CN105129841A - Preparation method of indium oxide with octahedral morphology - Google Patents
Preparation method of indium oxide with octahedral morphology Download PDFInfo
- Publication number
- CN105129841A CN105129841A CN201510249868.XA CN201510249868A CN105129841A CN 105129841 A CN105129841 A CN 105129841A CN 201510249868 A CN201510249868 A CN 201510249868A CN 105129841 A CN105129841 A CN 105129841A
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- CN
- China
- Prior art keywords
- preparation
- indium oxide
- octahedral
- precursor
- indium
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Links
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229910003437 indium oxide Inorganic materials 0.000 title abstract description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 27
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004202 carbamide Substances 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002243 precursor Substances 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 5
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 7
- 238000007605 air drying Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 2
- 238000001816 cooling Methods 0.000 claims 1
- 239000008367 deionised water Substances 0.000 claims 1
- 229910021641 deionized water Inorganic materials 0.000 claims 1
- 238000009413 insulation Methods 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract 2
- 239000000243 solution Substances 0.000 abstract 2
- 238000003760 magnetic stirring Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 10
- 239000007788 liquid Substances 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 5
- 229910052738 indium Inorganic materials 0.000 description 3
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000010923 batch production Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
Abstract
The present invention relates to a preparation method of indium oxide with octahedral morphology, aims to solve the problems of difficult morphology control, complicated preparation process, higher synthesis temperature and longer reaction time of the preparation method of indium oxide with octahedral morphology in the prior art, and meanwhile provides a low-cost indium oxide octahedral structure material. The preparation method of the octahedral indium oxide structure is as follows: (1) a mixed solution of indium chloride and urea is prepared, ethylene glycol is added and dissolved, and by magnetic stirring, a homogeneous colorless and transparent solution is prepared; (2) the colorless and transparent solution is solvothermally reacted to collect a solvothermal product; (3) the solvothermal product is washed with absolute ethanol, centrifuged and dried to obtain a precursor; and (4) the indium oxide octahedral structure is obtained by calcination of the precursor. Advantages are that: the preparation method solves the difficult problem of product morphology control, is simple in process, low in synthesis temperature, and shorter in reaction time, so that the obtained product is low-cost, and has a wider range of application.
Description
Technical field
The present invention relates to a kind of preparation method with the Indium sesquioxide of shape of octahedron, be specifically related to a kind of solvent thermal has the Indium sesquioxide of shape of octahedron method in conjunction with high-temperature calcination preparation.
Background technology
Indium sesquioxide is a kind of new N-shaped transparent semiconductor functional materials, has wider energy gap, less resistivity and higher catalytic activity, is widely applied in photoelectric field, gas sensor, catalyzer.China is the country that indium resource is maximum, Ye Shi indium big producing country, but is still in the starting stage to the research of the deep processed product of its hi-tech.For making the indium resource of China reasonably be used and rise in value, development & production Indium sesquioxide and doped compound thereof should be strengthened.Recently, the synthesis with the indium oxide nanostructure of regular morphology causes the attention of people.People wish that this regular morphology can give the new character of nano material or potential application.
Summary of the invention
The object of the present invention is to provide a kind of preparation method with the Indium sesquioxide of shape of octahedron, its product good uniformity prepared, good crystallinity, and be easy to batch production.
The octahedral preparation method of said Indium sesquioxide is: (1) preparation indium chloride and urea mixing solutions, adds ethylene glycol and dissolves, make uniform colorless clear solution after magnetic agitation; (2) colourless transparent solution is reacted under solvent thermal, collect solvent thermal product; (3) by solvent thermal product washing with alcohol, centrifugal, be drying to obtain precursor; (4) precursor is obtained Indium sesquioxide octahedral structure through high-temperature roasting.
Product Process involved in the present invention is simple and easy to realize, and constant product quality and process repeatability can be good, and reaction parameter easily controls, safe and reliable, economical convenient and be easy to amplify and the advantage such as suitability for industrialized production; Gained there is the Indium sesquioxide pattern of shape of octahedron and dimensional homogeneity good, the advantages such as starting material are cheap and easy to get.
