CN101830523A - Method for preparing nickel-based oxide nano structure - Google Patents
Method for preparing nickel-based oxide nano structure Download PDFInfo
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- CN101830523A CN101830523A CN 201010195413 CN201010195413A CN101830523A CN 101830523 A CN101830523 A CN 101830523A CN 201010195413 CN201010195413 CN 201010195413 CN 201010195413 A CN201010195413 A CN 201010195413A CN 101830523 A CN101830523 A CN 101830523A
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- triphenylphosphine
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- oleyl amine
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Abstract
The invention discloses a method for preparing a nickel-based oxide nano structure, and belongs to the field of electronic information component materials. The method adopts an organic liquid-phase chemical reaction method, provides a high-temperature reaction environment by using the high boiling point of oil amine under oxygen atmosphere, and synthesizes NiO nuclear shell nano granules by using acetylacetone nickel as a nickel source and using triphenylphosphine as a surfactant. The method is simple, needs few raw materials, and has lower cost.
Description
Technical field
The invention belongs to field of electronic information component materials.
Background technology
In the present information age, extensively the information technology that adopts is that the magnetic information code is write magnetic mnemon on the different spatial, and reads and writes them by spacescan.In order to improve the Card read/write capacity, just must with magnetic mnemon corresponding ferromagnetic particle do more and more littler.For widely used single-phase ferromagnetic nano particle, particulate is ferromagnetic-super paramagnetic transition temperature constantly reduces along with reducing of volume, so that the coercive force of room temperature and residual magnetization be zero, lost the function as the magnetic information memory.So-called thereby " super paramagnetic limit " makes the miniaturization development of magnetic information functional device run into technical bottleneck, limited the further raising of magnetic information capacity.
When constantly scantling being reduced to nanoscale, scientists finds that the nano particle that is obtained has many chemistry and physical propertiess that are different from its corresponding bulk.Novel nano structure such as core-shell nano particle have the chemistry and the physical properties that are different from single-phase solid nano particle again, the present extremely scientist institute extensive concern in fields such as chemistry, physics and materialogy.And for the core-shell nano particle, the introducing of shell can influence the spin magnetic moment orientation of nuclear, so that the outer effects such as magnetic coupling that can produce nuclear and shell after the match, thereby has and the diverse magnetic property of single phase nano particle.Therefore, finding on the basis of nanometer magnetic phenomenon and rule at present, by design with prepare various novel nano structures, and explore nanometer magnetic effect and the function that it may have, may utilize the new nanometer magnetic effect of being found to break through " super paramagnetic limit ", and make further raising magnetic information capacity become possibility.
At present, the preparation method of nickel-based oxide nano structure and this material in various documents all without any report.
Summary of the invention
The objective of the invention is to address the above problem and a kind of preparation method of nickel-based oxide nano structure is provided, utilizing this method can prepare on magnetic structure with the antiferromagnetism is nuclear, and the class ferromegnetism is the NiO core-shell nano particle of shell.
The technical solution adopted in the present invention is:
A kind of preparation method of nickel-based oxide nano structure may further comprise the steps:
(a) acetylacetonate nickel is put in the there-necked flask, added oleyl amine, under aerating oxygen and the magnetic agitation, 80
oC～160
o C insulation 20～60 minutes, forerunner's complex liquid of formation nickel-oleyl amine, the concentration of this forerunner's complex liquid is 0.1～0.5mol/L, and wherein analytically pure acetylacetonate nickel is as the Ni ion source, and oleyl amine is as organic solvent;
(b) keeping triphenylphosphine being added in above-mentioned forerunner's complex liquid 80 under logical oxygen and the magnetic agitation situation
oC～160
o C insulation 20～60 minutes forms the deep green clear solution, and wherein analytically pure triphenylphosphine is as tensio-active agent, and the mol ratio of triphenylphosphine and acetylacetonate nickel is 5:1～10:1;
(c) be rapidly heated 180
oC～300
oC and be incubated 20～90 minutes forms dark solution, then cool to room temperature rapidly;
(d) to be cooled to room temperature, add excessive dehydrated alcohol and produce precipitation, remove supernatant liquid, the centrifugation product obtains the NiO nano particle then.
