CN103043710B - A kind of at α-Fe 2o 3nanocrystal surface Heteroepitaxy nano SnO 2method - Google Patents
A kind of at α-Fe 2o 3nanocrystal surface Heteroepitaxy nano SnO 2method Download PDFInfo
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- CN103043710B CN103043710B CN201110315850.7A CN201110315850A CN103043710B CN 103043710 B CN103043710 B CN 103043710B CN 201110315850 A CN201110315850 A CN 201110315850A CN 103043710 B CN103043710 B CN 103043710B
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- nanocrystalline
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Abstract
The invention provides a kind of at α-Fe
2o
3nanocrystal surface Heteroepitaxy nano SnO
2method.By the α-Fe obtained in advance
2o
3nanocrystal is dispersed in Sn (OH)
6 2-ethanolic soln in, by solvent thermal reaction at α-Fe
2o
3nanocrystalline upper Heteroepitaxy nano SnO
2, form heterojunction semiconductor.Preparation method's process of the present invention is easy, cheaper starting materials, productive rate are high, is applicable to the various pattern of current reported in literature and the α-Fe of exposure
2o
3nanocrystalline, and the impact of the tensio-active agent do not remained by nanocrystal surface.
Description
Technical field
The present invention relates to the field of chemical synthesis.
Background technology
α-Fe
2o
3and SnO
2two kinds of widely used semiconductor materials, wherein α-Fe
2o
3band gap is 2.2eV, is a kind of narrow bandgap semiconductor material; And SnO
2band gap length reach 3.8eV, be a kind of wide bandgap semiconductor materials.The nanocrystalline of this bi-material has respective superiority all respectively in Application Areass such as photochemical catalysis, air-sensitive, solar cells.There is bibliographical information in recent years, the nanocrystalline Heterogeneous Composite of this bi-material is formed SnO
2/ α-Fe
2o
3nano heterojunction, its photoelectric properties will be better than single-phase nano crystalline.Such as, the magazine in British royal physical society " nanotechnology " (Nanotechnology, 19 (2008) 205603) once there is in 2008 one section of article report to synthesize SnO
2/ α-Fe
2o
3nano heterojunction, this heterojunction powder has very strong selective gas effect for ethanol; And 2011 also have one section of reported in literature to synthesize SnO on the magazine " crystal engineering design " (Crystengcomm, 13 (2011) 4486) of British royal chemistry meeting
2/ α-Fe
2o
3nano junction, this nano material visible ray according under can organic pollutant effectively in degradation water solution.In addition, the internationally famous magazine such as magazine " crystal growth design " (Crystal Growth & Design) and " nanometer " (ACS Nano) of American Chemical Society has all occurred in recent years about SnO
2/ α-Fe
2o
3the report of nano heterojunction.
The SnO that current document is reported
2/ α-Fe
2o
3the synthetic method of nano heterogeneous mixture is all two-step approach, namely first synthesizes Fe
2o
3or SnO
2single-phase nano crystalline, and then Heteroepitaxy to go out second-phase nanocrystalline.But the nanocrystalline pattern of first-phase of synthesis and exposure is different and surface usually remains certain tensio-active agent, whether these factors all can affect second-phase can successful Heteroepitaxy.At present, the method reported for specific pattern and exposure or specific tensio-active agent, can only synthesize the SnO of specific microstructure and pattern
2/ α-Fe
2o
3nano heterojunction, some even can only synthesize simple two-phase mixture (SnO
2and Fe
2o
3heterogeneous interface is not formed) between nanocrystalline.In addition, the needs that have of these synthetic methods are by high-temperature heat treatment; What have then needs by specific solvent or tensio-active agent, not yet has easy, the efficient and synthetic method with certain universality to occur at present.
As everyone knows, the microscopic appearance of nano material has a great impact its physical and chemical performance, if can develop a kind of efficient, easy and there is the synthetic method of certain universality (can synthesize a series of pattern), performance optimization and the application and development of this nano material will be contributed to.This patent proposes a kind of efficient, easy at various Fe
2o
3nanocrystalline upper Heteroepitaxy nano SnO
2, form SnO
2/ α-Fe
2o
3the synthetic method of nano heterojunction.The method is applicable to the Fe of various pattern and exposure
2o
3nanocrystalline, and the impact of the tensio-active agent do not remained by nanocrystal surface.