Accompanying drawing explanation
X-ray diffraction (XRD) collection of illustrative plates that Fig. 1 is product shown in embodiment 1;
Scanning power shovel (SEM) the pattern photo that Fig. 2 is product shown in embodiment 1;
Embodiment
Embodiment 1
Take 0.2gInCl
34H
2o and 0.064g urea, puts into beaker, adds 15mL ethylene glycol, form clear solution through magnetic agitation 2h, finally mixing solutions liquid being transferred to liner is in the stainless steel autoclave of tetrafluoroethylene, is incubated 24h at 120 DEG C, be cooled to room temperature in atmosphere, collect sample.With absolute ethanol washing, centrifugal, obtain white powder at 80 DEG C of air drying 6h.By dried white powder in tube furnace, the lower 600 DEG C of calcining 3h of air conditions, must have the Indium sesquioxide of shape of octahedron.
Embodiment 2
Take 0.2gInCl
34H
2o and 0.064g urea, puts into beaker, adds 15mL ethylene glycol, form clear solution through magnetic agitation 2h, finally mixing solutions liquid being transferred to liner is in the stainless steel autoclave of tetrafluoroethylene, is incubated 18h at 160 DEG C, be cooled to room temperature in atmosphere, collect sample.With absolute ethanol washing, centrifugal, obtain white powder at 60 DEG C of air drying 10h.By dried white powder in tube furnace, the lower 650 DEG C of calcining 2h of air conditions, must have the Indium sesquioxide of shape of octahedron.
Embodiment 3
Take 0.2gInCl
34H
2o and 0.066g urea, puts into beaker, adds 15mL ethylene glycol, form clear solution through magnetic agitation 2h, finally mixing solutions liquid being transferred to liner is in the stainless steel autoclave of tetrafluoroethylene, is incubated 18h at 160 DEG C, be cooled to room temperature in atmosphere, collect sample.With absolute ethanol washing, centrifugal, obtain white powder at 80 DEG C of air drying 12h.By dried white powder in tube furnace, the lower 650 DEG C of calcining 2h of air conditions, must have the Indium sesquioxide of shape of octahedron.
Embodiment 4
Take 0.2gInCl
34H
2o and 0.066g urea, puts into beaker, adds 15mL ethylene glycol, form clear solution through magnetic agitation 2h, finally mixing solutions liquid being transferred to liner is in the stainless steel autoclave of tetrafluoroethylene, is incubated 18h at 160 DEG C, be cooled to room temperature in atmosphere, collect sample.With absolute ethanol washing, centrifugal, obtain white powder at 80 DEG C of air drying 6h.By dried white powder in tube furnace, the lower 550 DEG C of calcining 2h of air conditions, must have the Indium sesquioxide of shape of octahedron.
Embodiment 5
Take 0.2gInCl
34H
2o and 0.066g urea, puts into beaker, adds 15mL ethylene glycol, form clear solution through magnetic agitation 2h, finally mixing solutions liquid being transferred to liner is in the stainless steel autoclave of tetrafluoroethylene, is incubated 24h at 160 DEG C, be cooled to room temperature in atmosphere, collect sample.With absolute ethanol washing, centrifugal, obtain white powder at 60 DEG C of air drying 10h.By dried white powder in tube furnace, the lower 500 DEG C of calcining 3h of air conditions, must have the Indium sesquioxide of shape of octahedron.
From the XRD test result with the Indium sesquioxide of shape of octahedron that the present invention obtains, the Indium sesquioxide characteristic diffraction peak that the present invention obtains is manganous carbonate crystalline phase.Scanning electron microscope (SEM) pattern photo shows the Indium sesquioxide with shape of octahedron that the present invention obtains.
Should be understood that, for those of ordinary skills, can be improved according to the above description or convert, and all these improve and convert the protection domain that all should belong to claims of the present invention.
Claims (5)
1. there is a preparation method for the Indium sesquioxide of shape of octahedron structure, it is characterized in that, (1) preparation indium chloride and urea mixing solutions, add ethylene glycol and dissolve, after magnetic agitation, make uniform colorless clear solution; (2) colourless transparent solution is reacted under solvent thermal, collect solvent thermal product; (3) by solvent thermal product through centrifugal, namely obtain precursor by washing with alcohol; (4) precursor is obtained Indium sesquioxide octahedral structure through high-temperature roasting.
