CN102728389B - Preparation method for FePt/graphene composite nano-material - Google Patents
Preparation method for FePt/graphene composite nano-material Download PDFInfo
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- CN102728389B CN102728389B CN201210220459.3A CN201210220459A CN102728389B CN 102728389 B CN102728389 B CN 102728389B CN 201210220459 A CN201210220459 A CN 201210220459A CN 102728389 B CN102728389 B CN 102728389B
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Abstract
The invention provides a preparation method for a FePt/graphene composite nano-material. The method comprises the following steps: dispersing graphite oxide in glycol and carrying out ultrasonic treatment so as to obtain solution A; dissolving ferric acetylacetonate in the solution A under stirring and carrying out ultrasonic treatment so as to obtain solution B; dissolving platinum acetylacetonate in glycol under stirring so as to obtain solution C; adding the solution C into the solution B drop by drop and carrying out ultrasonic treatment so as to obtain solution D, adding 1,2-hexadecanediol into the solution D, wherein a mol ratio of 1,2-hexadecanediol to ferric acetylacetone or platinum acetylacetonate is 3:1, blowing in nitrogen and carrying out a reflux reaction at a temperature of 197 DEG C for 3 hours; and centrifuging, rinsing and drying an obtained product so as to obtain the FePt/graphene composite nano-material. According to the invention, the FePt/graphene composite nano-material is synthesized in one step by using the method of coreduction of ferric acetylacetonate, platinum acetylacetonate and graphite oxide in a glycol solution, usage of surfactant is avoided, and the purity of the material is improved; and the one-step synthesis method is simple, is easy to operate and has a good development prospect.
Description
Technical field
The invention belongs to the preparing technical field of nano material, be specifically related to a kind of preparation method of FePt/ Graphene composite nano materials.
Background technology
Along with the day by day exhaustion of global energy resource and the sharply deterioration of environmental pollution, the environmental protection new forms of energy beyond exploitation fossil energy have become the important topic of science and industrial research.The advantages such as fuel cell is efficient because having, environmental protection, fuel source are wide, become the focus of new forms of energy research.
Precious metals pt, because have good catalytic performance, is most important catalyst in Proton Exchange Membrane Fuel Cells.But because it is expensive, its application and popularization have greatly been limited.Research shows, introduces to have paramagnetic transition metal and can not only reduce costs, and contribute to improve its catalytic performance in Pt.Superparamagnetic FePt nano particle has extraordinary application prospect in fuel cell.Meanwhile, Graphene has excellent electricity and heat-conductive characteristic and high mechanical strength, and cheap, becomes the desirable carrier of FePt catalyst.
At present, the method of synthetic FePt nano particle all needs to add surfactant substantially, as conventional oleic oil ammonia etc., but because FePt has certain solubility in surfactant, this impact of purity for FePt is very large, and then directly has influence on the catalytic efficiency of fuel cell.In addition, existing method is two steps or multistep synthetic method, and process is more loaded down with trivial details.
Summary of the invention
The technical problem to be solved in the present invention is: the preparation method that a kind of simple to operate and FePt/ Graphene composite nano materials that product purity is higher is provided.
For realizing the object of the invention, the technical solution used in the present invention is:
A preparation method for FePt/ Graphene composite nano materials, is characterized in that it comprises the following steps:
(1) graphite oxide is scattered in ethylene glycol, ultrasonic, obtain solution A;
(2) ferric acetyl acetonade is added to stirring and dissolving in solution A, ultrasonic, obtain solution B;
(3) acetylacetone,2,4-pentanedione platinum is dissolved in ethylene glycol, stirs it is dissolved, obtain solution C;
(4) solution C is added drop-wise in solution B, ultrasonic, obtain solution D, in described solution D, the concentration of graphite oxide is 0.5g/L, in solution D, the mol ratio of ferric acetyl acetonade and acetylacetone,2,4-pentanedione platinum is 1:1, and in solution D, the concentration of ferric acetyl acetonade or acetylacetone,2,4-pentanedione platinum is 2.5 mM/ls, 0.5 mM/l or 0.25 mM/l;
(5) 1,2-hexadecane glycol is added in solution D, the mol ratio of 1,2-hexadecane glycol and ferric acetyl acetonade or acetylacetone,2,4-pentanedione platinum was 3:1, passes into nitrogen, 197 ℃ of back flow reaction 3 hours;
(6) by products therefrom centrifuge washing, dry, obtain described FePt/ Graphene composite nano materials.
In such scheme, the ultrasonic time in described step 1) is 3.5 hours.
In such scheme, described step 2) ultrasonic time in is 0.5 hour.
In such scheme, the ultrasonic time in described step 4) is 0.5 hour.
In such scheme, adopt water and ethanol to replace centrifuge washing in described step 6), then 60 ℃ of vacuum drying are 6 hours.
