CN104071821A

CN104071821A - Method for preparing Sm(OH)3/ZnO composite film by using homogeneous hydrothermal method

Info

Publication number: CN104071821A
Application number: CN201410280901.0A
Authority: CN
Inventors: 殷立雄; 王菲菲; 黄剑锋; 王丹; 郝巍; 李嘉胤
Original assignee: Shaanxi University of Science and Technology
Current assignee: Yancheng Dasheng Building Materials Co.,Ltd.
Priority date: 2014-06-20
Filing date: 2014-06-20
Publication date: 2014-10-01
Anticipated expiration: 2034-06-20
Also published as: CN104071821B

Abstract

The invention discloses a method for preparing a Sm(OH)3/ZnO composite film by using a homogeneous hydrothermal method. The method comprises the following steps of dissolving a certain quantity of analytically pure Sm(NO3)3.6H2O and Zn(NO3)3.6H2O into a proper amount of distilled water according to the molar ratio of (1 to 0.2)-(1 to 2) to obtain a solution A; regulating the pH value of the solution A to 7-13 by using analytically pure sodium hydroxide, and continuing to stir for 1-2h to form a reaction precursor solution; pouring the reaction precursor solution into a homogeneous hydrothermal kettle, placing a cleaned substrate into the homogeneous hydrothermal kettle, placing the homogeneous hydrothermal kettle into a homogeneous reaction instrument after sealing the homogeneous hydrothermal kettle, reacting at the temperature of 80-200 DEG C for 12-48h, and naturally cooling to room temperature after the reaction is ended; opening the hydrothermal kettle, washing the substrate 4-6 times by using distilled water and absolute ethyl alcohol, and drying the substrate in an electrically heated vacuum drying cabinet with the temperature of 40-60 DEG C for 0.5-2h to obtain the Sm(OH)3/ZnO composite film on the surface of the substrate.

Description

A kind of homogeneous phase hydrothermal method that adopts is prepared Sm (OH) 3the method of/ZnO laminated film

Technical field

The present invention relates to a kind of preparation method of Nano semiconductor matrix material, be specifically related to a kind of homogeneous phase hydrothermal method and prepare Sm (OH) ₃the method of/ZnO laminated film.

Background technology

Sm (OH) ₃be a kind of white powder, water insoluble, be soluble in mineral acid.Sm (OH) ₃as typical rare earth metal hydroxide material, nano level Sm (OH) ₃with the characteristic of rare earth and nano material, there is potential using value in multiple fields of the functional materialss such as high efficiency light-emitting device, magneticsubstance, catalytic material.ZnO white powder, water insoluble, ethanol and ammoniacal liquor.Nano zine oxide is because particle diameter is little, specific surface area has small-size effect greatly, and surface effects and quantum size effect etc., show the ultraviolet ability of unique piezoelectric property, high conductivity, photocatalysis performance and scattering and absorption.Nano zine oxide has excellent photocatalysis performance as functional materials, and the energy gap of its body phase material is 3.2eV.Under UV-irradiation, nano zine oxide has the effect of photocatalyst.Nano zine oxide has certain photocatalytic activity, cheap, has very wide application prospect in photocatalysis field.And nano composite material is by two or more material of different nature, by the method for physics or chemistry, in macroscopic view, composition has the material of new capability.Various materials make up for each other's deficiencies and learn from each other in performance, produce synergistic effect, make the over-all properties of matrix material be better than former composition material and meet various requirement.Sm (OH) ₃all have good photocatalysis performance with ZnO, both are compound, produce synergy, can obtain more excellent photocatalysis performance.

The surface properties of film as exposed crystal face, crystalline structure and form, grain size and film thickness etc., has been played the part of important role in the control of its electricity, optics and gas sensitive property.In addition, film has cell texture, and surface-area is large, is conducive to the application of catalysis aspect, can make catalytic efficiency greatly improve.Therefore prepare laminated film Sm (OH) ₃/ ZnO has very large using value.The present invention proposes a kind of simple homogeneous phase hydrothermal method and prepare Sm (OH) ₃the method of/ZnO laminated film.