2. method according to claim 1, it is characterized in that: described indium chloride and urea mixing solutions, its concentration is 0.7mmol Indium sesquioxide and the mixing of 1-2mmol urea, add 15mL ethylene glycol to dissolve, solvent thermal temperature is 120 DEG C-180 DEG C, insulation 6-36h, collects solvent thermal product after naturally cooling.
3. preparation method according to claim 1, is characterized in that described solvent thermal product, with washing with alcohol (can not use deionized water wash, precursor is met water and can be decomposed), at 60-80 DEG C of air drying 6-12h.
4. preparation method according to claim 1, is characterized in that precursor 400-700 DEG C of calcining 1-3h in tube furnace in described (4).
5. preparation method according to claim 1 obtains the Indium sesquioxide with shape of octahedron structure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510249868.XA CN105129841B (en) | 2015-05-16 | 2015-05-16 | Preparation method of indium oxide with octahedral morphology |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510249868.XA CN105129841B (en) | 2015-05-16 | 2015-05-16 | Preparation method of indium oxide with octahedral morphology |
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| Publication Number | Publication Date |
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| CN105129841A true CN105129841A (en) | 2015-12-09 |
| CN105129841B CN105129841B (en) | 2017-01-25 |
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| CN201510249868.XA Expired - Fee Related CN105129841B (en) | 2015-05-16 | 2015-05-16 | Preparation method of indium oxide with octahedral morphology |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105645464A (en) * | 2016-04-11 | 2016-06-08 | 中国石油大学(华东) | Preparation method of uniform-size In2O3 octahedral nanoparticles |
| CN110482593A (en) * | 2019-08-20 | 2019-11-22 | 临沂大学 | A kind of tufted In2O3Preparation method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08131815A (en) * | 1994-11-11 | 1996-05-28 | Catalysts & Chem Ind Co Ltd | Indium oxide sol. its production and substrate with conductive coating film |
| CN102863014A (en) * | 2012-10-18 | 2013-01-09 | 荣成百合生物技术有限公司 | Preparation method of shape-controllable nano indium oxides |
| CN104591264A (en) * | 2015-02-06 | 2015-05-06 | 西安工业大学 | Indium oxide nanosphere and preparation method thereof |
| CN104628263A (en) * | 2015-01-12 | 2015-05-20 | 济南大学 | Method for preparing indium oxide octahedral nanocrystal film |
-
2015
- 2015-05-16 CN CN201510249868.XA patent/CN105129841B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08131815A (en) * | 1994-11-11 | 1996-05-28 | Catalysts & Chem Ind Co Ltd | Indium oxide sol. its production and substrate with conductive coating film |
| CN102863014A (en) * | 2012-10-18 | 2013-01-09 | 荣成百合生物技术有限公司 | Preparation method of shape-controllable nano indium oxides |
| CN104628263A (en) * | 2015-01-12 | 2015-05-20 | 济南大学 | Method for preparing indium oxide octahedral nanocrystal film |
| CN104591264A (en) * | 2015-02-06 | 2015-05-06 | 西安工业大学 | Indium oxide nanosphere and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 董红星等: ""不同形貌氧化铟八面体的可控合成与发光性质"", 《科学通报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105645464A (en) * | 2016-04-11 | 2016-06-08 | 中国石油大学(华东) | Preparation method of uniform-size In2O3 octahedral nanoparticles |
| CN105645464B (en) * | 2016-04-11 | 2017-04-05 | 中国石油大学(华东) | A kind of size uniform In2O3The preparation method of octahedron nanometer particle |
| CN110482593A (en) * | 2019-08-20 | 2019-11-22 | 临沂大学 | A kind of tufted In2O3Preparation method |
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| Publication number | Publication date |
|---|---|
| CN105129841B (en) | 2017-01-25 |
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Granted publication date: 20170125 Termination date: 20210516 |