Summary of the invention
The present invention proposes a kind of efficient, easy at α-Fe
2o
3nanocrystal surface Heteroepitaxy nano SnO
2, form the method for semiconductor nano heterojunction.The present invention proposes synthetic method:
First, α-Fe is obtained by the mode of synthesizing voluntarily or buy
2o
3nanocrystalline (according to the obtainable α of current reported in literature-Fe
2o
3nanocrystallinely there are nanometer pseudo-cubic, spindle body, rhombohedron, nano-rings etc.); Take the SnCl that mol ratio is 1:6 ~ 60
4be dissolved in ethanol with NaOH, form Sn (OH)
6 2-ethanolic soln; By α-Fe
2o
3nanocrystallinely be scattered in Sn (OH)
6 2-in solution, α-Fe
2o
3with Sn (OH)
6 2-mol ratio be 1:1 ~ 50; Gained mixed solution is transferred in stainless steel cauldron, at the temperature of 180 ~ 240 DEG C, carries out solvent thermal reaction, more than 2 hours reaction times; Then, by high speed centrifugation collecting reaction product, namely SnO is obtained
2/ α-Fe
2o
3nano heterojunction powder.
The synthetic method that the present invention proposes, achieves SnO
2nanocrystalline at α-Fe
2o
3the heteroepitaxial growth of forerunner's nanocrystal surface, obtains the SnO of various pattern
2/ α-Fe
2o
3nano heterojunction.As shown in embodiment 1-5, the present invention is applicable to the α-Fe of various pattern
2o
3nanocrystalline, comprise the α-Fe of current reported in literature
2o
3nanometer pseudo-cubic, spindle body, rhombohedron, nano-rings etc.These nanocrystal surface remain different tensio-active agents, such as, nanometer pseudo-cubic remained on surface be polyvinylpyrrolidone; Spindle body remained on surface be phosphoric acid salt; Rhombohedron remained on surface be hexadecyl trimethyl ammonium bromide etc., and method of the present invention is by the impact of these residual tensio-active agents.Preparation method's process of the present invention is easy, cheaper starting materials, productive rate are high and suitability is strong.
Accompanying drawing explanation
Fig. 1 pseudo-cubic shape α-Fe
2o
3snO prepared by nanocrystalline and example 1
2/ α-Fe
2o
3(pseudo-cubic) nano heterojunction powder photo under an electron microscope: (a) α-Fe
2o
3nanocrystal, (b) nano heterojunction, illustration is the enlarged photograph of heterogeneous interface;
Fig. 2 spindle body shape α-Fe
2o
3snO prepared by nanocrystalline and example 2
2/ α-Fe
2o
3the Photomicrograph of (spindle body) nano heterojunction powder: (a) α-Fe
2o
3nanocrystal, (b) nano heterojunction;
Fig. 3 rhombohedron shape α-Fe
2o
3snO prepared by nanocrystalline and example 3
2/ α-Fe
2o
3the Photomicrograph of (rhombohedron) nano heterojunction powder: (a) α-Fe
2o
3nanocrystal, illustration is the nanocrystalline photo of rhombohedron amplified, (b) nano heterojunction;
Fig. 4 hollow ellipsoid shape α-Fe
2o
3snO prepared by nanocrystalline and example 4
2/ α-Fe
2o
3the Photomicrograph of (hollow ellipsoid) nano heterojunction powder: (a) α-Fe
2o
3nanocrystal, (b) nano heterojunction;
Fig. 5 ring-type α-Fe
2o
3snO prepared by nanocrystalline and example 5
2/ α-Fe
2o
3the Photomicrograph of (ring bodies) nano heterojunction powder: (a) α-Fe
2o
3nanocrystal, (b) nano heterojunction, illustration is the enlarged photograph of single heterojunction.
