CN100429152C - Process for preparing oxide nano sphere - Google Patents
Process for preparing oxide nano sphere Download PDFInfo
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- CN100429152C CN100429152C CNB2006101547285A CN200610154728A CN100429152C CN 100429152 C CN100429152 C CN 100429152C CN B2006101547285 A CNB2006101547285 A CN B2006101547285A CN 200610154728 A CN200610154728 A CN 200610154728A CN 100429152 C CN100429152 C CN 100429152C
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- oxide nano
- metal chlorate
- cupric
- alkali source
- formaldehyde
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- Inorganic Compounds Of Heavy Metals (AREA)
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Abstract
The invention discloses a making method of oxide nanometer ball, which comprises the following steps: dissolving metal chloride into deionized water; adding formaldehyde; adding alkali source into the solution; placing in the high-pressure autoclave; disposing under 100-200 deg. c for 1-48h; centrifuging; drying to obtain the product.
Description
Technical field
The present invention relates to a kind of method for preparing oxide nano sphere.
Background technology
Oxide compound is the important semiconductor material of a class, and they are widely used in optoelectronic areas such as varistor, photodiode, detector.Recently because many character that are different from the oxide compound block have been found in the development of nanotechnology, as the superior lithium ion battery performance of ferric oxide nano pipe etc.And the discovery of these new physics phenomenons has promoted explorations new, the various nanostructure methods of a large amount of, effective, low-cost preparations.The spherical oxide nanostructure is widely used in biomedical sectors such as magnetic resolution, medicament transport, nuclear magnetic resonance image enhancing at present.The method for preparing at present the spherical oxide nanostructure mainly is to realize by the parcel of template or tensio-active agent, and its shortcoming is a complex process, pollutes easily, and template is removed than shortcomings such as difficulties.
Summary of the invention
The purpose of this invention is to provide that a kind of technology is simple, surfactant-free, do not need the method for preparing oxide nano sphere of template.
The method for preparing oxide nano sphere of the present invention may further comprise the steps:
1) the metal chlorate is dissolved in the deionized water, and adds formaldehyde, the mol ratio of formaldehyde and metal chlorate is 0.1～10: 1;
2) add alkali source in above-mentioned solution, the mol ratio of alkali source and metal chlorate is 0.1～10: 1;
3) step 2) solution that makes puts into autoclave, handles 1～48 hour under 100～200 ℃ of temperature, and is centrifugal then, dry, obtains oxide nano sphere.
Above-mentioned metal chlorate can be iron(ic) chloride or cupric 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, utilizes formaldehyde can avoid the use of template and organic surface active agent for reaction solvent.
Description of drawings
Fig. 1 is the stereoscan photograph of ferricoxide nanospheres;
Fig. 2 is the transmission projection Electronic Speculum of ferricoxide nanospheres;
Fig. 3 is the stereoscan photograph of cupric oxide nano ball;
Fig. 4 is the transmission projection Electronic Speculum of cupric oxide nano ball.
Embodiment
Further specify the present invention below in conjunction with embodiment.
Embodiment 1
6 mmole iron(ic) chloride are dissolved in 40 ml waters, the formaldehyde that adds 0.6 mmole then, stir after 10 minutes, add 30 milliliter of 2 mol sodium hydroxide again, the above-mentioned solution for preparing is put into autoclave, handled 48 hours down at 200 ℃, the solution centrifugal of handling well, drying, the nanometer ball of acquisition ferric oxide.Fig. 1 and Fig. 2 are respectively the scanning electron microscope and the transmission electron microscope photos of ferricoxide nanospheres, and the diameter of nanometer ball is about 100～300nm.
Embodiment 2
10 mmole iron(ic) chloride are dissolved in 40 ml waters, the formaldehyde that adds 100 mmoles then, stir after 10 minutes, add 5 milliliter of 2 mol potassium hydroxide again, the above-mentioned solution for preparing is put into autoclave, handled 2 hours down at 100 ℃, the solution centrifugal of handling well, drying, the nanometer ball of acquisition ferric oxide.The diameter of the nanometer ball of ferric oxide is about 100～300nm.