The invention has the beneficial effects as follows:
1. the present invention adopts ferric acetyl acetonade, the method for acetylacetone,2,4-pentanedione platinum and graphite oxide coreduction in ethylene glycol solution, one-step synthesis FePt/ grapheme material, removed surfactant from, improved the purity of material.And one-step method for synthesizing is simple, easy operating, is applicable to large-scale industrialization and produces, and can greatly promote superparamagnetic FePt nano particle in the application of fuel cell field, has good development prospect.
2. in simple reaction system, by adjusting the consumption of reactant, realized at an easy rate the controlledly synthesis of different composition FePt/ Graphene composite nano materials, product pattern is single.
Accompanying drawing explanation
Fig. 1 is the field transmission electromicroscopic photograph that embodiment 1 obtains product.
Fig. 2 is the Raman collection of illustrative plates that embodiment 1 obtains product.
Fig. 3 is the XRD collection of illustrative plates that embodiment 1 obtains product.
Fig. 4 is the field transmission electromicroscopic photograph that embodiment 2 obtains product.
Fig. 5 is the XRD collection of illustrative plates that embodiment 2 obtains product.
Fig. 6 is the field transmission electromicroscopic photograph that embodiment 3 obtains product.
Fig. 7 is the XRD collection of illustrative plates that embodiment 3 obtains product.
The specific embodiment
Below in conjunction with drawings and Examples, the invention will be further described, and certain following embodiment should not be construed as limitation of the present invention.
embodiment 1:
1) graphite oxide 100 mg are added in 100 mL ethylene glycol, ultrasonic dispersion 3.5 hours, obtains solution A;
2) ferric acetyl acetonade of 0.5mmol (is abbreviated as to Fe (acac) below
3) add stirring and dissolving in solution A, more ultrasonic 0.5 hour, solution B obtained;
3) the acetylacetone,2,4-pentanedione platinum of 0.5 mmol (is abbreviated as to Pt (acac) below
2) add in 100 mL ethylene glycol, stir it is dissolved, obtain solution C;
4) solution C is slowly added drop-wise in solution B, ultrasonic 0.5 hour, obtain solution D, in described solution D, the concentration of graphite oxide is 0.5g/L, in solution D, the concentration of ferric acetyl acetonade and acetylacetone,2,4-pentanedione platinum is 2.5 mM/ls;
5) by 1 of 1.5 mmol, 2-hexadecane glycol adds solution D, stirs and to make it to dissolve and pass into nitrogen, in 197 ℃ of back flow reaction 3 hours; Products therefrom water and ethanol replace centrifuge washing, and then 60 ℃ of vacuum drying are 6 hours, obtain described FePt/ Graphene composite nano materials.
Fig. 1 is the transmission electron microscope photo of products therefrom, shows that nano particle is successfully carried on Graphene.Fig. 2 shows that by Raman collection of illustrative plates products therefrom is Graphene.Fig. 3 is the XRD collection of illustrative plates of products therefrom, proves that products therefrom is FePt/ Graphene composite nano materials.Table 1 is the ICP data of products therefrom, and the mol ratio of proved response product Fe:Pt is 2:3.
Table 1
| Composition | Fe | Pt |
| Concentration | 6.709 wt% | 38.04 wt% |
embodiment 2:
1) graphite oxide 100 mg are added in 100 mL ethylene glycol, ultrasonic dispersion 3.5 hours, obtains solution A;
2) by the Fe of 0.1 mmol (acac)
3add stirring and dissolving in solution A, more ultrasonic 0.5 hour, solution B obtained;
3) by the Pt of 0.1 mmol (acac)
2add in 100 mL ethylene glycol, stir it is dissolved, obtain solution C;
4) solution C is slowly added drop-wise in solution B, ultrasonic 0.5 hour, obtain solution D, in described solution D, the concentration of graphite oxide is 0.5g/L, in solution D, the concentration of ferric acetyl acetonade and acetylacetone,2,4-pentanedione platinum is 0.5 mM/l; ;
5) by 1 of 0.3 mmol, 2-hexadecane glycol adds solution D, stirs and to make it to dissolve and pass into nitrogen, in 197 ℃ of back flow reaction 3 hours; Products therefrom water and ethanol replace centrifuge washing, and then 60 ℃ of vacuum drying are 6 hours, obtain described FePt/ Graphene composite nano materials.
Fig. 4 is the transmission electron microscope photo of products therefrom, shows that nano particle is successfully carried on Graphene.Fig. 5 is the XRD collection of illustrative plates of products therefrom, proves that products therefrom is FePt/ Graphene composite nano materials.Table 2 is products therefrom ICP data, and the mol ratio of proved response product Fe:Pt is 1:3.
