CN101941733B

CN101941733B - Method for preparing In2O3 microspheres assembled from lotus root slice structure

Info

Publication number: CN101941733B
Application number: CN2010102908889A
Authority: CN
Inventors: 程知萱; 任晓会; 徐甲强; 张剑平; 张源
Original assignee: University of Shanghai for Science and Technology
Current assignee: University of Shanghai for Science and Technology
Priority date: 2010-09-21
Filing date: 2010-09-21
Publication date: 2012-08-08
Anticipated expiration: 2030-09-21
Also published as: CN101941733A

Abstract

The invention relates to a method for preparing In2O3 microspheres assembled from a lotus root slice structure, which belongs to the technical field of preparation process for chemical materials. The method is characterized by comprising the following steps of: performing treatment on sodium citrate serving as a structure directing agent and soluble indium salt serving as an indium source by a solvothermal and annealing route under a room temperature condition at a certain temperature so as to obtain a white gelatinous precipitate, namely, a precursor InOOH for the In2O3 microspheres assembled from the lotus root slice structure; and drying the obtained precursor in a vacuum drying oven at the temperature of 70 DEG C for 2 hours, putting the dried precursor into a muffle furnace for thermal treatment at the temperature of 600 DEG C for 3 hours and naturally cooling the treated precursor so as to obtain the In2O3 microspheres assembled from the lotus root slice structure. The method for preparing the In2O3 microspheres assembled from the lotus root slice structure by the solvothermal and annealing route has the advantages of simple and practical process, easy operation, high purity of prepared material and complete crystal form of a product. Due to a large number of pore structures on the surface of a material and a large number of pores produced by material accumulation, and compared with the ordinary material, the obtained material has a larger pore volume and molecules can enter a larger inner surface and a larger cavity. Therefore, the method has good application prospect in the field of gas sensors.

Description

A kind of In of lotus root chip architecture assembling 2O 3The preparation method of microballoon

Technical field

The present invention relates to a kind of In of lotus root chip architecture assembling ₂O ₃The preparation method of microballoon belongs to chemical material preparation process technical field.

Background technology

In ₂O ₃N molded breadth forbidden band transparent semiconductor material as a kind of uniqueness; Its direct band gap width is 3.6e V; Indirect band gap is 2.6ev; Have the energy gap of broad, less resistivity and advantages of high catalytic activity, have in fields such as photochemical catalysis, solar cell, gas sensors comparatively widely and use.At present, mainly concentrate on the regulation and control of the nano material of its different dimensions and pattern syntheticly for the research of Indium sesquioxide nano material, and break through, comprise nano-device, solar cell or the like in the hope of obtaining its application in fields such as photoelectricity.Along with research go deep into, people can adopt multiple physics and chemical process to prepare the Indium sesquioxide nano material of different dimensions and pattern, comprise nanocrystalline, nanometer rod, nano wire, nano belt, hollow ball etc.

Trisodium Citrate is a kind of common coordination agent and morphology control agent, and the formation of product pattern is had significant effects.At first, as a kind of strong ligand, it can with In ³⁺Ion forms the title complex of Hydrocerol A and indium, thereby has alleviated In ³⁺The ionic hydrolysis rate; Secondly, thereby citrate can also be adsorbed on the growth that suppresses it on some crystal face, and this characteristic has been applied to the ZnO three-dimensional structure, above Ag nanometer rod and CuO nanometer rod synthetic.For with solvent thermal and annealing path, prepare a kind of In of lotus root chip architecture assembling as structure directing agent with Trisodium Citrate ₂O ₃The preparation method of microballoon does not see that also report is arranged in the document at home and abroad.

Summary of the invention

The In that the purpose of this invention is to provide a kind of lotus root chip architecture assembling ₂O ₃The preparation method of microballoon.

The In of a kind of lotus root chip architecture assembling of the present invention ₂O ₃The preparation method of microballoon is characterized in that with the Trisodium Citrate being structure directing agent, is the indium source with the indium salt (indium nitrate, indium chloride, indium sulfate) of solubility, adopts solvent thermal and annealing path, and thermal treatment at a certain temperature prepares a kind of In of isometric system ₂O ₃Material; Its step of preparation process is following:

A. solubility indium salt (indium nitrate, indium chloride, indium sulfate) is dissolved in (V in the mixing solutions of a certain proportion of ethanol and water _Ethanol: V _Water=1: 1～5: 1), stir to clarify, being made into concentration range is 0.045～0.135molL ^-1

B. gets a certain amount of above-mentioned solution, add Trisodium Citrate, and the mol ratio of indium salt and Trisodium Citrate is 2: 1～5: 1 that abundant stir about is 30～50 minutes under the room temperature, obtains the gluey troubled liquor of a kind of white;

C. with the sealing of above-mentioned troubled liquor,, obtain gel precipitate 120～220 ℃ of thermal treatments 2～48 hours, this throw out is used deionized water, absolute ethanol washing respectively after, place 70 ℃ of vacuum-dryings;

D. dried above-mentioned materials is placed 300～600 ℃ of thermal treatments of retort furnace 3 hours, get final product the In of lotus root chip architecture assembling ₂O ₃Microballoon.

