CN104108746B - A kind of cube indium hydroxide thin film and preparation method thereof - Google Patents
A kind of cube indium hydroxide thin film and preparation method thereof Download PDFInfo
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- CN104108746B CN104108746B CN201410250924.7A CN201410250924A CN104108746B CN 104108746 B CN104108746 B CN 104108746B CN 201410250924 A CN201410250924 A CN 201410250924A CN 104108746 B CN104108746 B CN 104108746B
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Abstract
A kind of cube indium hydroxide thin film, it is made up of indium nitride matrix and cube hydroxide indium layer being grown on indium nitride surface, and this cube of hydroxide indium layer is that cubical nanometer indium hydroxide crystal forms by pattern.The mean sizes of this nanometer indium hydroxide crystal is 150nm.The preparation method of above-mentioned cube of indium hydroxide thin film: in air, after 15-30 minute, is cooled to room temperature in 200 DEG C-300 DEG C heating by indium nitride film; The ammonium acetate and the hexamethylenetetramine that by mol ratio are 1:1 are water-soluble, obtained mixing solutions; The indium nitride base sheet of step 1. gained is immersed in the mixing solutions of step 2. gained, in≤90 DEG C of thermotonus at least 3-5 hour; Reaction terminates to take out step 3. gained base sheet washing with water, in 70-80 DEG C of oven dry.Preparation method of the present invention is simple, temperature of reaction is low and the product prepared is the crystal cubic indium hydroxide thin film of superior performance.
Description
Technical field
The present invention relates to a kind of indium hydroxide thin film and preparation method thereof.
Background technology
Indium hydroxide is widely used in being used as inhibiter in alkaline cell, is also the raw material preparing indium tin oxide simultaneously, has very important application in photoelectric display field.As a kind of good semiconductor material, its nanostructure is the basic module building nanoscale devices, realizes the control synthesis of indium hydroxide nano material morphology and size etc. significant.Existing many research at present comes developing zinc oxide indium hydroxide nano and micro materials by changing various reaction conditions, is mostly to adopt high―temperature nuclei or comparatively complicated chemical reaction.The material simultaneously prepared exists mainly with powder, for synthesis indium hydroxide nano film then rare report.
Summary of the invention
A kind of preparation method is simple, temperature of reaction is low and the product prepared is cube indium hydroxide thin film of crystal and preparation method thereof to being to provide for object of the present invention.The present invention is mainly matrix with indium nitride, adopts amine acetate and hexamethylenetetramine to be raw material, adopts two-step growth method to prepare the film be made up of nanometer indium hydroxide cubes.
Cube hydroxide indium layer that of the present invention cube of indium hydroxide thin film is longer than indium nitride surface by indium nitride film forms, this cube of hydroxide indium layer is that cubical nanometer indium hydroxide crystal forms by pattern, and the mean sizes of this nanometer indium hydroxide crystal is 100-250nm.
The preparation method of above-mentioned cube of indium hydroxide thin film is as follows:
1., in air, indium nitride film after 15-30 minute, is cooled to room temperature in 200 DEG C-300 DEG C heating, obtains the indium nitride base sheet of surface portion oxidation;
2. the amine acetate and the hexamethylenetetramine that by mol ratio are 1:1 are water-soluble, and rapid stirring is even, and obtained mixing solutions, the concentration of amine acetate and hexamethylenetetramine is 50mM.
3. the indium nitride base sheet of step 1. gained is immersed in the mixing solutions of step 2. gained, in≤90 DEG C of thermotonus at least 3-5 hour.
4. reaction terminates to take out step 3. gained indium nitride base sheet washing with water, preferably uses deionized water, in 70-80 DEG C of oven dry.
The present invention compared with prior art tool has the following advantages:
1, the film that the product obtained is made up of nanometer indium hydroxide cubes, it is more superior than powdery indium hydroxide nano material property.
2, preparation method of the present invention does not need catalyzer, and temperature of reaction is low, and mild condition is simple to operate, low cost of manufacture.
3, the present invention adopts amine acetate and hexamethylenetetramine low-temperature aqueous solution method to show growth indium hydroxide nano cubes film at indium nitride, and have controllability, its size can be controlled by the concentration of reaction system.