Table 2
| Composition | Fe | Pt |
| Concentration | 2.362 wt% | 23.81 wt% |
embodiment 3:
1) graphite oxide 100 mg are added in 100 mL ethylene glycol, ultrasonic dispersion 3.5 hours, obtains solution A;
2) by the Fe of 0.05 mmol (acac)
3add stirring and dissolving in solution A, more ultrasonic 0.5 hour, solution B obtained;
3) by the Pt of 0.05 mmol (acac)
2add in 100 mL ethylene glycol, stir it is dissolved, obtain solution C; Solution C is slowly added drop-wise in solution B, ultrasonic 0.5 hour, obtain solution D, in described solution D, the concentration of graphite oxide is 0.5g/L, in solution D, the concentration of ferric acetyl acetonade and acetylacetone,2,4-pentanedione platinum is 0.25 mM/l; ;
4) by 1 of 0.15 mmol, 2-hexadecane glycol adds solution D, stirs and to make it to dissolve and pass into nitrogen, in 197 ℃ of back flow reaction 3 hours; Products therefrom water and ethanol replace centrifuge washing, and then 60 ℃ of vacuum drying are 6 hours, obtain described FePt/ Graphene composite nano materials.
Fig. 6 is the transmission electron microscope photo of products therefrom, shows that nano particle is successfully carried on Graphene.Fig. 7 is the XRD collection of illustrative plates of products therefrom, proves that products therefrom is FePt/ Graphene composite nano materials.Table 3 is products therefrom ICP data, and the mol ratio of proved response product Fe:Pt is 1:3.
Table 3
| Composition | Fe | Pt |
| Concentration | 0.981 wt% | 10.81 wt% |
Claims (5)
1. a preparation method for FePt/ Graphene composite nano materials, is characterized in that it comprises the following steps:
1) graphite oxide is scattered in ethylene glycol, ultrasonic, obtain solution A;
2) ferric acetyl acetonade is added to stirring and dissolving in solution A, ultrasonic, obtain solution B;
3) acetylacetone,2,4-pentanedione platinum is dissolved in ethylene glycol, stirs it is dissolved, obtain solution C;
4) solution C is added drop-wise in solution B, ultrasonic, obtain solution D, in described solution D, the concentration of graphite oxide is 0.5g/L, in solution D, the mol ratio of ferric acetyl acetonade and acetylacetone,2,4-pentanedione platinum is 1:1, and in solution D, the concentration of ferric acetyl acetonade or acetylacetone,2,4-pentanedione platinum is 2.5 mM/ls, 0.5 mM/l or 0.25 mM/l;
5) 1,2-hexadecane glycol is added in solution D, the mol ratio of 1,2-hexadecane glycol and ferric acetyl acetonade or acetylacetone,2,4-pentanedione platinum was 3:1, passes into nitrogen, 197 ℃ of back flow reaction 3 hours;
6) by products therefrom centrifuge washing, dry, obtain described FePt/ Graphene composite nano materials.
2. preparation method as claimed in claim 1, is characterized in that, the ultrasonic time in described step 1) is 3.5 hours.
3. preparation method as claimed in claim 1, is characterized in that, described step 2) in ultrasonic time be 0.5 hour.
4. preparation method as claimed in claim 1, is characterized in that, the ultrasonic time in described step 4) is 0.5 hour.
5. preparation method as claimed in claim 1, is characterized in that, adopts water and ethanol to replace centrifuge washing in described step 6), and then 60 ℃ of vacuum drying are 6 hours.
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| CN110676469B (en) * | 2019-08-26 | 2020-10-27 | 宁德师范学院 | Carbon-supported platinum-based nanomaterial |
| CN113813972A (en) * | 2020-06-03 | 2021-12-21 | 深圳先进技术研究院 | Composite nano material, preparation method and catalyst |
| CN113429582B (en) * | 2021-08-12 | 2023-01-10 | 福州大学 | Preparation and application of graphene oxide grafted polyether modified silicone oil |
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Non-Patent Citations (4)
| Title |
|---|
| FePt Nanoparticles Assembled on Graphene as Enhanced Catalyst for Oxygen Reduction Reaction;Shaojun Gao et al.,;《 Journal of the American Chemical Society》;20120126;第134卷;2492-2495 * |
| Formation Mechanism via a Heterocoagulation Approach of FePt Nanoparticles Using the Modified Polyol Process;Watson Beck et al.,;《the Journal of Physical Chemistry》;20110506;第115卷;10475-10482 * |
| Shaojun Gao et al.,.FePt Nanoparticles Assembled on Graphene as Enhanced Catalyst for Oxygen Reduction Reaction.《 Journal of the American Chemical Society》.2012,第134卷2492-2495. |
| Watson Beck et al.,.Formation Mechanism via a Heterocoagulation Approach of FePt Nanoparticles Using the Modified Polyol Process.《the Journal of Physical Chemistry》.2011,第115卷10475-10482. |
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