CN105436510A - Method for preparing chemical and magnetic ordered-phase nanoparticles - Google Patents
Method for preparing chemical and magnetic ordered-phase nanoparticles Download PDFInfo
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- CN105436510A CN105436510A CN201410437402.8A CN201410437402A CN105436510A CN 105436510 A CN105436510 A CN 105436510A CN 201410437402 A CN201410437402 A CN 201410437402A CN 105436510 A CN105436510 A CN 105436510A
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Abstract
The invention provides a method for preparing chemical and magnetic ordered-phase nanoparticles through a one-step solid-phase high-temperature sintering process. The method comprises the steps that a large amount of solid dispersing agent powder, such as NaCl and KCl, which can be dissolved in water easily and metal precursor powder are evenly mixed; high-temperature calcination is directly conducted on the mixed powder for the thermal decomposition reaction, so that other elements, except metal elements, in a precursor are removed; and the calcination temperature is controlled to be higher than the magnetic ordered-phase forming temperature, so that crystal-phase growth of prepared nanoparticles is promoted by using dispersing agents as carriers, and thus the chemical and magnetic ordered-phase nanoparticles are obtained. Compared with an existing preparation technique that chemical and magnetic ordered-phase nanoparticles can be obtained only after annealing of chemical disorder nanoparticles synthetized in liquid-phase mode, by the adoption of the method, the chemical and magnetic ordered-phase nanoparticles can be obtained through one-step synthesis without the annealing process, phenomena of agglomeration and growth of the nanoparticles in the high-temperature calcinations are avoided, and the method has good application prospects.
Description
Technical field
The invention belongs to magnetic nanoparticle preparing technical field, particularly relate to the preparation method of a kind of chemistry and magnetic order phase nano particle.
Background technology
At present, the main stream approach preparing magnetic metal nano particle is high-temperature liquid-phase chemical synthesis, the method is dissolved in reaction dissolvent by metal precursor, and add dispersant etc., heat up under liquid phase environment after Homogeneous phase mixing and carry out chemical heat decomposition reaction, then centrifugation liquid phase, obtains magnetic nanoparticle, then carries out annealing in process.Such as, the people such as Sun, S. report in certain reaction dissolvent in following document 1 with document 2, with oleic acid and oleyl amine for surfactant, are prepared the method for FePt dispersed nano particle by thermal decomposition various metals salt.
Document 1:SunS.etal.MonodisperseFePtnanoparticlesandferromagneti cFePtnanocrystalsuperlattices [J] .Science, 2000,287 (5460): 1989-1992.
Document 2:SunS.etal.Size-controlledsynthesisofmagnetitenanoparti cles [J] .JournaloftheAmericanChemicalSociety, 2002,124 (28): 8204-8205.
But the nano particle utilizing above-mentioned high-temperature liquid-phase chemical synthesis process to prepare often in chemical unordered phase and magnetic disorder phase, adopts the further the high temperature anneal of nano particle that will obtain at present for this reason.Such as, the nano particle of FCC structure (i.e. face-centred cubic structure) through the FePt particle of high-temperature liquid-phase chemical synthesis in above-mentioned document 1 and document 2, its crystalline phase is chemistry and magnetic disorder phase, in order to obtain the FCT structure (i.e. face-centered tetragonal structure) with chemistry and magnetic order phase, need to adopt the high temperature anneal further to the nano particle of this FCC structure.
But nano particle is easily reunited, is grown up in annealing process.In order to avoid this phenomenon, there is researcher coated Si O on prepared nano particle
2, carry out high annealing after the shell such as CaO, when acquisition chemistry and magnetic order mutually after remove this shell again.Although the method is conducive to preventing nanoparticle agglomerates from growing up, is the increase in processing step, improves preparation cost.In addition, also have researcher adopt salt bed subsequent heat treatment technique, but still need with first with high temperature thermal decomposition legal system for go out nano particle.
Summary of the invention
For the above-mentioned state of the art, the invention provides the new method of a kind of preparative chemistry and magnetic order phase nano particle, the method cost is low, simple, and high-temperature heat treatment one step can be adopted to obtain having the nano particle of chemistry and magnetic order phase.
Technical scheme of the present invention is: a kind of method of preparative chemistry and magnetic order phase nano particle, the method is using the material soluble in water such as NaCl, KCl as dispersant, by metal precursor powder and dispersant powder Homogeneous phase mixing, the mole of described dispersant powder is greater than the mole of metal precursor powder; Then, mix powder is carried out high-temperature calcination, to remove all the other elements in metal precursor except metallic element, and control calcining heat and to coordinate phase temperature higher than magnetic order, make metallic element be that carrier carries out grain growth with dispersant; Finally, be cooled to room temperature, be dissolved in by calcined product in deionized water, centrifugal segregation dispersant, obtains magnetic nanoparticle.