Embodiment
Example 1:SnO
2/ α-Fe
2o
3preparation, the appearance structure of (pseudo-cubic) nano heterojunction powder characterize
Nanometer pseudo-cubic shape α-Fe selected by this example
2o
3manocrystalline powders pattern is shown in Fig. 1 a, and its remained on surface has tensio-active agent polyvinylpyrrolidone.Take 0.087g SnCl
45H
2o and 0.267g NaOH is dissolved in (SnCl in 15mL ethanol
4be 1:6 with NaOH mole), obtain Sn (OH)
6 2-solution; Take 0.010g pseudo-cubic shape α-Fe
2o
3forerunner is nanocrystalline, and ultrasonic disperse is in prefabricated Sn (OH)
6 2-in solution, α-Fe
2o
3with Sn (OH)
6 2-mol ratio is 1:1; The suspension liquid of gained is transferred in the stainless steel cauldron of 25mL, in retort furnace, at 220 DEG C, carries out solvent thermal reaction 2 hours; Product is collected by high speed centrifugation; Product is used respectively deionized water and washing with alcohol 3 times, under vacuum drying oven, 50 DEG C of inner dryings 4 hours, namely obtain SnO
2/ α-Fe
2o
3(pseudo-cubic) nano heterojunction powder.
X-ray diffraction, transmission electron microscope and sem test result show, gained SnO
2/ α-Fe
2o
3nano heterogeneously become SnO
2nanometer rod heteroepitaxial growth is in α-Fe
2o
3pseudo-cubic surface, forms multistage SnO
2/ α-Fe
2o
3composite structure (see Fig. 1 b).As can be seen from figure b illustration, SnO
2nanocrystalline with α-Fe
2o
3between have the connection of lattice fringe, illustrate that these two kinds of semi-conductors define Nano semiconductor heterojunction, instead of simple mixture.
The material rate that following instance will change in formula, at different α-Fe
2o
3nanocrystalline upper Heteroepitaxy SnO
2nanocrystalline.
Example 2:SnO
2/ α-Fe
2o
3preparation, the appearance structure of (spindle body) nano heterojunction powder characterize
Nano-spun hammer body shape α-Fe selected by this example
2o
3manocrystalline powders pattern is shown in Fig. 2 a, and its remained on surface has tensio-active agent phosphoric acid salt.Take 0.870g SnCl
45H
2o and 26.700g NaOH is dissolved in (SnCl in 150mL ethanol
4be 1:60 with NaOH mole), obtain Sn (OH)
6 2-solution; Take 0.010g spindle shaped alpha-Fe
2o
3forerunner is nanocrystalline, and ultrasonic disperse is in prefabricated Sn (OH)
6 2-(α-Fe in solution
2o
3with Sn (OH)
6 2-mol ratio is 1:8); The suspension liquid of gained is transferred in the stainless steel cauldron of 25mL, in retort furnace, carries out solvent thermal reaction 2 hours in 200 DEG C; Product is collected by high speed centrifugation; Product is used respectively deionized water and washing with alcohol 3 times, in 50 DEG C of dryings 4 hours in vacuum drying oven, obtain SnO
2/ α-Fe
2o
3(spindle body) nano heterojunction powder.
X-ray diffraction, transmission electron microscope and sem test result show, gained SnO
2/ α-Fe
2o
3nano heterogeneously become SnO
2nanocrystalline heteroepitaxial growth is in α-Fe
2o
3spindle body surface, by α-Fe
2o
3spindle body forerunner plane of crystal covers (see Fig. 2 b) completely.
Example 3:SnO
2/ α-Fe
2o
3preparation, the appearance structure of (rhombohedron) nano heterojunction powder characterize
Nanometer rhombohedron shape α-Fe selected by this example
2o
3manocrystalline powders pattern is shown in Fig. 3 a, and its remained on surface has tensio-active agent hexadecyl trimethyl ammonium bromide.Take 0.870g SnCl
45H
2o and 26.700g NaOH is dissolved in (SnCl in 75mL ethanol
4be 1:60 with NaOH mole); Take 0.010g rhombohedron shape α-Fe
2o
3nanocrystalline, ultrasonic disperse is in prefabricated Sn (OH)
6 2-(α-Fe in dilute solution
2o
3with Sn (OH)
6 2-mol ratio is 1:20); The suspension liquid of gained is transferred in the stainless steel reaction of 25mL, in retort furnace, carries out solvent thermal reaction 3 hours in 240 DEG C; Product is collected by high speed centrifugation; Product is used respectively deionized water and washing with alcohol 3 times, in 50 DEG C of dryings 4 hours in vacuum drying oven, namely obtain SnO
2/ α-Fe
2o
3(rhombohedron) nano heterojunction powder.
