CN102294211A - Preparation method for TaOx@Ta2O5 core-shell nanometer particle - Google Patents

Preparation method for TaOx@Ta2O5 core-shell nanometer particle Download PDF

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CN102294211A
CN102294211A CN2011102364723A CN201110236472A CN102294211A CN 102294211 A CN102294211 A CN 102294211A CN 2011102364723 A CN2011102364723 A CN 2011102364723A CN 201110236472 A CN201110236472 A CN 201110236472A CN 102294211 A CN102294211 A CN 102294211A
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tao
taox
ta2o5
preparation
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CN102294211B (en
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梁长浩
李强
张和民
刘俊
田振飞
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Hefei Institutes of Physical Science of CAS
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Hefei Institutes of Physical Science of CAS
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Abstract

The invention discloses a preparation method for TaOx@Ta2O5 core-shell nanometer particles. The method comprises the following steps: immersing a simple tantalum target material in anhydrous ethanol, and ablating the simple tantalum target material for half an hour by using Nd:YAG pulsed laser so as to obtain a colloidal solution of TaOx@Ta2O5; carrying out centrifugation and drying to obtain TaOx@Ta2O5. The method provided in the invention has the following advantages: the short preparation period is short, experimental equipment is simple, the prepared colloidal solution is very stable, etc. The unnormal method enables a stably existing TaOx@Ta2O5 core-shell structure nanometer granular material to be obtained, and the material with the core-shell structure is more favorable for separation between photoinduced electrons and photoinduced holes and enables composition of the two to be reduced, thereby effectively improving photocatalytic activity of the material.