Embodiment 3
12 mmole cupric chlorides are dissolved in 40 ml waters, the formaldehyde that adds 2 mmoles then, stir after 10 minutes, add 30 milliliter of 2 mol potassium hydroxide again, the above-mentioned solution for preparing is put into autoclave, handled 20 hours down at 180 ℃, the solution centrifugal of handling well, drying, the nanometer ball of acquisition cupric oxide.Fig. 3 and Fig. 4 are respectively the scanning electron microscope and the transmission electron microscope photos of cupric oxide nano ball.The diameter of cupric oxide nano ball is approximately 100～300nm.
Embodiment 4
20 mmole cupric chlorides are dissolved in 40 ml waters, the formaldehyde that adds 2 mmoles then, stir after 10 minutes, add 1 milliliter of 2 mol sodium hydroxide again, the above-mentioned solution for preparing is put into autoclave, handled 1 hour down at 200 ℃, the solution centrifugal of handling well, drying, the nanometer ball of acquisition cupric oxide.The diameter of cupric oxide nano ball is approximately 100～300nm.
Claims (2)
1. method for preparing ferric oxide or cupric oxide nano ball is characterized in that may further comprise the steps:
1) the metal chlorate is dissolved in the deionized water, and adds formaldehyde, the mol ratio of formaldehyde and metal chlorate is 0.1～10: 1;
2) add alkali source in above-mentioned solution, the mol ratio of alkali source and metal chlorate is 0.1～10: 1;
3) step 2) solution that makes puts into autoclave, handles 1～48 hour under 100～200 ℃ of temperature, and is centrifugal then, dry, obtains oxide nano sphere;
Above-mentioned metal chlorate is iron(ic) chloride or cupric chloride.
2. the above-mentioned method for preparing ferric oxide or cupric oxide nano ball 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 |
|---|---|---|---|
| CNB2006101547285A CN100429152C (en) | 2006-11-21 | 2006-11-21 | Process for preparing oxide nano sphere |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101547285A CN100429152C (en) | 2006-11-21 | 2006-11-21 | Process for preparing oxide nano sphere |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1994889A CN1994889A (en) | 2007-07-11 |
| CN100429152C true CN100429152C (en) | 2008-10-29 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006101547285A Expired - Fee Related CN100429152C (en) | 2006-11-21 | 2006-11-21 | Process for preparing oxide nano sphere |
Country Status (1)
| Country | Link |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101279758B (en) * | 2008-05-16 | 2010-06-02 | 西北师范大学 | Preparation of nano-cupric oxide powder |
| CN105036174A (en) * | 2015-07-10 | 2015-11-11 | 安鹏九 | Production method for submicron electronic-grade copper oxide powder |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1364730A (en) * | 2002-02-08 | 2002-08-21 | 无锡威孚吉大新材料应用开发有限公司 | Method for preparing super-fine nanometer ferric oxide powder |
| CN1524796A (en) * | 2003-02-28 | 2004-09-01 | 中国科学院过程工程研究所 | Method for synthesizing ferric oxide nanometer powder by hydrothermal back extraction |
| CN1709799A (en) * | 2004-06-16 | 2005-12-21 | 中南大学 | Method for preparing superfine/nano iron oxide/iron powder |
| EP1614659A2 (en) * | 2000-07-31 | 2006-01-11 | Sumitomo Chemical Company, Limited | Titanium oxide production process |
-
2006
- 2006-11-21 CN CNB2006101547285A patent/CN100429152C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1614659A2 (en) * | 2000-07-31 | 2006-01-11 | Sumitomo Chemical Company, Limited | Titanium oxide production process |
| CN1364730A (en) * | 2002-02-08 | 2002-08-21 | 无锡威孚吉大新材料应用开发有限公司 | Method for preparing super-fine nanometer ferric oxide powder |
| CN1524796A (en) * | 2003-02-28 | 2004-09-01 | 中国科学院过程工程研究所 | Method for synthesizing ferric oxide nanometer powder by hydrothermal back extraction |
| CN1709799A (en) * | 2004-06-16 | 2005-12-21 | 中南大学 | Method for preparing superfine/nano iron oxide/iron powder |
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| CN1994889A (en) | 2007-07-11 |
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Granted publication date: 20081029 Termination date: 20121121 |