CN103613123B - Method for preparing monodisperse stannic oxide nanocrystalline particles - Google Patents
Method for preparing monodisperse stannic oxide nanocrystalline particles Download PDFInfo
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- CN103613123B CN103613123B CN201310680788.0A CN201310680788A CN103613123B CN 103613123 B CN103613123 B CN 103613123B CN 201310680788 A CN201310680788 A CN 201310680788A CN 103613123 B CN103613123 B CN 103613123B
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- stannic oxide
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Abstract
The invention belongs to the technical field of preparation of nano materials and relates to a method for preparing monodisperse stannic oxide nanocrystalline particles. The method comprises the following steps: uniformly mixing deionized water with ethanol or isopropanol to serve as a solvent, and then respectively dissolving SnCl4.5H2O and benzimidazole in the solvent to obtain a mixed solution; transferring the mixed solution into a stainless steel reaction kettle lined with polytetrafluoroethylene to react to obtain a white sample; and then, sequentially cleaning the white sample with deionized water and ethanol, and drying to obtain the monodisperse stannic oxide nanocrystalline particles; the preparation method is simple in preparation process, simple and convenient to operate, reliable in principle, low in production cost, high in product yield and is environmental-friendly, and the prepared nanocrystalline particles are small in size, good in monodispersity, large in specific surface area and high in purity, has a wide application prospect on the aspects of gas sensors and can be put into large-scale industrial production easily.
Description
Technical field:
The invention belongs to technical field of nanometer material preparation, relate to a kind of technique utilizing benzoglyoxaline to do mineralizer controlled synthesis bigger serface, monodisperse stannic oxide nanocrystalline particle, a particularly preparation method for monodisperse stannic oxide nanocrystalline particle, can be used for the fields such as catalyzer, gas sensor and electrode materials.
Background technology:
Tindioxide is a kind of wide bandgap semiconductor oxide compound (energy gap is 3.6eV), Lacking oxygen is there is in its actual building-up process, present n-type semiconductor characteristic, tindioxide has unique gas sensing property, electroconductibility and light transmission, have broad application prospects in the field such as photoelectricity and gas sensor, its potential using value causes the extensive concern of people, the brilliant particle of tindioxide of dispersed nano size has larger specific surface area, there is many defects in higher activity and surface, its photoelectric property and air-sensitive performance show the excellent properties being different from block materials, and its sensitivity, selectivity can be improved by other element of doping, therefore, many researchists are devoted to the preparation method studying monodisperse stannic oxide nanocrystalline particle.At present, SnO
2the preparation method of nano particle comprises physics synthesis method and chemical synthesis, and wherein, physics synthesis method comprises sputtering method, vapour deposition process and plasma method, and these methods require high to plant and instrument, and productive expense is expensive, and it is high to consume energy; Compared with traditional physics synthesis method, the low in raw material price of chemical synthesis process, plant and instrument is simple, and building-up process is easy to control, and existing chemical synthesis has developed hydrothermal method (H.C.Chiu; C.S.Yeh.J.Phys.Chem.C.2007,111,7256; H.L.Zhu; D.Yang; G.X.Yu; H.Zhang; K.H.Yao.Nanotechnology, 2006,17,2386), sol-gel method (F.Gu.; S.F.Wang.; M.K.Lu; G.J.Zhou.; D.Xu.; D.R.Yuan.J.Phys.Chem.B, 2004,108,8119), ultrasonic synthesis (J.J.Zhu; Z.H.Lu; S.T.Aruna; D.Aurbach; A.Gedanken.Chem.Mater., 2000,12,2557) and the method such as conbustion synthesis (CN1887722), the wherein SnO for preparing of hydrothermal method
2nano particle has the advantages such as grain development is complete, narrow particle size distribution, reunion mild degree, significantly improves the performance of material, is considered to a kind of important means preparing tin oxide nano particles.But traditional hydrothermal synthesis method needs to prepare monodispersed tin oxide nano particles by means of tensio-active agent; owing to introducing tensio-active agent; the purity of prepared stannic oxide particle is not high, just must can obtain high purity, single dispersing tin oxide nano particles (Y.D.Wang. by follow-up further process (such as high-temperature calcination); C.L.Ma.; X.D.Sun.; H.D.Li.Nanotechnology, 2002,13,565), energy consumption is high, complicated process of preparation.Therefore, develop a kind of single stage method and prepare that diameter is little, the method tool of single dispersing, highly purified tin dioxide nanocrystal particle is of great significance.
Summary of the invention:
The object of the invention is the shortcoming overcoming prior art existence, provides a kind of benzoglyoxaline that utilizes for the method for the tin dioxide nanocrystal particle of mineralizer controlled synthesis single dispersing, high purity, bigger serface.