Accompanying drawing explanation
The X-ray diffractogram of cube indium hydroxide thin film of Fig. 1 obtained by the embodiment of the present invention 1;
The SEM figure of cube indium hydroxide thin film of Fig. 2 obtained by the embodiment of the present invention 1;
The AFM orthographic plan of cube indium hydroxide thin film of Fig. 3 obtained by the embodiment of the present invention 1;
The AFM 3 dimensional drawing of cube indium hydroxide thin film of Fig. 4 obtained by the embodiment of the present invention 1;
The photoluminescence spectrogram of cube indium hydroxide thin film of Fig. 5 obtained by the embodiment of the present invention 1;
The SEM figure of cube indium hydroxide thin film of Fig. 6 obtained by the embodiment of the present invention 2;
The SEM figure of cube indium hydroxide thin film of Fig. 7 obtained by the embodiment of the present invention 3;
The SEM figure of cube indium hydroxide thin film of Fig. 8 obtained by the embodiment of the present invention 4.
As can be seen from Figure 1, except the diffraction peak of substrate layer InN film, all the other two stronger diffraction peaks corresponding indium hydroxide (200) and (400) crystal face respectively.
As can be seen from Figure 2, prepared indium hydroxide thin film is made up of nanocubes, and its median size is at about 200nm.
As can be seen from Fig. 3 and Fig. 4, the thin film boundary of nanocubes composition is regular, and its median size is at about 200nm.
As can be seen from Figure 5, cube indium hydroxide thin film obtained by the embodiment of the present invention 1 has blue-light-emitting characteristic.
As can be seen from Figure 6, prepared indium hydroxide thin film is made up of nanocubes, and its median size is at about 100nm.
As can be seen from Figure 7, prepared indium hydroxide thin film is made up of nanocubes, and its median size is at about 150nm.
As can be seen from Figure 8, prepared indium hydroxide thin film is made up of nanocubes, and its median size is at about 250nm.
Embodiment
Following non-limiting example can make the present invention of those of ordinary skill in the art's comprehend, but does not limit the present invention in any way.
Test method described in following embodiment, if no special instructions, is ordinary method; Described reagent and material, if no special instructions, all can obtain from commercial channels.
Embodiment 1
In atmosphere to the heating of 1cm × 1cm indium nitride film, under 200 DEG C of conditions, heat 15 minutes, naturally cooling to room temperature, to obtain indium nitride base sheet for subsequent use.Then accurately take 0.7009g hexamethylenetetramine and 0.9308g ammonium acetate respectively with electronic balance, put into beaker.Then add 100ml deionized water, rapid stirring is even.Above-mentioned indium nitride base sheet is put into beaker, wraps beaker mouth with masking foil, then put into water-bath, start heating.Arranging final Heating temperature is 90 DEG C, thermostatically heating 3 hours.After question response terminates, taking out beaker and take out indium nitride base sheet, repeatedly rinsing to remove unnecessary ammonium salt and ion with deionized water, drying in order to characterizing in 70 DEG C.The sample of above-mentioned gained is carried out to the test of photoluminescence spectrum, as shown in Figure 4, the thin-film material showing synthesis in figure has stronger glow peak in the blue region of 417nm and 434nm to result.
Embodiment 2
In atmosphere to the heating of 1cm × 1cm indium nitride film, under 250 DEG C of conditions, heat 20 minutes, naturally cooling to room temperature, to obtain indium nitride base sheet for subsequent use.Then accurately take 0.0701g hexamethylenetetramine and 0.093g ammonium acetate respectively with electronic balance, put into beaker.Then add 100ml deionized water, rapid stirring is even.Above-mentioned indium nitride base sheet is put into beaker, wraps beaker mouth with masking foil, then put into water-bath, start heating.Arranging final Heating temperature is 90 DEG C, thermostatically heating 3.5 hours.After question response terminates, taking out beaker and take out indium nitride base sheet, repeatedly rinsing to remove unnecessary ammonium salt and ion with deionized water, drying in order to characterizing in 80 DEG C.
Embodiment 3
In atmosphere to the heating of 1cm × 1cm indium nitride film, under 300 DEG C of conditions, heat 15 minutes, naturally cooling to room temperature, to obtain indium nitride base sheet for subsequent use.Then accurately take 0.028g hexamethylenetetramine and 0.037g ammonium acetate respectively with electronic balance, put into beaker.Then add 100ml deionized water, rapid stirring is even.Above-mentioned indium nitride base sheet is put into beaker, wraps beaker mouth with masking foil, then put into water-bath, start heating.Arranging final Heating temperature is 88 DEG C, thermostatically heating 4 hours.After question response terminates, taking out beaker and take out indium nitride base sheet, repeatedly rinsing to remove unnecessary ammonium salt and ion with deionized water, drying in order to characterizing in 75 DEG C.