Described metallic element comprises any one or two or more complex elements in Fe, Co, Ni, Mn, Pt etc.
Described metal precursor comprises metallic element, and described metal precursor is not limit, and can be the salt or acid etc. of corresponding metal.
As preferably, described metal precursor is one or both the mixture in the acetylacetonate of corresponding metal, carbonyls.
When metallic element is Fe, metal precursor includes but not limited to the mixture of one or more in ferric acetyl acetonade, carbonyl iron etc.
When metallic element is Pt, metal precursor includes but not limited to the mixture of one or more in acetylacetone,2,4-pentanedione platinum, chloroplatinic acid etc.
Described dispersant powder and the mixed method of metal salt powder are not limit, and comprise ball milling, mechanical mixture etc.In order to ensure the uniformity mixed, can mix with dispersant powder after in metallic precursor powder dispersion to solvent as optimization.
As preferably, the particle diameter of described dispersant powder is 1-20 micron; The particle diameter of metal precursor powder is 1-30 micron.
As preferably, the ratio of the mole of described dispersant powder and the mole of metal precursor powder is 10-1000, more preferably 100-500;
Described high-temperature calcination stove is not limit, and comprises tube furnace, batch-type furnace etc.
As preferably, in calcination process, pass into inert gas.As further preferably, in calcination process, first pass into inert gas Ar deaeration, then pass into Ar and H that volume ratio is 95:5
2mist; This mixed gas flow is preferably 10-400ml/min.
As preferably, in calcination process, heating rate is 1 DEG C/min-10 DEG C/min.
As preferably, after temperature rises to calcining heat, carry out isothermal holding, temperature retention time is preferably 0.5-4h.
In sum, the present invention adopts solid dispersion powder soluble in water in a large number and metal precursor powder Homogeneous phase mixing, pyrolysis is carried out in direct for mixed-powder high-temperature calcination, to remove all the other elements in presoma except metallic element, and control the one-tenth phase temperature of calcining heat higher than this magnetic order phase, to impel this metallic element to be that carrier carries out crystalline phase growth with dispersant, thus obtain the metal nanoparticle with chemistry and magnetic order phase, its grain size is 2-100nm.Compared with prior art, the method has following beneficial effect:
(1) adopt solid dispersion soluble in water, and control the mole that its mole is greater than metal precursor powder, these technical measures produce following (a)-(c) beneficial effect:
A () is when effectively being split by this solid dispersion powder particle between metal precursor powder particle after this metal dispersion powder and metal precursor powder Homogeneous phase mixing, and as avoiding the isolated material of nanoparticle agglomerates during high-temperature calcination, thus avoid the reunion between the metal nanoparticle that obtains in high-temperature calcination, phenomenon of growing up.
B () is in high-temperature burning process, this solid dispersion can be used as carrier simultaneously, metal nanoparticle is carried out into grow up mutually, from but the magnetic nanoparticle of a step solid phase high temperature method synthetic chemistry and magnetic order, unordered with existing liquid phase synthesis chemistry, could obtain chemistry to compare with the technology of preparing of the nano particle of magnetic order in order after annealing, without the need to annealing process, one-step synthesis obtains the metal nanoparticle with chemistry and magnetic order phase to the method.
C, after () high-temperature calcination, can remove this dispersant after directly adopting deionized water centrifugal treating, therefore simple, cost is low, has a good application prospect.
(2) the method one-step synthesis can obtain chemistry and the nano particle of magnetic order phase, in addition safety non-toxic, environmentally friendly, output is large.
Accompanying drawing explanation
Fig. 1 is the TEM figure of the FePt nano particle that the embodiment of the present invention 1 obtains;
Fig. 2 is the XRD figure of the FePt nano particle that the embodiment of the present invention 1 obtains;
Fig. 3 is the room temperature hysteresis curve of the FePt nano particle that the embodiment of the present invention 1 obtains;
Fig. 4 is the TEM figure of the FePt nano particle that the embodiment of the present invention 2 obtains;
Fig. 5 is the XRD figure of the FePt nano particle that the embodiment of the present invention 2 obtains;
Fig. 6 is the room temperature hysteresis curve of the FePt nano particle that the embodiment of the present invention 2 obtains.
Detailed description of the invention
Below in conjunction with accompanying drawing and embodiment, the present invention is described in further detail, it is pointed out that the following stated embodiment is intended to be convenient to the understanding of the present invention, and any restriction effect is not play to it.