In order to realize foregoing invention object, the present invention is with SnCl
45H
2o is raw material, and benzoglyoxaline makees mineralizer, and the mixed solution of water and ethanol or propyl alcohol is solvent, preparation monodisperse stannic oxide nanocrystalline particle, and its concrete technology step comprises:
(1), using deionized water and ethanol or propyl alcohol by volume for the ratio of 1:1 mixes as solvent, then by SnCl
45H
2o and benzoglyoxaline are dissolved in solvent and obtain mixing solutions, wherein, and SnCl
45H
2the weight ratio of O and solvent is 1:100, SnCl
45H
2the weight ratio of O and benzoglyoxaline is 7:2-12;
(2), the mixing solutions that step (1) obtains is transferred in teflon-lined stainless steel cauldron, at 160-200 DEG C, react 12-24 hour, obtain white pigmented samples;
(3) white pigmented samples, by step (2) obtained is dried at 60-150 DEG C with after deionized water and ethanol purge successively, obtains monodisperse stannic oxide nanocrystalline particle.
Compared with prior art, its preparation technology is simple, easy and simple to handle in the present invention, principle is reliable, production cost is low, and product yield is high, environmental friendliness, the nano-crystalline granule size of preparation is little, monodispersity is good, and specific surface area is large, and purity is high, have broad application prospects in gas sensor, be easy to carry out large-scale commercial production.
Accompanying drawing illustrates:
Fig. 1. be SnO prepared by the embodiment of the present invention 1
2the XRD figure spectrum of nano particle, shows that material is the monocrystalline SnO of tetragonal crystal structure
2particle.
Fig. 2 is SnO prepared by the embodiment of the present invention 2
2the XRD figure spectrum of nano particle, shows that material is the monocrystalline SnO of tetragonal crystal structure
2particle.
Fig. 3 is SnO prepared by the embodiment of the present invention 3
2the XRD figure spectrum of nano particle, shows that material is the monocrystalline SnO of tetragonal crystal structure
2particle.
Fig. 4 is SnO prepared by the embodiment of the present invention 1
2the transmission electron microscope photo of nano-crystalline granule, wherein (a) is SnO
2the low power transmission electron microscope photo of nano-crystalline granule, (b) is SnO
2the high power transmission electron microscope photo of nano-crystalline granule; Show that this material is the brilliant particle of monodispersed ball shaped nano, particle size is relatively more even, and mean diameter is 3.4nm greatly.
Fig. 5 is SnO prepared by the embodiment of the present invention 2
2the transmission electron microscope photo of nano-crystalline granule, wherein (a) is SnO
2the low power transmission electron microscope photo of nano-crystalline granule, (b) is SnO
2the high power transmission electron microscope photo of nano-crystalline granule; Show that this material is monodispersed elliposoidal nano-crystalline granule, particle size is relatively more even, its major diameter average out to 7.4nm, minor axis average out to 4.8nm.
Fig. 6 is SnO prepared by the embodiment of the present invention 3
2the transmission electron microscope photo of nano-crystalline granule, wherein (a) is SnO
2the low power transmission electron microscope photo of nano-crystalline granule, (b) is SnO
2the high power transmission electron microscope photo of nano-crystalline granule; Show that this material is the brilliant particle of ball shaped nano, and occur clustering phenomena, mean diameter is about 5.2nm.
Fig. 7 is SnO prepared by the embodiment of the present invention 1
2the size distribution plot of nano-crystalline granule, shows the SnO prepared
2the size of particle is relatively more even, is distributed in 2.3-4.5nm.
Fig. 8 is SnO prepared by the embodiment of the present invention 2
2the size distribution plot of nano-crystalline granule, shows the SnO prepared
2the size of particle is relatively more even, and major diameter is distributed in 6.8-8.0nm, and minor axis is distributed in 4.5-6.0nm.
Fig. 9 is SnO prepared by the embodiment of the present invention 3
2the size distribution plot of nano-crystalline granule, shows the SnO prepared
2the distribution of sizes of particle is at 3.5-6.0nm.
Figure 10 is SnO prepared by the embodiment of the present invention 1
2the N of nano-crystalline granule
2adsorption-desorption isothermal and graph of pore diameter distribution, show that this material has typical meso-hole structure.
Figure 11 is SnO prepared by the embodiment of the present invention 2
2the N of nano-crystalline granule
2adsorption-desorption isothermal and graph of pore diameter distribution, show that this material has typical meso-hole structure.
Figure 12 is SnO prepared by the embodiment of the present invention 3
2the N of nano-crystalline granule
2adsorption-desorption isothermal and graph of pore diameter distribution, show that this material has typical meso-hole structure.
Embodiment:
Also be described further by reference to the accompanying drawings below by embodiment.
