CN101311359A - Preparation method of cuboid indium oxide single crystal - Google Patents
Preparation method of cuboid indium oxide single crystal Download PDFInfo
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- CN101311359A CN101311359A CNA2008100359305A CN200810035930A CN101311359A CN 101311359 A CN101311359 A CN 101311359A CN A2008100359305 A CNA2008100359305 A CN A2008100359305A CN 200810035930 A CN200810035930 A CN 200810035930A CN 101311359 A CN101311359 A CN 101311359A
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Abstract
The invention discloses a preparation method of a cuboid indium oxide single crystal, belonging to a hydrothermal method. By using the shape control agent, the problems that the shape of a sample is difficult to control and easy to collapse and the formed crystal is polycrystalline in the hydrothermal method in the prior art are solved, and the preparation of the cuboid indium oxide single crystal with controllable shape by using the hydrothermal method is realized; the indium oxide single crystal prepared by the preparation method has good dispersibility and uniform and controllable appearance; the preparation method is simple, the raw materials are easy to obtain, the cost is low, and the large-scale industrial production can be realized.
Description
Technical Field
The invention relates to a preparation method of indium oxide, in particular to a preparation method of a cuboid indium oxide single crystal.
Background
Stoichiometric indium oxide is a wide bandgap insulator, while doped, unmetered indium oxide is a wide band n-type semiconductor with good conductivity (over 1S m) -1 ) High transparency in the visible regionDegree and light transmittance exceeding 80%. Because of these characteristics, the use of indium oxide has attracted a great deal of attention from scientists. An important use of indium oxide is to form an indium tin oxide thin film (ITO film) which is transparent to visible light, has good conductivity, has low film resistance, and strongly reflects infrared rays, with tin oxide. In addition, indium oxide is also used in thin film sensors and detectors, insulating layers in capacitors, piezoelectric media in surface acoustic wave devices, and insulators between multiple metallization lines in tape heads. In the field of electrochemistry, indium oxide can be used as a mercury-substituted corrosion inhibitor for a zinc cathode in an alkaline zinc-manganese dioxide battery. Currently, research on the application of indium oxide in the field of gas sensors is active. Indium oxide as a gas detection material has the following advantages: (1) The resistance value is low and easy to regulate and control, and the method is suitable for manufacturing low-power-consumption elements; (2) Has high sensitivity to toxic gas, and is suitable for developing sensor for environmental monitoring, such as O detection 3 Nox, CO, trimethylamine (TMA), etc.; (3) The gas sensitivity can be regulated and controlled by doping, and the development of a selective gas sensitive element is facilitated; (4) The film is easy to be thinned, and the miniaturization, integration and multi-functionalization of elements are convenient; and (5) the working temperature is low, which is beneficial to reducing the power consumption of the element. However, the existing indium oxide gas-sensitive element also has some disadvantages: higher cost, lower stability and selectivity, etc.
Because factors such as microstructure, size and morphology of the material have a great influence on the performance and application of the material, the intrinsic properties of the material need to be fully exerted, and the structure, size and morphology of the material need to be controlled to improve the performance of the material. The known methods for preparing indium oxide mainly include a gas phase method, a liquid phase method and a solid phase method, and specifically include a sputtering method, a vapor deposition method, a sol-gel method, a uniform precipitation method, a template method, a microemulsion method, a room temperature solid phase method, a mechanochemical method and the like. Although the gas phase method can synthesize nanometer indium oxide with various shapes and excellent performance, the requirements on the adjustment of various parameters of equipment are high, the yield is low, and the industrial production is difficult to realize; the solid phase method is used for synthesizing the nano particles which are difficult to obtain uniformly; the liquid phase method requires low temperature and is beneficial to large-scale production, while the liquid phase methods in the current literature reports mainly comprise a precipitation method and a hydrothermal/solvothermal method, a calcination step is needed to obtain a final product, and simultaneously, due to calcination, the appearance of a sample is difficult to control and easy to collapse, and formed crystals are polycrystalline, so that how to prepare the morphology-controllable single crystal indium oxide by using the hydrothermal method is not reported so far.