Embodiment 1:
(1) get 1molNaCl, in vacuum drying chamber after drying, add 25ml normal heptane and put into planetary ball mill ball milling together 2 days, obtain the NaCl powder of particle size below 20 microns;
(2) together with the NaCl powder acetylacetone,2,4-pentanedione platinum of the ferric acetyl acetonade of 0.75mmol and 0.5mmol and step (1) obtained, ball milling 10h mixes;
(3) put into Noah's ark after mixed-powder taking-up being dried, be then placed in tubular annealing stove and calcine, tubular annealing stove first with Ar gas deaeration, passes into Ar and H during heating
2mist, Ar and H
2percent by volume be 95:5, mixed gas flow is 10ml-400ml/min, control programming rate be 10 DEG C/min, after being warming up to 750 DEG C be incubated 1 hour, insulation terminate after under atmosphere protection, be cooled to room temperature, obtain calcined product;
(4) add in calcined product by deionized water, to dissolve NaCl wherein, then put into centrifuge separation and wash away NaCl, obtain FePt nano particle.
Fig. 1 is the TEM figure of above-mentioned obtained FePt nano particle, therefrom can find out that this particle is dispersed, and grain size is nanoscale.Fig. 2 is the XRD figure of above-mentioned obtained FePt nano particle, therefrom can find out that this FePt is FCT structure, i.e. face-centered tetragonal structure.Fig. 3 is the room temperature hysteresis curve of above-mentioned obtained FePt nano particle, therefrom can find out that it has the coercivity of 5400Oe, is all the coercivity provided by the FePt of FCT (i.e. face-centered tetragonal, chemistry and magnetic ordering structure).
Embodiment 2:
(1) get 1molNaCl, in vacuum drying chamber after drying, add 25ml normal heptane and put into planetary ball mill ball milling together 2 days, obtain the NaCl powder of particle size below 20 microns;
(2) together with the NaCl powder acetylacetone,2,4-pentanedione platinum of the ferric acetyl acetonade of 1mmol and 0.5mmol and step (1) obtained, ball milling 10h mixes;
(3) put into Noah's ark after mixed-powder taking-up being dried, be then placed in tubular annealing stove and calcine, tubular annealing stove first with Ar gas deaeration, passes into Ar and H during heating
2mist, Ar and H
2percent by volume be 95:5, mixed gas flow is 10ml-400ml/min, control programming rate be 10 DEG C/min, after being warming up to 650 DEG C be incubated 1 hour, insulation terminate after under atmosphere protection, be cooled to room temperature, obtain calcined product;
(4) add in calcined product by deionized water, to dissolve NaCl wherein, then put into centrifuge separation and wash away NaCl, obtain FePt nano particle.
Fig. 4 is the TEM figure of above-mentioned obtained FePt nano particle, therefrom can find out that this particle is dispersed, and grain size is nanoscale.Fig. 5 is the XRD figure of above-mentioned obtained FePt nano particle, therefrom can find out that this FePt is FCT structure, i.e. face-centered tetragonal structure.Fig. 6 is the room temperature hysteresis curve of above-mentioned obtained FePt nano particle, therefrom can find out that it has the coercivity of 5000Oe, is all the coercivity provided by the FePt of FCT (i.e. face-centered tetragonal, chemistry and magnetic ordering structure).
Above-described embodiment has been described in detail technical scheme of the present invention and beneficial effect; be understood that and the foregoing is only specific embodiments of the invention; be not limited to the present invention; all any amendments and improvement etc. made in spirit of the present invention, all should be included within protection scope of the present invention.
Claims (10)
1. the method for a preparative chemistry and magnetic order phase nano particle, it is characterized in that: using the mixture of one or more in NaCl, KCl as dispersant, by metal precursor powder and dispersant powder Homogeneous phase mixing, the mole of described dispersant powder is greater than the mole of metal precursor powder; Then, mix powder is carried out high-temperature calcination, to remove all the other elements in metal precursor except metallic element, and control calcining heat and to coordinate phase temperature higher than magnetic order, make metallic element be that carrier carries out grain growth with dispersant; Finally, be cooled to room temperature, be dissolved in by calcined product in deionized water, centrifugal segregation dispersant, obtains magnetic nanoparticle.
2. the method for preparative chemistry as claimed in claim 1 and magnetic order phase nano particle, is characterized in that: described metallic element is any one or two or more complex elements in Fe, Co, Ni, Mn, Pt.
3. the method for preparative chemistry as claimed in claim 1 and magnetic order phase nano particle, is characterized in that: described metal precursor is the salt of this metallic element, acid.
4. the method for preparative chemistry as claimed in claim 1 and magnetic order phase nano particle, is characterized in that: described metal precursor is one or both the mixture in the acetylacetonate of corresponding metal, carbonyls.
5. the method for preparative chemistry as claimed in claim 1 and magnetic order phase nano particle, it is characterized in that: when described metallic element is Pt, described metal precursor is one or both the mixture in acetylacetone,2,4-pentanedione platinum, chloroplatinic acid; When described metallic element is Fe, described metal precursor is one or both the mixture in ferric acetyl acetonade, carbonyl iron.