Description

A kind of TaO xTa 2O 5The preparation method of core-shell nano particle
Technical field
The present invention relates to a kind of TaO xTa 2O 5The preparation method of core-shell nano particle.
Background technology
Because Ta 2O 5Have good chemical stability and heat endurance, and characteristics such as fusing point height, have wide practical use in the fields such as degraded, sewage disposal and photolysis water hydrogen of pigment.Yet, because semi-conductor type metal oxide Ta 2O 5In the light-catalyzed reaction process, have bigger energy gap (3.9 eV), photocatalysis response only can be arranged in the ultra-violet (UV) band, to sunshine to absorb efficient lower.Given this, people have adopted a lot of methods to Ta 2O 5Carry out modification to promote its performance.Mainly contain following three kinds: one, regulate shape, pattern have influenced its performance to a great extent, by the regulation and control of pattern, and then improve its performance.Two, mix, mix and reduced its energy gap on the one hand, improved absorption and utilization, can promote separating of light induced electron and photohole effectively on the other hand, reduce their recombination probability, improve photocatalytic activity visible light.Three, modify, modification mainly can make photohole-duplet effectively separate, thereby improves its performance.To Ta 2O 5Mix and modify report mainly contain solid reaction process and cold plasma treatment technology.
Summary of the invention
The object of the present invention is to provide a kind of TaO xTa 2O 5The preparation method of core-shell nano particle.
The present invention adopts following technical scheme to achieve these goals:
TaO xTa 2O 5The preparation method of core-shell nano particle is characterized in that may further comprise the steps:
Tantalum simple substance target is immersed in the absolute ethyl alcohol, adopts the Nd:YAG pulse laser, wavelength is 1064 nm, and energy is 85-95 mJ, and ablation tantalum simple substance target 25-35 minute obtains TaO XTa 2O 5Colloidal solution; Centrifugal, drying obtains TaO xTa 2O 5
Described TaO xTa 2O 5The preparation method of core-shell nano particle is characterized in that: described Nd:YAG pulse laser wavelength is 1064 nm, and energy is 90 mJ.
Described TaO xTa 2O 5The preparation method of core-shell nano particle is characterized in that: the rotation that target does not stop together with bottom support bracket in the process of ablating.
Beneficial effect of the present invention:
The inventive method has advantages such as manufacturing cycle is short, and experimental provision is simple, and the colloidal solid of preparation is highly stable; By XRD material phase analysis, SEM and TEM Electronic Speculum and electron spectrum structure, constituent analysis, proved that synthetic product is the TaO of nucleocapsid structure xTa 2O 5Nano composite material, and have the Ta of photocatalytic activity 2O 5Shell has only 2-3 nm thick, moves to the catalyst granules surface apace thereby more help light induced electron, and TaO xExistence also can reduce light induced electron-hole to compound probability, therefore be expected to obtain with respect to pure Ta 2O 5The photocatalysis efficiency that nano particle is higher.
Description of drawings
Fig. 1 TaO xTa 2O 5Core-shell nano structure building-up process schematic diagram.
The XRD figure of sample behind Fig. 2 laser ablation.
Fig. 3 TaO xTa 2O 5The scanning electron microscopy of nuclear shell structure nano particle (SEM) picture (a), transmission electron microscopy (TEM) picture (b), the high-resolution TEM picture (c) of single nucleocapsid structure and corresponding to the partial enlarged drawing (d) of (c) figure.
Fig. 4 TaO xTa 2O 5The surperficial phenetic analysis of the x-ray photoelectron spectroscopy of nuclear shell structure nano particle (XPS).
The specific embodiment
Embodiment 1:TaO xTa 2O 5The preparation method of core-shell nano particle may further comprise the steps:
Tantalum simple substance target is immersed in the 13-18 mL absolute ethyl alcohol, adopts the Nd:YAG pulse laser, wavelength is 1064 nm, and energy is 90 mJ, and ablation tantalum simple substance target 30 minutes obtains TaO XTa 2O 5Colloidal solution; Centrifugal, drying obtains TaO xTa 2O 5, the rotation that target does not stop together with bottom support bracket in the process of ablating.
Embodiment 2:As shown in Figure 1, Fig. 1 is TaO xTa 2O 5Core-shell nano structure building-up process schematic diagram; Fig. 2 is the X-ray material phase analysis diffraction pattern (XRD) of products therefrom, can see that from scheming to go up us most XRD diffraction maximum comes from TaO, has only a peak to belong to Ta 2The O phase.Fig. 3 a be the SEM figure of product, product is made up of the nano particle of a large amount of even size distribution as can be seen, Fig. 3 b is low power TEM figure, by Fig. 3 b as can be known, product is spherical nano particle, particle size is about 30 nm, can see that particle is a nucleocapsid structure, Fig. 3 c is the high-resolution electron micrograph image (HRTEM) of typical single particle, and clearly, products therefrom is the nano spherical particle of nucleocapsid structure, and inside is that the surface of crystallization then is amorphous amorphous, Fig. 3 d is the partial enlarged drawing of single particle, and by calculating, interplanar distance 0.256 nm and 0.240 nm value be (111) face and the Ta of corresponding TaO respectively 2(220) interplanar distance of O in order further to determine surface-element and electronics valence state thereof, has been carried out the surperficial phenetic analysis of x-ray photoelectron spectroscopy (XPS) to products therefrom, as shown in Figure 4, Fig. 4 a is the full spectrogram of photoelectron spectroscopy, has clearly demonstrated Ta, O, the binding energy of C element.Binding energy 26.01 eV and 28.02 eV belong to Ta4f respectively among Fig. 4 b 7/2And Ta4f 5/2Electron orbit, can determine it is the tantalum ion of pentavalent by looking into the xps energy spectrum handbook, the O1s valence band spectrum clearly is made up of three peaks among Fig. 4 c, handle by swarming, binding energy belongs to the binding energy of Ta-O key at 530.38 eV, two other binding energy can be owing to the binding energy of surface contamination and C-O key, and the atomic ratio of O and Ta is near 2.5:1, thus we to draw the surface be that composition is Ta 2O 5We draw the TaO that product is a nucleocapsid structure comprehensive XRD, TEM and XPS xTa 2O 5Nano composite material.For TaO xTa 2O 5The core-shell nano material formation mechanism, we think, in the liquid laser ablation process, after beam of laser and the interaction of solid tantalum target, will cause the material surface evaporation, produce superhigh temperature, the super-pressure plasma, this plasma that comprises various high density free radicals just can form at laser action 60 ns, its temperature can be up to 6000K, its local pressure can be up to 1GPa, the local plasmon body is with ultrasonic outside adiabatic expansion then, while and surrounding environment take place to interact and violent chemical reaction, thus cooling fast, cohesion, until burying in oblivion of plasma.Under this extreme condition, various physics, chemical reaction will take place in induced with laser various atoms, molecule, ion, group that produce and that liquid medium provided at a terrific speed, thereby cause the growth and the assembling of novel metastable nanostructured.
TaO xTa 2O 5The formation of core-shell nano structure can simply be divided into 4 steps: 1) at first after a branch of pulsed laser irradiation is to the simple substance tantalum target, moment produces the plasma of HTHP high density tantalum on solid/liquid interfaces; 2) plasma of tantalum because of the confinement effect of its HTHP and ethanol medium with adiabatic expansion, simultaneously the temperature of its edge begins to reduce, and causes the generation of tantalum cluster; 3) in the process that plasma is buried in oblivion, after tantalum cluster and ethanol interact, form TaO and Ta with metastable phase 2O; 4) because the oxide TaO of low price tantalum xUnstable meeting continues dissolved oxygen or oxidation of ethanol, thereby has formed stable Ta on the surface 2O 5Shell, chemical reaction related in this process is:
Figure 2011102364723100002DEST_PATH_IMAGE002
Figure 2011102364723100002DEST_PATH_IMAGE004
The localized regions of elevated temperature high pressure extreme environment that produces in the liquid laser ablation process provides unique reaction condition for the interaction of tantalum cluster and ethanol molecule.