Disclosure of Invention
The invention aims to provide a preparation process for preparing a cuboid indium oxide single crystal with controllable shape by a hydrothermal method, which aims to solve the problems that the shape of a sample is difficult to control and easy to collapse and the formed crystal is polycrystalline in the hydrothermal method in the prior art.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a method for preparing a cuboid indium oxide single crystal, comprising the steps of:
a) Preparing a morphology control agent: sequentially adding ammonia water, n-heptanol, cyclohexylamine and nonanoic acid according to the proportion, and mixing and stirring for 5min at the temperature of-5 ℃, wherein: the volume ratio of ammonia water, n-heptanol, cyclohexylamine and nonanoic acid is 3: 20;
b) Preparing an indium salt solution: adding an indium salt compound into distilled water, and stirring at-5 ℃ to completely dissolve the indium salt compound to form a transparent solution, wherein: the molar concentration of the indium ions is 0.07-0.08 mol/L;
c) Preparing a precursor: dropwise adding the prepared indium salt solution into the prepared morphology control agent at the temperature of-5 ℃, wherein the dropwise adding speed is controlled at 60 drops/min; stirring for 5 minutes after dripping; then transferring the mixture into a reaction kettle, putting the reaction kettle into a melting furnace, heating the reaction kettle to 150-200 ℃, and preserving heat for 2-4 hours, wherein: the volume ratio of the indium salt solution to the shape control agent solution is (1.4-1.8) to 1;
d) Centrifuging, and drying the obtained jelly at 60 deg.C for 2 hr;
e) Calcining the dried substance at 500-800 ℃ for 1-3 hours;
f) And naturally cooling to obtain the target product.
The indium salt compound may be selected from indium nitrate, indium chloride or indium acetate, preferably indium chloride.
The calcination temperature is preferably 700 ℃.
Compared with the prior art, the invention has the following beneficial effects:
1) By using the morphology control agent, the problems that the morphology of a sample is difficult to control and easy to collapse and the formed crystal is polycrystalline in the hydrothermal method in the prior art are solved, and the purpose of preparing the cuboid indium oxide single crystal with controllable morphology by using the hydrothermal method is realized;
2) The indium oxide single crystal prepared by the preparation method has good dispersibility and uniform and controllable appearance;
3) The preparation method is simple, the raw materials are easy to obtain, the cost is low, and the large-scale industrial production can be realized.
Drawings
FIG. 1 is an XRD pattern of a rectangular parallelepiped indium oxide single crystal produced by the production method of the present invention;
fig. 2 to 4 are SEM images of a rectangular parallelepiped indium oxide single crystal produced by the production method of the present invention.
Detailed Description
The invention is further illustrated by the following examples, which are intended only for a better understanding of the invention and do not limit the scope of the invention.
Example 1
The method for preparing a cuboid indium oxide single crystal provided in this embodiment includes the following steps:
a) Preparing a morphology control agent: sequentially adding ammonia water, n-heptanol, cyclohexylamine and nonanoic acid according to the proportion, and mixing and stirring at 0 ℃ for 5min, wherein: the volume ratio of ammonia water, n-heptanol, cyclohexylamine and nonanoic acid is 3: 20;
b) Preparing an indium salt solution: adding indium chloride compound into distilled water, stirring at 0 ℃ to completely dissolve the indium chloride compound to form a transparent solution, wherein: the molar concentration of the indium ions is 0.077mol/L;
c) Preparing a precursor: dropwise adding the prepared indium salt solution into the prepared morphology control agent at 0 ℃, wherein the dropwise adding speed is controlled at 60 drops/min; stirring for 5 minutes after dripping; then transferring the mixture into a reaction kettle, putting the reaction kettle into a smelting furnace, heating the mixture to 180 ℃, and preserving heat for 3 hours, wherein: the volume ratio of the indium salt solution to the morphology control agent solution is 1.6: 1;
d) Centrifuging, and drying the obtained jelly at 60 deg.C for 2 hr;
e) Calcining the dried substance at 700 ℃ for 1 hour;
f) And naturally cooling to obtain the target product.
Example 2
The method for preparing a cuboid indium oxide single crystal provided in this embodiment includes the following steps:
a) Preparing a morphology control agent: sequentially adding ammonia water, n-heptanol, cyclohexylamine and nonanoic acid according to the proportion, mixing and stirring at-5 ℃ for 5min, wherein: the volume ratio of ammonia water, n-heptanol, cyclohexylamine and nonanoic acid is 3: 20;
b) Preparing an indium salt solution: adding an indium nitrate compound into distilled water, and stirring at-5 ℃ to completely dissolve the indium nitrate compound to form a transparent solution, wherein: the molar concentration of the indium ions is 0.077mol/L;
c) Preparing a precursor: dropwise adding the prepared indium salt solution into the prepared morphology control agent at the temperature of minus 5 ℃, wherein the dropwise adding speed is controlled at 60 drops/min; stirring for 5 minutes after dripping; then transferring the mixture into a reaction kettle, putting the reaction kettle into a smelting furnace, heating the mixture to 200 ℃, and preserving heat for 2 hours, wherein: the volume ratio of the indium salt solution to the morphology control agent solution is 1.8: 1;
d) Centrifuging, and drying the obtained jelly at 60 deg.C for 2 hr;
e) Calcining the dried substance at 800 ℃ for 1 hour;
f) And naturally cooling to obtain the target product.