X-ray diffraction, transmission electron microscope and sem test result show, gained SnO
2/ α-Fe
2o
3nano heterogeneously become SnO
2nanometer stub heteroepitaxial growth is in α-Fe
2o
3rhombohedron surface (as Fig. 3 b).
Example 4:SnO
2/ α-Fe
2o
3preparation, the appearance structure of (hollow ellipsoid) nano heterojunction powder characterize
Hollow ellipsoid shape α-Fe selected by this example
2o
3manocrystalline powders pattern is shown in Fig. 4 a, and its remained on surface has phosphoric acid salt.Take 0.870g SnCl
45H
2o and 13.300g NaOH is dissolved in (SnCl in 50mL ethanol
4be 1:30 with NaOH mole); Take 0.010g spindle shaped alpha-Fe
2o
3forerunner is nanocrystalline, and ultrasonic disperse is in prefabricated Sn (OH)
6 2-in solution, α-Fe
2o
3with Sn (OH)
6 2-mol ratio is 1:50; The suspension liquid of gained is transferred in the stainless steel reaction of 25mL, in retort furnace, carries out solvent thermal reaction 2 hours in 180 DEG C; Product is collected by high speed centrifugation; Product is used respectively deionized water and washing with alcohol 3 times, in 50 DEG C of dryings 4 hours in vacuum drying oven, obtain SnO
2/ α-Fe
2o
3(hollow ellipsoid) nano heterojunction powder.
X-ray diffraction, transmission electron microscope and sem test show, gained SnO
2/ α-Fe
2o
3nano heterogeneously become SnO
2nanometer stub hetero epitaxy is born in α-Fe
2o
3the surfaces externally and internally (as Fig. 4 b) of nano hollow ellipsoid.
Example 5:SnO
2/ α-Fe
2o
3preparation, the appearance structure of (ring-type) nano heterojunction powder characterize
Ring-type α-Fe selected by this example
2o
3manocrystalline powders pattern is shown in Fig. 5 a, and its remained on surface has phosphoric acid salt and vitriol.Take 0.087g SnCl
45H
2o and 0.267g NaOH is dissolved in (SnCl in 15mL ethanol
4be 1:6 with NaOH mole), obtain Sn (OH)
6 2-solution; Take 0.010g pseudo-cubic shape α-Fe
2o
3forerunner is nanocrystalline, and ultrasonic disperse is in prefabricated Sn (OH)
6 2-in solution, α-Fe
2o
3with Sn (OH)
6 2-mol ratio is 1:1; The suspension liquid of gained is transferred in the stainless steel cauldron of 25mL, in retort furnace, at 220 DEG C, carries out solvent thermal reaction 2 hours; Product is collected by high speed centrifugation; Product is used respectively deionized water and washing with alcohol 3 times, under vacuum drying oven, 50 DEG C of inner dryings 4 hours, namely obtain SnO
2/ α-Fe
2o
3(ring-type) nano heterojunction powder.
X-ray diffraction, transmission electron microscope and sem test show, gained SnO
2/ α-Fe
2o
3nano heterogeneously become SnO
2nanometer stub heteroepitaxial growth is in α-Fe
2o
3the interior outer side (as Fig. 4 b) of nano-rings.
Example 6: change the SnO of reaction times to synthesis
2/ α-Fe
2o
3the impact of nano heterojunction powder
According to the formula of example 1, change the solvent thermal reaction time (extending to 5 hours from 1 hour), found in conjunction with XRD test by electron microscope sem observation, be less than 2 hours when reacted, there is no SnO
2nanocrystalline generation.Therefore method of the present invention is utilized to synthesize SnO
2/ α-Fe
2o
3nano heterojunction, Heteroepitaxy nano SnO
2reaction times should more than 2 hours.
Claims (1)
1. one kind at α-Fe
2o
3nanocrystal surface Heteroepitaxy nano SnO
2method, it is characterized by: be the SnCl of 1:6 ~ 60 by molar ratio
4mix in ethanol with NaOH, form Sn (OH)
6 2-ethanolic soln; By the α-Fe obtained in advance
2o
3nanocrystal is dispersed in Sn (OH)
6 2-in ethanolic soln, α-Fe
2o
3nanocrystalline with Sn (OH)
6 2-mol ratio be 1:1 ~ 50; The mixed solution of gained is carried out solvent thermal reaction, and temperature is 180 ~ 240 DEG C, and the reaction times is more than 2 hours.
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