Further, it is nuclear that resulting NiO nano particle has on magnetic structure with the antiferromagnetism, and the class ferromegnetism is the core-shell nano particle of shell, has exchange bias effect at low temperature.
The present invention has the following advantages:
Utilizing method of the present invention can obtain on magnetic structure with the antiferromagnetism is nuclear, and the class ferromegnetism is the NiO core-shell nano particle of shell, and has tangible exchange bias effect in low-temperature test.The nano particle that obtains has the controlled and homogeneous distribution of particle size, and is widely used in the important inorganic materials in fields such as battery electrode, catalyzer, magneticsubstance and ceramic coloring material; Present method is simple simultaneously, and required starting material are less, and cost is lower.
Description of drawings
Fig. 1 is the XRD figure spectrum of NiO core-shell nano particulate samples among the embodiment 1;
Fig. 2 is the TEM collection of illustrative plates of NiO core-shell nano particulate samples among the embodiment 1;
Fig. 3 is the M-H collection of illustrative plates of NiO core-shell nano particulate samples among the embodiment 1.
Embodiment
Embodiment 1
Adopt the organic liquid phase chemical reaction method, under oxygen atmosphere, utilize the high boiling point of oleyl amine that the pyroreaction environment is provided, and be that nickel source and triphenylphosphine are that tensio-active agent synthesizes NiO core-shell nano particle with the acetylacetonate nickel.The first step takes by weighing the 0.002mol acetylacetonate nickel and puts in the there-necked flask of 250mL, adds oleyl amine 13mL, under logical oxygen atmosphere and magnetic agitation, and 100
o C insulation 30 minutes, forerunner's complex liquid of formation nickel-oleyl amine, this concentration of driving complex liquid is 0.15mol/L.In second step, keeping the 0.014mol triphenylphosphine being added in the above-mentioned solution 100 under logical oxygen atmosphere and the magnetic agitation situation
oC insulation 20 minutes forms the deep green clear solution, and the mol ratio of triphenylphosphine and acetylacetonate nickel is 7:1.In the 3rd step, be rapidly heated 200
oC and be incubated 30 minutes forms dark solution, then cool to room temperature rapidly.The 4th step, to be cooled to room temperature, add excessive dehydrated alcohol and produce gray precipitate, remove supernatant liquid, the centrifugation product obtains NiO core-shell nano particle then.
Utilize embodiment 1 to prepare NiO core-shell nano particulate XRD as shown in Figure 1, sample has formed good cube phase structure NiO as can be seen from Figure 1.NiO core-shell nano particles dispersed is formed suspension in normal hexane, drops on the copper mesh that is sprayed with carbon film and in drying at room temperature, the transmission electron microscope collection of illustrative plates of this sample as shown in Figure 2, the M-H collection of illustrative plates of this NiO core-shell nano particulate samples is as shown in Figure 3.
Embodiment 2
Adopt the organic liquid phase chemical reaction method, under oxygen atmosphere, utilize the high boiling point of oleyl amine that the pyroreaction environment is provided, and be that nickel source and triphenylphosphine are that tensio-active agent synthesizes NiO core-shell nano particle with the acetylacetonate nickel.The first step takes by weighing the 0.004mol acetylacetonate nickel and puts in the there-necked flask of 250mL, adds oleyl amine 15mL, under logical oxygen atmosphere and magnetic agitation, and 160
o C insulation 20 minutes, forerunner's complex liquid of formation nickel-oleyl amine, this concentration of driving complex liquid is 0.26mol/L.In second step, keeping the 0.020mol triphenylphosphine being added in the above-mentioned solution 160 under logical oxygen atmosphere and the magnetic agitation situation
oC insulation 40 minutes forms the deep green clear solution, and the mol ratio of triphenylphosphine and acetylacetonate nickel is 5:1.In the 3rd step, be rapidly heated 180
oC and be incubated 20 minutes forms dark solution, then cool to room temperature rapidly.The 4th step, to be cooled to room temperature, add excessive dehydrated alcohol and produce gray precipitate, remove supernatant liquid, the centrifugation product obtains NiO core-shell nano particle then.