Example 3
The method for preparing a cuboid indium oxide single crystal provided in this embodiment includes the following steps:
a) Preparing a morphology control agent: sequentially adding ammonia water, n-heptanol, cyclohexylamine and nonanoic acid according to the mixture ratio, and mixing and stirring at 5 ℃ for 5min, wherein: the volume ratio of ammonia water, n-heptanol, cyclohexylamine and nonanoic acid is 3: 20;
b) Preparing an indium salt solution: adding an indium acetate compound into distilled water, and stirring at 5 ℃ to completely dissolve the indium acetate compound to form a transparent solution, wherein: the molar concentration of the indium ions is 0.077mol/L;
c) Preparing a precursor: dropwise adding the prepared indium salt solution into the prepared morphology control agent at 5 ℃, wherein the dropwise adding speed is controlled at 60 drops/min; stirring for 5 minutes after dripping; then transferring the mixture into a reaction kettle, putting the reaction kettle into a melting furnace, heating the reaction kettle to 150 ℃, and preserving heat for 4 hours, wherein: the volume ratio of the indium salt solution to the morphology control agent solution is 1.4: 1;
d) Centrifuging, and drying the obtained jelly at 60 deg.C for 2 hr;
e) Calcining the dried product at 500 ℃ for 3 hours;
f) And naturally cooling to obtain the target product.
The XRD analysis and SEM analysis of the samples obtained in examples 1, 2 and 3, respectively, showed that: the sample prepared by the preparation method is an indium oxide single crystal, and the XRD pattern of the sample is completely consistent with the standard pattern of the indium oxide single crystal (shown in figure 1); the prepared indium oxide single crystal is cuboid, and has good dispersibility and uniform appearance (shown in figures 2 to 4).
Claims (4)
1. A method for producing a cuboid indium oxide single crystal, characterized by comprising the steps of:
a) Preparing a morphology control agent: sequentially adding ammonia water, n-heptanol, cyclohexylamine and nonanoic acid according to the proportion, and mixing and stirring for 5min at the temperature of-5 ℃, wherein: the volume ratio of ammonia water, n-heptanol, cyclohexylamine and nonanoic acid is 3: 20;
b) Preparing an indium salt solution: adding an indium salt compound into distilled water, and stirring at-5 ℃ to completely dissolve the indium salt compound to form a transparent solution, wherein: the molar concentration of the indium ions is 0.07-0.08 mol/L;
c) Preparing a precursor: dropwise adding the prepared indium salt solution into the prepared morphology control agent at the temperature of-5 ℃, wherein the dropwise adding speed is controlled at 60 drops/min; stirring for 5 minutes after dripping; then transferring the mixture into a reaction kettle, putting the reaction kettle into a melting furnace, heating the reaction kettle to 150-200 ℃, and preserving heat for 2-4 hours, wherein: the volume ratio of the indium salt solution to the shape control agent solution is (1.4-1.8) to 1;
d) Centrifuging, and drying the obtained jelly at 60 deg.C for 2 hr;
e) Calcining the dried substance at 500-800 ℃ for 1-3 hours;
f) And naturally cooling to obtain the target product.
2. The method for producing a cuboid-shaped indium oxide single crystal according to claim 1, wherein the indium salt compound is selected from indium nitrate, indium chloride, and indium acetate.
3. The method for producing a cuboid-shaped indium oxide single crystal according to claim 2, wherein the indium salt compound is indium chloride.
4. The method for producing a cuboid indium oxide single crystal according to claim 1, characterized in that the calcination temperature is 700 ℃.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102234130A (en) * | 2010-05-07 | 2011-11-09 | 广西民族大学 | Simple preparation method of indium oxide nano-cube |
| CN102963922A (en) * | 2012-10-26 | 2013-03-13 | 河南圣玛斯光电科技有限公司 | Hydrothermal synthesis method for indium oxide with cubic crystal structure |
| CN108394930A (en) * | 2018-05-14 | 2018-08-14 | 太原理工大学 | A kind of fast preparation method of additive Mn indium oxide gas sensitive |
| CN113604879A (en) * | 2021-06-10 | 2021-11-05 | 安徽工业大学 | Single crystal indium micron sheet and synthesis method and application thereof |
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2008
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102234130A (en) * | 2010-05-07 | 2011-11-09 | 广西民族大学 | Simple preparation method of indium oxide nano-cube |
| CN102234130B (en) * | 2010-05-07 | 2013-04-03 | 广西民族大学 | Simple preparation method of indium oxide nano-cube |
| CN102963922A (en) * | 2012-10-26 | 2013-03-13 | 河南圣玛斯光电科技有限公司 | Hydrothermal synthesis method for indium oxide with cubic crystal structure |
| CN108394930A (en) * | 2018-05-14 | 2018-08-14 | 太原理工大学 | A kind of fast preparation method of additive Mn indium oxide gas sensitive |
| CN113604879A (en) * | 2021-06-10 | 2021-11-05 | 安徽工业大学 | Single crystal indium micron sheet and synthesis method and application thereof |
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| CN100577895C (en) | 2010-01-06 |
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