Embodiment 4
In atmosphere to the heating of 1cm × 1cm indium nitride film, under 200 DEG C of conditions, heat 30 minutes, naturally cooling to room temperature, to obtain indium nitride base sheet for subsequent use.Then accurately take 1.4018g hexamethylenetetramine and 1.8616g respectively with electronic balance, put into beaker.Then add 100ml deionized water, rapid stirring is even.Above-mentioned indium nitride base sheet is put into beaker, wraps beaker mouth with masking foil, then put into water-bath, start heating.Arranging final Heating temperature is 85 DEG C, thermostatically heating 5 hours.After question response terminates, taking out beaker and take out indium nitride base sheet, repeatedly rinsing to remove unnecessary ammonium salt and ion with deionized water, drying in order to characterizing in 80 DEG C.
Claims (5)
1. one kind of cube of indium hydroxide thin film, it is characterized in that: cube hydroxide indium layer that described cube indium hydroxide thin film is longer than indium nitride surface by indium nitride film forms, this cube of hydroxide indium layer is that cubical nanometer indium hydroxide crystal forms by pattern.
2. according to claim 1 cube of indium hydroxide thin film, is characterized in that: the mean sizes of this nanometer indium hydroxide crystal is 150nm.
3. the preparation method of cube indium hydroxide thin film of claim 1, is characterized in that:
1., in air, indium nitride film after 15-30 minute, is cooled to room temperature in 200 DEG C-300 DEG C heating,
2. the ammonium acetate and the hexamethylenetetramine that by mol ratio are 1:1 are water-soluble, obtained mixing solutions,
3. the indium nitride base sheet of step 1. gained is immersed in the mixing solutions of step 2. gained, in≤90 DEG C of thermotonus 3-5 hour,
4. reaction terminates to take out step 3. gained indium nitride base sheet washing with water, in 70-80 DEG C of oven dry.
4. the preparation method of according to claim 3 cube of indium hydroxide thin film, is characterized in that: ammonium acetate and hexamethylenetetramine water-soluble, their concentration is 50mM.
5. the preparation method of according to claim 3 cube of indium hydroxide thin film, is characterized in that: ammonium acetate and hexamethylenetetramine water-soluble, rapid stirring is even.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1410348A (en) * | 2002-10-25 | 2003-04-16 | 中国科学院上海硅酸盐研究所 | Preparation method of nano indium nitride powder |
| CN101690889A (en) * | 2009-09-21 | 2010-04-07 | 东北林业大学 | Method of preparing catalytic material for indium hydroxide thin film with controllable shape and thickness |
| CN102244159A (en) * | 2011-06-28 | 2011-11-16 | 中国科学院半导体研究所 | Method for roughening surface of ITO (indium tin oxide) transparent conductive film |
| CN102719886A (en) * | 2012-06-20 | 2012-10-10 | 大连民族学院 | Method for growing large-area zinc oxide micron wall |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1410348A (en) * | 2002-10-25 | 2003-04-16 | 中国科学院上海硅酸盐研究所 | Preparation method of nano indium nitride powder |
| CN101690889A (en) * | 2009-09-21 | 2010-04-07 | 东北林业大学 | Method of preparing catalytic material for indium hydroxide thin film with controllable shape and thickness |
| CN102244159A (en) * | 2011-06-28 | 2011-11-16 | 中国科学院半导体研究所 | Method for roughening surface of ITO (indium tin oxide) transparent conductive film |
| CN102719886A (en) * | 2012-06-20 | 2012-10-10 | 大连民族学院 | Method for growing large-area zinc oxide micron wall |
Non-Patent Citations (2)
| Title |
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| "Growth of wurtzite InN on bulk In2O3(111) wafers";Sergey Sadofev et al.;《APPLIED PHYSICS LETTERS》;20121022;第101卷;第172102-1~ 172102-4页 * |
| "沿[100]晶向择优生长的花状In(OH)3晶体的合成与表征";康灵等;《长沙理工大学学报(自然科学版)》;20100630;第7卷(第2期);第81-86、92页 * |
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