The method of preparing film of reporting is at present mainly vacuum vapour deposition [DAKHEL A A.Dielectric and optical properities of samarium oxide thin films[J] .Alloys compd, 2004,365:233-239], sol-gel method [Ching-Feng Lia.NH ₃sensing properties of ZnO thin films prepared via sol – gel method[J] .Journal of Alloys and Compounds, 2014,5 (606): 27-31], hydrothermal method [Zelalem N.Urgessa.Hydrothermal synthesis of ZnO thin films and its electrical characterization[J] .Materials Letters.2012,15 (79): 266-269].Wherein to prepare film very high to equipment requirements for vacuum vapour deposition, and equipment and instrument is more expensive, little to raw material availability; Sol-gel method craft process temperature is low, but reaction time is long, and aftertreatment is more loaded down with trivial details; Compared with vacuum vapour deposition, sol-gel method, hydrothermal method is prepared film and is once completed in liquid phase, be not subject to the restriction of substrate shape and size, do not need the hot thermal treatment of purification in later stage, avoided cracking that film may cause in heat treatment process, the defect such as curling, and taking inorganics as precursor, water is reaction medium, and raw material is easy to get, and has reduced preparation cost, and add stirring on the basis of common hydro-thermal, make reaction more abundant.

Summary of the invention

The object of the present invention is to provide that a kind of equipment requirements is low, technique is simple, and easy and simple to handle, energy consumption is low, the Sm that photocatalysis performance is good (OH) is prepared in easy control, employing homogeneous phase hydrothermal method that security is good ₃the method of/ZnO laminated film.

For achieving the above object, the technical solution used in the present invention is:

1) by analytically pure Sm (NO ₃) ₃6H ₂o and Zn (NO ₃) ₃6H ₂o is dissolved in and in distilled water, makes solution A with the mol ratio of 1:0.2～1:2;

2) under magnetic agitation, adopt pH to 7～13 of analytically pure sodium hydrate regulator solution A, continue to stir 1～2h and form reaction precursor liquid;

3) reaction precursor liquid is poured in homogeneous phase hydrothermal reaction kettle, clean substrate is placed in one, after envelope still, put into homogeneous reaction instrument, hydro-thermal reaction 12～48h at 80～200 DEG C, naturally cools to room temperature after reaction finishes;

4) substrate is used to distilled water and absolute ethanol washing 4～6 times, be placed in 40～60 DEG C of electric vacunm drying case inner drying 0.5～2h, obtain Sm (OH) at substrate surface ₃/ ZnO laminated film.

The solvent of described homogeneous phase hydro-thermal reaction is distilled water.

Reaction medium of the present invention is the aqueous solution, safe, and reaction raw materials is easy to get, and feasibility is strong, and processing unit is simple.Utilize homogeneous phase to stir and make reaction more full and uniform, make the Sm (OH) with better photocatalytic activity ₃/ ZnO laminated film.Utilize sodium hydroxide to regulate the pH of reaction system, the presoma making, pours in homogeneous phase hydrothermal reaction kettle, and clean substrate is placed in one, and puts into homogeneous reaction instrument and reacts, the Sm (OH) of gained after envelope still ₃/ ZnO laminated film thickness homogeneous.The raw material of this reaction be easy to get and cost low, processing unit is simple, energy consumption is low, and this reaction carries out under normal pressure, with water, as reaction solvent, security is good, feasibility is strong, so very economical, practical, there is good industrial prospect.

Brief description of the drawings

Fig. 1 is the prepared Sm of the present invention (OH) ₃the XRD figure of/ZnO laminated film;

Embodiment

Embodiment 1:

1) by analytically pure Sm (NO ₃) ₃6H ₂o and Zn (NO ₃) ₃6H ₂o is dissolved in and in distilled water, makes solution A with the mol ratio of 1:0.2;

2) under magnetic agitation, adopt the pH to 7 of analytically pure sodium hydrate regulator solution A, continue to stir 1～2h and form reaction precursor liquid;

3) reaction precursor liquid is poured in homogeneous phase hydrothermal reaction kettle, clean substrate is placed in one, after envelope still, put into homogeneous reaction instrument, at 80 DEG C, taking distilled water as aqueous solvent thermal response 12h, after reaction finishes, naturally cool to room temperature;

4) substrate is used to distilled water and absolute ethanol washing 4～6 times, be placed in 40 DEG C of electric vacunm drying case inner drying 0.5h, obtain Sm (OH) at substrate surface ₃/ ZnO laminated film.

