CN1974413B - Process of preparing nanometer hexagonal oxide sheet - Google Patents
Process of preparing nanometer hexagonal oxide sheet Download PDFInfo
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- CN1974413B CN1974413B CN 200610154730 CN200610154730A CN1974413B CN 1974413 B CN1974413 B CN 1974413B CN 200610154730 CN200610154730 CN 200610154730 CN 200610154730 A CN200610154730 A CN 200610154730A CN 1974413 B CN1974413 B CN 1974413B
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- Prior art keywords
- solution
- hexagonal oxide
- oxide sheet
- nanometer hexagonal
- preparing
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- 238000000034 method Methods 0.000 title claims abstract description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000003513 alkali Substances 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 3
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 3
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 2
- 238000001035 drying Methods 0.000 abstract description 5
- 229910001510 metal chloride Inorganic materials 0.000 abstract 1
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 10
- 235000015165 citric acid Nutrition 0.000 description 6
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 5
- 239000002086 nanomaterial Substances 0.000 description 5
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000003643 water by type Substances 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- MPMSMUBQXQALQI-UHFFFAOYSA-N cobalt phthalocyanine Chemical compound [Co+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 MPMSMUBQXQALQI-UHFFFAOYSA-N 0.000 description 2
- 230000005693 optoelectronics Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
- Compounds Of Iron (AREA)
Abstract
The present invention discloses process of preparing nanometer hexagonal oxide flake. The process includes the following steps: dissolving metal chloride in deionized water, adding citric acid and alkali source into the solution, treating the solution in a high pressure kettle at 100-200 deg.c for 1-48 hr, centrifuging and drying. The process is simple, can obtain nanometer hexagonal oxide flake in special 2D nanometer structure, and lays foundation for the deep research and application in photoelectronic field.
Description
Technical field
The present invention relates to a kind of method for preparing nanometer hexagonal oxide sheet.
Background technology
Oxide compound is the important semiconductor material of a class, and they are widely used in the optoelectronic areas such as sensor, photodiode, detector.Recently due to the development of nanotechnology, many character that are different from the oxide compound block have been found, as the Laser emission of array zinc oxide etc.And the discovery of these new physics phenomenons impels people to explore new, a large amount of, effective, the low-cost method for preparing nano material.Comparatively ripe for the preparation of oxide compound one dimension Nano structure such as nano wire, nanometer rod and nanotube at present, and for the oxide compound two-dimensional nanostructure of no less important, the particularly preparation of regular flake nano structure and application studied lessly, more lacks general preparation method and mechanism.
Summary of the invention
The purpose of this invention is to provide a kind of simple method that effectively prepares nanometer hexagonal oxide sheet.
The method for preparing nanometer hexagonal oxide sheet of the present invention comprises the following steps:
1) the metal chlorate is dissolved in deionized water, then adds citric acid in solution, the mol ratio of citric acid and metal chlorate is 0.1～10: 1;
2) add alkali source in mentioned solution, the mol ratio of alkali source and metal-salt is 0.1～10: 1;
3) step 2) solution that makes puts into autoclave, and processed 1～48 hour at 100～200 ℃ of temperature, then centrifugal, dry, obtain nanometer hexagonal oxide sheet.
Above-mentioned metal chlorate can be iron(ic) chloride or cobalt chloride; Said alkali source can be sodium hydroxide or potassium hydroxide.The pressure of autoclave is determined by temperature.
Beneficial effect of the present invention is:
Preparation technology is simple, adopts the inventive method can obtain the special two-dimensional nanostructure of nanometer hexagonal oxide sheet, for further investigation and the application of optoelectronic areas provides the basis.
Description of drawings
The stereoscan photograph of Fig. 1 ferric oxide nano-hexagonal sheet;
The transmission electron microscope photo of Fig. 2 ferric oxide nano-hexagonal sheet;
The stereoscan photograph of Fig. 3 cobaltosic oxide nano six square pieces;
The transmission electron microscope photo of Fig. 4 cobaltosic oxide nano six square pieces.
Embodiment
Further illustrate the present invention below in conjunction with embodiment.