6. the method for preparative chemistry as claimed in claim 1 and magnetic order phase nano particle, is characterized in that: described dispersant powder and the mixed method of metal salt powder are one or more in ball milling, mechanical mixture, grinding.
7. the method for preparative chemistry as claimed in claim 1 and magnetic order phase nano particle, is characterized in that: the particle diameter of described dispersant powder is 1-20 micron; The particle diameter of metal precursor powder is 1-30 micron.
8. the method for the preparative chemistry as described in claim arbitrary in claim 1 to 7 and magnetic order phase nano particle, is characterized in that: the mole of described dispersant powder and the mole ratio of metal precursor powder are 10-1000.
9. the method for the preparative chemistry as described in claim arbitrary in claim 1 to 7 and magnetic order phase nano particle, is characterized in that: the mole of described dispersant powder and the mole ratio of metal precursor powder are 100-500.
10. the method for the preparative chemistry as described in claim arbitrary in claim 1 to 7 and magnetic order phase nano particle, is characterized in that: after temperature rises to calcining heat, carry out isothermal holding, and temperature retention time is 0.5-4h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109604628A (en) * | 2019-02-01 | 2019-04-12 | 东南大学 | A kind of preparation method of ordered phase nanometer Fe-Pt particle and cobalt platinum nano particle |
| CN110202166A (en) * | 2019-06-24 | 2019-09-06 | 东北大学 | The chemical method of liquid phase assisted Solid-state sintering synthesis fct-FePt nanoparticle |
| CN115064718A (en) * | 2022-06-03 | 2022-09-16 | 北京亿华通科技股份有限公司 | Small-particle-size PtFe structure ordered fuel cell catalyst and preparation method and application thereof |
| CN115446304A (en) * | 2022-10-27 | 2022-12-09 | 辽宁工程技术大学 | Superfine Pt-based alloy nano particle and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050274225A1 (en) * | 2001-11-02 | 2005-12-15 | The Trustees Of Princeton University | Methods for the preparation of metallic alloy nanoparticles and compositions thereof |
| CN1947901A (en) * | 2006-11-24 | 2007-04-18 | 金川集团有限公司 | Method for producing nano-iron powder |
| CN101954480A (en) * | 2010-11-08 | 2011-01-26 | 华东理工大学 | Method for preparing carbon-coated core-shell nanoparticles continuously |
| CN102218543A (en) * | 2011-05-20 | 2011-10-19 | 湖北大学 | Method for one-step synthesis of FePt nanoparticles with an fct (face centered tetragonal) structure and product thereof |
| CN102744419A (en) * | 2012-06-20 | 2012-10-24 | 中国科学院宁波材料技术与工程研究所 | Morphology control method of magnetic nanometer particles |
-
2014
- 2014-08-29 CN CN201410437402.8A patent/CN105436510A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050274225A1 (en) * | 2001-11-02 | 2005-12-15 | The Trustees Of Princeton University | Methods for the preparation of metallic alloy nanoparticles and compositions thereof |
| CN1947901A (en) * | 2006-11-24 | 2007-04-18 | 金川集团有限公司 | Method for producing nano-iron powder |
| CN101954480A (en) * | 2010-11-08 | 2011-01-26 | 华东理工大学 | Method for preparing carbon-coated core-shell nanoparticles continuously |
| CN102218543A (en) * | 2011-05-20 | 2011-10-19 | 湖北大学 | Method for one-step synthesis of FePt nanoparticles with an fct (face centered tetragonal) structure and product thereof |
| CN102744419A (en) * | 2012-06-20 | 2012-10-24 | 中国科学院宁波材料技术与工程研究所 | Morphology control method of magnetic nanometer particles |
Non-Patent Citations (1)
| Title |
|---|
| HE C N等: "One-step solid-phase synthesis of ultrasmall homogeneous face-centered tetragonal FePt nanoparticles encapsulated in thin carbon shells", 《JOURNAL OF MATERIALS CHEMISTRY》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109604628A (en) * | 2019-02-01 | 2019-04-12 | 东南大学 | A kind of preparation method of ordered phase nanometer Fe-Pt particle and cobalt platinum nano particle |
| CN109604628B (en) * | 2019-02-01 | 2021-12-24 | 东南大学 | Preparation method of ordered phase iron platinum nano-particles and cobalt platinum nano-particles |
| CN110202166A (en) * | 2019-06-24 | 2019-09-06 | 东北大学 | The chemical method of liquid phase assisted Solid-state sintering synthesis fct-FePt nanoparticle |
| CN115064718A (en) * | 2022-06-03 | 2022-09-16 | 北京亿华通科技股份有限公司 | Small-particle-size PtFe structure ordered fuel cell catalyst and preparation method and application thereof |
| CN115446304A (en) * | 2022-10-27 | 2022-12-09 | 辽宁工程技术大学 | Superfine Pt-based alloy nano particle and preparation method thereof |
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