simultaneously 2+existence, uniform sheet Fe can be induced 2o 3the generation of nanoparticle.
 
See accompanying drawing, Fig. 1 is the embodiment of the present invention 1 gained Fe 2o 3-SnO 2transmission electron microscope (TEM) picture of/Graphene tri compound nano material.Tem analysis: adopt Jeol Ltd. JEOL-200CX type transmission electron microscope observation material morphology.As can be seen from TEM picture, the Graphene tri compound nano material that the present invention obtains, maintains complete graphene film Rotating fields, and the surface uniform of Graphene is dispersed with rectangular pieces stratiform Fe 2o 3nanoparticle, and equally distributed extra small nanoparticle is SnO around it 2.
See accompanying drawing, Fig. 2 is the embodiment of the present invention 1 gained Fe 2o 3-SnO 2the XRD spectra of/Graphene tri compound nano material.XRD analysis: carry out on Japanese RigaKu D/max-2550 type X-ray diffractometer; Adopt CuK α diffraction.As we know from the figure, Fe 2o 3hematite-type Fe in the position of diffraction peak and standard spectrum 2o 3standard card (JCPDS No.33-0664) can well mate, prove the hematite-type Fe of well-crystallized 2o 3successfully load on graphene nanometer sheet.
See accompanying drawing, Fig. 3 is the embodiment of the present invention 1 gained Fe 2o 3-SnO 2raman spectrum (Raman) spectrogram of/Graphene tri compound nano material.Raman analyzes: the Invia Raman spectrometer adopting Reinshaw (Renishaw) company of Britain, its excitation wavelength is 514.5 nm, and sweep limit is 1000-1800 cm -1.As can be seen from Raman spectrogram, be positioned at 1349 cm -1with 1591 cm -1there is very strong absorption peak, be respectively characteristic peak D peak and the G peak of graphene carbon material.Compared with pure Graphene, the I of Graphene trielement composite material d/ I gchange to some extent, this illustrates that the disordering degree of Graphene changes to some extent, is mainly caused by the defect of materials grain boundaries, carbon atom space, interstitial carbon and disordered carbon arrangement etc. after the metal oxide nanoparticles introducing load.
See accompanying drawing, Fig. 4 is gained Fe in comparative example of the present invention 2o 3the TEM picture of/Graphene binary composite nano material.Therefrom known, fashionable when adding without any Xi Yuan, the Fe of load on graphene nanometer sheet 2o 3nanoparticle pattern heterogeneity, presents blocky-shaped particle and piles up, after material is carried out supersound process, and the Fe of load 2o 3nanoparticle has obscission, and Fe is described 2o 3the combination of nanoparticle and graphene film is also insecure, and the structural stability of material is not good.

Claims (1)

1. a Fe 2o 3-SnO 2the hydrothermal preparing process of/Graphene tri compound nano material, is characterized in that the concrete steps of the method are:
A. redox graphene is dissolved in deionized water, is mixed with the suspension liquid of 0.20 ~ 0.30 wt%;
The stannous chloride solution of to be b. the ferric chloride Solution of 0.12 mol/L and concentration by concentration be 0.07 mol/L joins in 28 ~ 42 mL step a gained suspension liquids successively, and supersound process 20 min, obtains mixing solutions; Wherein in mixed solution, the mass ratio of Graphene, iron(ic) chloride and tin protochloride is 1:0.16 ~ 0.35:0.1 ~ 0.26;
C. by step b gained mixing solutions at 180 DEG C of Water Under thermal response 1 ~ 24 h; Product is taken out, through the step such as centrifugal, washing, oven dry of routine, obtains Fe 2o 3-SnO 2/ Graphene tri compound nano material.
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CN105950109A (en) * 2016-04-29 2016-09-21 安徽理工大学 Reduced graphene oxide, tin dioxide and ferric oxide composite material
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
CN107381652A (en) * 2017-07-13 2017-11-24 济南大学 A kind of Sn with alcohol sensible effect2O3Nanometer sheet/α Fe2O3Nanocube heterojunction material
CN108034407A (en) * 2017-12-07 2018-05-15 上海电机学院 A kind of preparation method of absorbing material
CN108598403A (en) * 2018-04-16 2018-09-28 江西师范大学 The forming method of lithium ion battery transiton metal binary oxides negative material
CN109273675A (en) * 2018-08-03 2019-01-25 深圳市山木新能源科技股份有限公司 A kind of graphene composite material and preparation method thereof and negative electrode of lithium ion battery
CN110586100A (en) * 2019-10-08 2019-12-20 扬州大学 Fe2O3/FeO heterostructure and preparation method and application thereof
CN112964758A (en) * 2021-01-29 2021-06-15 浙江大学 Manganese dioxide nanosheet/titanium dioxide nanowire array composite resistance type sensor and preparation method and application thereof

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CN105529441A (en) * 2015-09-17 2016-04-27 上海大学 SnO<2>-TiO<2>@ graphene ternary composite nanomaterial and preparation method thereof
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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
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
CN107381652A (en) * 2017-07-13 2017-11-24 济南大学 A kind of Sn with alcohol sensible effect2O3Nanometer sheet/α Fe2O3Nanocube heterojunction material
CN107381652B (en) * 2017-07-13 2019-11-12 济南大学 A kind of Sn with alcohol sensible effect2O3Nanometer sheet/α-Fe2O3Nanocube heterojunction material
CN108034407A (en) * 2017-12-07 2018-05-15 上海电机学院 A kind of preparation method of absorbing material
CN108598403A (en) * 2018-04-16 2018-09-28 江西师范大学 The forming method of lithium ion battery transiton metal binary oxides negative material
CN108598403B (en) * 2018-04-16 2020-07-24 江西师范大学 Method for forming binary transition metal oxide cathode material of lithium ion battery
CN109273675A (en) * 2018-08-03 2019-01-25 深圳市山木新能源科技股份有限公司 A kind of graphene composite material and preparation method thereof and negative electrode of lithium ion battery
CN109273675B (en) * 2018-08-03 2020-10-23 深圳市山木新能源科技股份有限公司 Graphene composite material, preparation method thereof and lithium ion battery cathode
CN110586100A (en) * 2019-10-08 2019-12-20 扬州大学 Fe2O3/FeO heterostructure and preparation method and application thereof
CN112964758A (en) * 2021-01-29 2021-06-15 浙江大学 Manganese dioxide nanosheet/titanium dioxide nanowire array composite resistance type sensor and preparation method and application thereof

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