Embodiment 1
6 mmole iron(ic) chloride are dissolved in 40 ml waters, then add 0.6 mmole citric acid, stir after 10 minutes, add again 30 milliliters of 2M sodium hydroxide, the above-mentioned solution for preparing is put into autoclave, processed 20 hours under 200 ℃, the solution centrifugal of handling well, drying, the nano-hexagonal sheet of acquisition ferric oxide.Fig. 1 and Fig. 2 are stereoscan photograph and the transmission electron microscope photos of ferric oxide nano-hexagonal sheet.As seen from the figure, the nano-hexagonal sheet is of a size of 100 nanometers, and thickness is 20 nanometers.
Embodiment 2:
40 mmole iron(ic) chloride are dissolved in 40 ml waters, then add 40 mmole citric acids, stir after 10 minutes, add again 2 milliliter of 2 mol/L potassium hydroxide, the above-mentioned solution for preparing is put into autoclave, processed 48 hours under 100 ℃, the solution centrifugal of handling well, drying, the nano-hexagonal sheet of acquisition ferric oxide.Its result is similar with example 1.
Embodiment 3:
2 mmole Cobaltous diacetates are dissolved in 80 ml waters, then the citric acid that adds 0.2 mmole, stir after 10 minutes, add again 10 milliliter of 2 mol/L sodium hydroxide, the above-mentioned solution for preparing is put into autoclave, processed 12 hours under 160 ℃, the solution centrifugal of handling well, drying, the nano-hexagonal sheet of acquisition tricobalt tetroxide.Fig. 3 and Fig. 4 are stereoscan photograph and the transmission electron microscope photos of cobaltosic oxide nano six square pieces.
Embodiment 4:
20 mmole Cobaltous diacetates are dissolved in 80 ml waters, then the citric acid that adds 20 mmoles, stir after 10 minutes, add again 1 milliliter of 2 mol/L potassium hydroxide, the above-mentioned solution for preparing is put into autoclave, processed 12 hours under 180 ℃, the solution centrifugal of handling well, drying, the nano-hexagonal sheet of acquisition tricobalt tetroxide.Its result is similar with example 3.
Claims (2)
1. method for preparing nanometer hexagonal oxide sheet is characterized in that comprising the following steps:
1) the metal chlorate is dissolved in deionized water, then adds citric acid in solution, the mol ratio of citric acid and metal chlorate is 0.1～10:1, and said metal chlorate is iron(ic) chloride or cobalt chloride;
2) add alkali source in mentioned solution, the mol ratio of alkali source and metal-salt is 0.1～10:1;
3) step 2) solution that makes puts into autoclave, and processed 1～48 hour at 100～200 ℃ of temperature, then centrifugal, dry, obtain nanometer hexagonal oxide sheet.
2. the method for preparing nanometer hexagonal oxide sheet according to claim 1, is characterized in that said alkali source is sodium hydroxide or potassium hydroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610154730 CN1974413B (en) | 2006-11-21 | 2006-11-21 | Process of preparing nanometer hexagonal oxide sheet |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610154730 CN1974413B (en) | 2006-11-21 | 2006-11-21 | Process of preparing nanometer hexagonal oxide sheet |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1974413A CN1974413A (en) | 2007-06-06 |
| CN1974413B true CN1974413B (en) | 2013-06-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 200610154730 Expired - Fee Related CN1974413B (en) | 2006-11-21 | 2006-11-21 | Process of preparing nanometer hexagonal oxide sheet |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102139929A (en) * | 2011-03-28 | 2011-08-03 | 浙江理工大学 | Method for preparing Co3O4 nanometer sheet |
| CN107500363B (en) * | 2017-08-16 | 2018-12-28 | 青岛大学 | A kind of preparation method of prism hexa-prism nano iron oxide |
| CN107697943A (en) * | 2017-10-31 | 2018-02-16 | 电子科技大学 | A kind of preparation method of flake nano metal oxide |
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- 2006-11-21 CN CN 200610154730 patent/CN1974413B/en not_active Expired - Fee Related
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| CN1974413A (en) | 2007-06-06 |
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