The present embodiment is with SnCl
45H
2o is raw material, and benzoglyoxaline makees mineralizer, and the mixed solution of water and ethanol or propyl alcohol is solvent, and prepare single dispersing, bigger serface, highly purified tin dioxide nanocrystal particle, its concrete technology step comprises:
(1), using deionized water and ethanol or propyl alcohol by volume for the ratio of 1:1 mixes as solvent, then by SnCl
45H
2o and benzoglyoxaline are dissolved in solvent and obtain mixing solutions, wherein, and SnCl
45H
2the weight ratio of O and solvent is 1:100, SnCl
45H
2the weight ratio of O and benzoglyoxaline is 7:2-12;
(2), the mixing solutions that step (1) obtains is transferred in teflon-lined stainless steel cauldron, at 160-200 DEG C, react 12-24 hour, obtain white pigmented samples;
(3) white pigmented samples, by step (2) obtained is dried at 60-150 DEG C with after deionized water and ethanol purge successively, obtains monodisperse stannic oxide nanocrystalline particle.
Embodiment 1:
The present embodiment is with SnCl
45H
2o is raw material, and benzoglyoxaline makees mineralizer, and the mixed solution of water and ethanol is solvent, reacts 20 hours under 180 DEG C of conditions, obtained single dispersing, bigger serface, highly purified tin dioxide nanocrystal particle, and its concrete technology step comprises:
(1), 20mL deionized water and 20mL ethanol are mixed as solvent, by 0.35gSnCl
45H
2o and 0.1g benzoglyoxaline is also dissolved in solvent and obtains mixing solutions;
(2), by the mixing solutions of gained transfer in 50mL teflon-lined stainless steel cauldron, at 180 DEG C, react 20h obtain white pigmented samples;
(3), by the white pigmented samples of gained use deionized water and ethanol purge successively, then 100 DEG C of oven dry obtain the single dispersing SnO that mean diameter is about 3.4nm in atmosphere
2the brilliant particle of ball shaped nano, its specific surface area is 223.6m
2g
-1, aperture is 5.6nm.
Embodiment 2:
In the present embodiment, the consumption of benzoglyoxaline is 0.3g, and other experiment condition is identical with embodiment 1, prepares the single dispersing SnO of elliposoidal
2nano-crystalline granule, its major diameter average out to 7.4nm, minor axis is on average about 4.8nm, and specific surface area is 181.2m
2g
-1, aperture is 6.4nm.
Embodiment 3:
In the present embodiment, the consumption of benzoglyoxaline is 0.6g, and other experiment condition is identical with embodiment 1, the SnO prepared
2there is clustering phenomena in nano-crystalline granule, particle is spherical, and its mean diameter is about 5.2nm, and specific surface area is 109.7m
2g
-1, compare specific surface area with embodiment 1 with 2 and obviously decline; Aperture is 4.3nm.
The present embodiment is by regulating the consumption regulation and control SnO of mineralizer benzoglyoxaline
2nanocrystalline particle size and pattern, under the regulating and controlling effect of benzoglyoxaline, the SnO of preparation
2the advantages such as nano particle has size uniformity, and monodispersity is good, and degree of crystallinity is high, and reference area is large, and have potential application in fields such as catalyzer, gas sensor and electrode materialss.
Claims (1)
1. a preparation method for monodisperse stannic oxide nanocrystalline particle, is characterized in that with SnCl
45H
2o is raw material, and benzoglyoxaline makes mineralizer, and the mixed solution of water and ethanol or propyl alcohol is solvent, and the concrete technology step of preparation monodisperse stannic oxide nanocrystalline particle comprises:
(1), using deionized water and ethanol or propyl alcohol by volume for the ratio of 1:1 mixes as solvent, then by SnCl
45H
2o and benzoglyoxaline are dissolved in solvent and obtain mixing solutions, wherein, and SnCl
45H
2the weight ratio of O and solvent is 1:100, SnCl
45H
2the weight ratio of O and benzoglyoxaline is 7:2-12;
(2), the mixing solutions that step (1) obtains is transferred in teflon-lined stainless steel cauldron, at 160-200 DEG C, react 12-24 hour, obtain white pigmented samples;
(3) white pigmented samples, by step (2) obtained is dried at 60-150 DEG C with after deionized water and ethanol purge successively, obtains monodisperse stannic oxide nanocrystalline particle.
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| CN113956493B (en) * | 2020-07-20 | 2022-07-19 | 中国科学院福建物质结构研究所 | Non-alkyl tin oxygen cluster compound and synthetic method and application thereof |
| CN113403050B (en) * | 2021-07-02 | 2022-05-17 | 北京宏勤石油助剂有限公司 | Nano plugging agent and preparation method thereof |
| CN113504271A (en) * | 2021-07-09 | 2021-10-15 | 复微感知(合肥)科技有限公司 | Low-concentration acetone gas sensitive material, and preparation method and application thereof |
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| CN101209856B (en) * | 2007-12-21 | 2011-09-28 | 中国科学院长春应用化学研究所 | Method for synthesizing tin oxide nanocrystalline by mould plate method combined with hydrothermal condition |
| CN101928561A (en) * | 2009-06-26 | 2010-12-29 | 中国科学院福建物质结构研究所 | Erbium ion-doped tin dioxide nanocrystal near-infrared light-emitting material and preparation method and application thereof |
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