Embodiment 2:

1) by analytically pure Sm (NO ₃) ₃6H ₂o and Zn (NO ₃) ₃6H ₂o is dissolved in and in distilled water, makes solution A with the mol ratio of 1:0.5;

2) under magnetic agitation, adopt the pH to 9 of analytically pure sodium hydrate regulator solution A, continue to stir 1～2h and form reaction precursor liquid;

3) reaction precursor liquid is poured in homogeneous phase hydrothermal reaction kettle, clean substrate is placed in one, after envelope still, put into homogeneous reaction instrument, at 100 DEG C, taking distilled water as aqueous solvent thermal response 24h, after reaction finishes, naturally cool to room temperature;

4) substrate is used to distilled water and absolute ethanol washing 4～6 times, be placed in 50 DEG C of electric vacunm drying case inner drying 1h, obtain Sm (OH) at substrate surface ₃/ ZnO laminated film.

Embodiment 3:

1) by analytically pure Sm (NO ₃) ₃6H ₂o and Zn (NO ₃) ₃6H ₂o is dissolved in and in distilled water, makes solution A with the mol ratio of 1:0.8;

2) under magnetic agitation, adopt the pH to 11 of analytically pure sodium hydrate regulator solution A, continue to stir 1～2h and form reaction precursor liquid;

3) reaction precursor liquid is poured in homogeneous phase hydrothermal reaction kettle, clean substrate is placed in one, after envelope still, put into homogeneous reaction instrument, at 120 DEG C, taking distilled water as aqueous solvent thermal response 24h, after reaction finishes, naturally cool to room temperature;

4) substrate is used to distilled water and absolute ethanol washing 4～6 times, be placed in 60 DEG C of electric vacunm drying case inner drying 1h, obtain Sm (OH) at substrate surface ₃/ ZnO laminated film.

Embodiment 4:

1) by analytically pure Sm (NO ₃) ₃6H ₂o and Zn (NO ₃) ₃6H ₂o is dissolved in and in distilled water, makes solution A with the mol ratio of 1:1;

2) under magnetic agitation, adopt the pH to 12 of analytically pure sodium hydrate regulator solution A, continue to stir 1～2h and form reaction precursor liquid;

3) reaction precursor liquid is poured in homogeneous phase hydrothermal reaction kettle, clean substrate is placed in one, after envelope still, put into homogeneous reaction instrument, at 160 DEG C, taking distilled water as aqueous solvent thermal response 48h, after reaction finishes, naturally cool to room temperature;

Embodiment 5:

1) by analytically pure Sm (NO ₃) ₃6H ₂o and Zn (NO ₃) ₃6H ₂o is dissolved in and in distilled water, makes solution A with the mol ratio of 1:2;

2) under magnetic agitation, adopt the pH to 13 of analytically pure sodium hydrate regulator solution A, continue to stir 1～2h and form reaction precursor liquid;

3) reaction precursor liquid is poured in homogeneous phase hydrothermal reaction kettle, clean substrate is placed in one, after envelope still, put into homogeneous reaction instrument, at 200 DEG C, taking distilled water as aqueous solvent thermal response 24h, after reaction finishes, naturally cool to room temperature;

4) substrate is used to distilled water and absolute ethanol washing 4～6 times, be placed in 60 DEG C of electric vacunm drying case inner drying 2h, obtain Sm (OH) at substrate surface ₃/ ZnO laminated film.

Fig. 1 is the prepared Sm of the present invention (OH) ₃the XRD figure of/ZnO laminated film, as we can see from the figure Sm (OH) ₃characteristic diffraction peak with ZnO.

Claims

1. one kind adopts homogeneous phase hydrothermal method to prepare Sm (OH) ₃the method of/ZnO laminated film, is characterized in that comprising the following steps:

2. homogeneous phase hydrothermal method according to claim 1 is prepared Sm (OH) ₃/ ZnO laminated film method: it is characterized in that: the solvent of described homogeneous phase hydro-thermal reaction is distilled water.