Claims (3)

1.TaO xTa 2O 5The preparation method of core-shell nano particle is characterized in that may further comprise the steps:
Tantalum simple substance target is immersed in the absolute ethyl alcohol, adopts the Nd:YAG pulse laser, wavelength is 1064 nm, and energy is 85-95 mJ, and ablation tantalum simple substance target 25-35 minute obtains TaO XTa 2O 5Colloidal solution; Centrifugal, drying obtains TaO xTa 2O 5
2. TaO according to claim 1 xTa 2O 5The preparation method of core-shell nano particle is characterized in that: described Nd:YAG pulse laser wavelength is 1064 nm, and energy is 90 mJ.
3. TaO according to claim 1 xTa 2O 5The preparation method of core-shell nano particle is characterized in that: the rotation that target does not stop together with bottom support bracket in the process of ablating.
CN 201110236472 2011-08-17 2011-08-17 Preparation method for TaOx@Ta2O5 core-shell nanometer particle Expired - Fee Related CN102294211B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101429644A (en) * 2008-03-21 2009-05-13 中国科学院上海硅酸盐研究所 Production method of metal or metal oxide nano particle
CN102134095A (en) * 2011-04-21 2011-07-27 浙江理工大学 Method for preparing titanium dioxide nanoparticles with core-shell structure

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101429644A (en) * 2008-03-21 2009-05-13 中国科学院上海硅酸盐研究所 Production method of metal or metal oxide nano particle
CN102134095A (en) * 2011-04-21 2011-07-27 浙江理工大学 Method for preparing titanium dioxide nanoparticles with core-shell structure

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
PEISHENG LIU, WEIPING CAI,* AND HAIBO ZENG: "Fabrication and Size-Dependent Optical Properties of FeO Nanoparticles Induced by Laser Ablation in a Liquid Medium", 《J. PHYS. CHEM. C》, vol. 112, no. 9, 2 December 2008 (2008-12-02), pages 3261 - 3266 *

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