It should be noted last that, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can make amendment or be equal to replacement technical scheme of the present invention, and not breaking away from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (2)
1. the preparation method of a nickel-based oxide nano structure is characterized in that, may further comprise the steps:
(a) acetylacetonate nickel is put in the there-necked flask, added oleyl amine, under aerating oxygen and the magnetic agitation, 80
oC～160
oC insulation 20～60 minutes, forerunner's complex liquid of formation nickel-oleyl amine, the concentration of this forerunner's complex liquid is 0.1～0.5mol/L, and wherein analytically pure acetylacetonate nickel is as the Ni ion source, and oleyl amine is as organic solvent;
(b) keeping triphenylphosphine being added in above-mentioned forerunner's complex liquid 80 under logical oxygen and the magnetic agitation situation
oC～160
oC insulation 20～60 minutes forms the deep green clear solution, and wherein analytically pure triphenylphosphine is as tensio-active agent, and the mol ratio of triphenylphosphine and acetylacetonate nickel is 5:1～10:1;
(c) be rapidly heated 180
oC～300
oC and be incubated 20～90 minutes forms dark solution, then cool to room temperature rapidly;
(d) to be cooled to room temperature, add excessive dehydrated alcohol and produce precipitation, remove supernatant liquid, the centrifugation product obtains the NiO nano particle then.
2. the preparation method of nickel-based oxide nano structure according to claim 1, it is characterized in that, it is nuclear that resulting NiO nano particle has on magnetic structure with the antiferromagnetism, and the class ferromegnetism is the core-shell nano particle of shell, has exchange bias effect at low temperature.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108816262A (en) * | 2018-04-25 | 2018-11-16 | 西安交通大学 | A kind of preparation method of nickel oxide-nitridation carbon composite photocatalyst |
| CN112246281A (en) * | 2020-10-28 | 2021-01-22 | 南京工程学院 | Catalyst for preparing lactic acid from glycerol, preparation method and application |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101525161A (en) * | 2009-04-03 | 2009-09-09 | 天津大学 | Method for preparing nickel oxide one dimension nano material |
| CN101624216A (en) * | 2008-07-10 | 2010-01-13 | 中国石油化工股份有限公司 | Method for preparing nano nickel oxide |
| US20100031775A1 (en) * | 2008-08-05 | 2010-02-11 | Samsung Electro-Mechanics Co., Ltd. | Method for preparing nickel nanoparticles |
| CN101691246A (en) * | 2009-09-27 | 2010-04-07 | 武汉理工大学 | Method for synthesizing nickel oxide nano particles by one step |
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2010
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101624216A (en) * | 2008-07-10 | 2010-01-13 | 中国石油化工股份有限公司 | Method for preparing nano nickel oxide |
| US20100031775A1 (en) * | 2008-08-05 | 2010-02-11 | Samsung Electro-Mechanics Co., Ltd. | Method for preparing nickel nanoparticles |
| CN101525161A (en) * | 2009-04-03 | 2009-09-09 | 天津大学 | Method for preparing nickel oxide one dimension nano material |
| CN101691246A (en) * | 2009-09-27 | 2010-04-07 | 武汉理工大学 | Method for synthesizing nickel oxide nano particles by one step |
Non-Patent Citations (3)
| Title |
|---|
| 《Polyhedron》 20090206 Salavati-Niasari M. et al. Synthesis and characterization of NiO nanoclusters via thermal decomposition 1111-1114 1-2 第28卷, 2 * |
| 《中国陶瓷》 20040430 李秀艳等 超细NiO粉体的制备及其应用 21-24 1-2 第40卷, 第2期 2 * |
| 《化学工程》 20070831 李建芬等 均匀沉淀法制备纳米氧化镍及其工艺优化 53-56 1-2 第35卷, 第8期 2 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108816262A (en) * | 2018-04-25 | 2018-11-16 | 西安交通大学 | A kind of preparation method of nickel oxide-nitridation carbon composite photocatalyst |
| CN112246281A (en) * | 2020-10-28 | 2021-01-22 | 南京工程学院 | Catalyst for preparing lactic acid from glycerol, preparation method and application |
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