Above-mentioned indium salt is: indium nitrate, indium chloride, indium sulfate

Description of drawings

Fig. 1 is X-ray powder diffraction (XRD) spectrogram of the precursor InOOH of the product of the inventive method preparation

Fig. 2 is X-ray powder diffraction (XRD) spectrogram of the product of the inventive method preparation

Fig. 3 is sem (SEM) spectrogram of the product of the inventive method preparation

Fig. 4 is sem (SEM) spectrogram of the product of the inventive method preparation

Embodiment

After embodiments of the invention specifically being described at present.

Embodiment 1: raw material is indium nitrate, Trisodium Citrate.

E. 2.0mmol is the commercially available indium nitrate that contains crystal water is dissolved in V _Ethanol: V _Water=4: 1 mixed solution is stirred to indium nitrate and dissolves fully;

F. in above-mentioned solution, add the 0.4mmol Trisodium Citrate, stir 30min, be transferred to the 50mL reaction kettle; 180 ℃ of thermal treatment 4 hours; Be cooled to room temperature, the white product that obtains is centrifugal, and be washed till filtrating with deionized water, absolute ethyl alcohol respectively and be neutral; Then product is placed 70 ℃ of vacuum-dryings, getting the white gels throw out is the In of lotus root chip architecture assembling ₂O ₃The precursor InOOH of microballoon;

G. above-mentioned precursor is placed 600 ℃ of thermal treatments of retort furnace 3 hours, get final product the In of lotus root chip architecture assembling ₂O ₃Microballoon.

Embodiment 2: raw material is indium nitrate, Trisodium Citrate.

H. 2.0mmol is the commercially available indium nitrate that contains crystal water is dissolved in V _Ethanol: V _Water=4: 1 mixed solution is stirred to indium nitrate and dissolves fully;

I. in above-mentioned solution, add the 0.4mmol Trisodium Citrate, stir 30min, be transferred to the 50mL reaction kettle, 220 ℃ of thermal treatment 2 hours is cooled to room temperature;

J. with the white product that obtains centrifugal after, be neutral with deionized water, absolute ethanol washing to solution respectively, place 70 ℃ of vacuum-dryings after, product be the In of lotus root chip architecture assembling ₂O ₃The precursor InOOH of microballoon;

K. this precursor is placed 600 ℃ of thermal treatments of retort furnace 3 hours, promptly obtain the In of lotus root chip architecture assembling ₂O ₃Microballoon.

With characterization methods such as X-ray powder diffraction (XRD), sem (SEM), nitrogen adsorption-desorption isotherms crystalline phase, pattern and the pore structure etc. of product are analyzed.Analytical results shows the In of the lotus root chip architecture assembling of adopting the inventive method can successfully prepare body-centered cubic phase [spacer is Ia3 (206)] ₂O ₃Microballoon (its XRD figure spectrum and JCPDS card: 65-3170 is consistent), the precursor of this material are rhombic InOOH (its XRD figure spectrum and JCPDS card: 17-0549 is consistent).

Claims

1. the In of lotus root chip architecture assembling ₂O ₃The preparation method of microballoon is characterized in that having following steps:

A. the volume ratio that indium nitrate is dissolved in ethanol and water is in 1: 1～5: 1 the mixed solution, to stir to clarify, and being made into concentration is 0.045～0.135molL ^-1The indium salts solution;

B. get a certain amount of above-mentioned indium salts solution, add Trisodium Citrate, the mol ratio of indium salt and Trisodium Citrate is 2: 1～5: 1, fully stirs 30～50 minutes under the room temperature, obtains white gluey troubled liquor;

C. with the gluey turbid solution sealing of above-mentioned white,, obtain gel precipitate in 120～220 ℃ of following thermal treatments 2～48 hours;

D. after the gained gel precipitate being used deionized water, absolute ethanol washing respectively, place 70 ℃ of vacuum-dryings;

E. dried above-mentioned materials is placed 300～600 ℃ of thermal treatments of retort furnace 3 hours, get final product the In of lotus root chip architecture assembling ₂O ₃Microballoon.