CN102593476A - Nano-porous PtSi material and preparation method thereof - Google Patents

Nano-porous PtSi material and preparation method thereof Download PDF

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CN102593476A
CN102593476A CN2012100677484A CN201210067748A CN102593476A CN 102593476 A CN102593476 A CN 102593476A CN 2012100677484 A CN2012100677484 A CN 2012100677484A CN 201210067748 A CN201210067748 A CN 201210067748A CN 102593476 A CN102593476 A CN 102593476A
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ptsi
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electrode
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CN102593476B (en
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余金山
周新贵
张长瑞
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National University of Defense Technology
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Abstract

The invention discloses a nano-porous PtSi material and a preparation method thereof. The nano-porous PtSi material mainly comprises a PtSi compound, wherein three-dimensional connected nano pores are uniformly distributed in the nano-porous PtSi material. The preparation method of the nano-porous PtSi material includes the following steps: feeding a platinum sheet and silicon powder in an inert gas atmosphere and heating and melting; maintaining the temperature for 30-60 minutes until a melt is uniform, then cooling the melt to room temperature and obtaining a PtmSi100-m master alloy, wherein m is 10-40; re-melting the PtmSi100-m master alloy; preparing a PtmSi100-m master alloy strip by adopting a single-roller strip-casting method, wherein the rotating speed of the roller is 300-6000r/min; and with the PtmSi100-m master alloy strip as a work electrode, establishing an electromechanical work station by adopting a tri-electrode method, and dissolving a Si matrix by adopting an anodic oxidation method to obtain the nano-porous PtSi material. The nano-porous PtSi material can be used as an anode catalyst of a methanol fuel cell and has the advantages of simple process, short period, low cost, favorable effect and the like.

Description

Nanoporous PtSi material and preparation method thereof
Technical field
The present invention relates to the porous nanometer material field, relate in particular to a kind of nanoporous PtSi material.
Background technology
DMFC (Direct Methanol Fuel Cell; DMFC) be a kind of of Proton Exchange Membrane Fuel Cells; It is directly methyl alcohol to be injected into to carry out the electro-catalysis generating in the fuel cell; And need not pass through any fuel reformation modifying apparatus earlier, so DMFC does not exist preparation, storage, transportation and the security problems of hydrogen; And have simple in structurely, easy to operate, store easy to carry; Fuel source is abundant, and methyl alcohol uses the back pollution-free, advantages such as clean environment firendly; Thereby great competitive advantage is arranged in fields such as small-sized civilian power supplys such as notebook computer and compact powers, have broad application prospects.
In the DMFC course of work, the electrocatalysis of catalyst is very crucial on anode and the negative electrode.Early stage fuel cell is owing to using the metal platinum of a large amount of costlinesses to make catalyst, so development is very slow.Development along with nanometer technology; The Pt nanoparticle of supported or the compound nano-particle of platinum are widely used as eelctro-catalyst; This catalyst decentralization and the more early stage catalyst of specific area improve greatly; Thereby feasible fuel cell has in recent years attracted a large amount of researchers' interest, and development rapidly.
At present, the anode catalyst of the DMFC of commercial application is to do with Pt nanoparticle (Pt/C) or platinum rhodium nano particle (Pt-Ru/C) that active carbon particle is done carrier.Because platinum, rhodium are noble metal, cost an arm and a leg and resource-constrained, must adopt effective measures to reduce the consumption of platinum; In addition because the unsteadiness of simple substance nano metal itself, be prone to reunion in the course of work and reduce activity of such catalysts and specific area significantly, thereby catalyst was lost efficacy gradually.On the other hand, simple metal platinum has very strong suction-operated to Methanol Decomposition intermediate CO, has adsorbed the platinum meeting " poisoning " of CO and loses electrocatalysis.Therefore, how to reduce the consumption of platinum, improve catalyst chemical stability; Prevent platinosis; Seek the anodised eelctro-catalyst of methyl alcohol of high efficiency, low cost, improve the anodised speed of methyl alcohol, the loss that reduces anode catalyst is one of important directions of DMFC application study.
Nano-porous materials is a kind of nano material with three-dimensional communication nano-pore structure.This nano material has very big specific area and surface activity, and its exclusive three-dimensional connected porous structure allows liquid phase medium to flow freely therein, is suitable for very much the electrochemical catalyst of fuel cell.But the simple substance nanoporous noble metal galvanic anode catalyst that acts as a fuel also faces the electrochemical stability problem, promptly in use owing to nano material huge surface area and high surface are reunited.
Summary of the invention
Technical problem to be solved by this invention is: to the problem that prior art exists, the present invention provides that a kind of electrochemical stability is good, nanoporous PtSi material with three-dimensional connected porous structure and preparation method thereof.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of nanoporous PtSi material, said nanoporous PtSi material mainly comprises the PtSi compound, (wherein the element of PtSi compound is formed and to be generally Pt to be evenly equipped with the nanoaperture of three-dimensional communication in the said nanoporous PtSi material mSi 100-m, m is 10～40).
The aperture of nanoaperture is preferably 50 nm～2000 nm in the above-mentioned nanoporous PtSi material.
Above-mentioned nanoporous PtSi material profile preferably is laminar.
As a total technical conceive, the present invention also provides a kind of above-mentioned nanoporous PtSi preparation methods, may further comprise the steps:
(1) melting Pt mSi 100-mFoundry alloy: platinized platinum (being preferably 4N) and silica flour (be preferably the polycrystalline silica flour, be preferably 4N, 200 orders) are placed heating and melting under inert gas (the being preferably high-purity argon gas) atmosphere, be incubated 30～60 minutes to melt evenly after, cool to room temperature makes Pt mSi 100-mFoundry alloy; Wherein, m is 10～40;
(2) get rid of band method (melting-spinning) preparation Pt mSi 100-mFoundry alloy band: with said Pt mSi 100-mThe foundry alloy refuse is adopted single roller to get rid of the band legal system and is equipped with Pt mSi 100-mFoundry alloy band, roller rotating speed are 2000 r/min～6000 r/min;
(3) electrochemical method selective dissolution Si matrix: with the Pt that makes mSi 100-mThe foundry alloy band is a work electrode, adopts three-electrode method to set up electrochemical workstation, adopts anode oxidation method with said Pt mSi 100-mThe dissolving of Si matrix obtains said nanoporous PtSi material in the foundry alloy band.
Among the above-mentioned preparation method, said electrochemical workstation is an electrolyte with hydrofluoric acid (preferred 0.1ml/L) preferably, is to electrode with platinum black electrode, is reference electrode with silver electrode/silver chloride electrode.Before setting up behind the said electrochemical workstation and adopting said anode oxidation method dissolving Si, preferably earlier adopt cyclic voltammetry to confirm anodised current potential, on said work electrode, load the voltage that forms this current potential then with said Si matrix dissolving.
Among the above-mentioned preparation method, the voltage of said loading is preferably 0.5v～0.8v, and the dissolving duration is preferably 500s～2000s.
Among the above-mentioned preparation method, the Pt that said step (2) makes mSi 100-mThe foundry alloy beam thickness is preferably 10 μ m～50 μ m, width 1 mm～2mm.
Among the above-mentioned preparation method, said Pt mSi 100-mM in the foundry alloy preferably gets 30.
Compared with prior art, the invention has the advantages that:
1, nanoporous PtSi material of the present invention is the nano material with three-dimensional connected porous structure, and it is mobile in hole that it helps medium, can improve the catalytic efficiency of material.This material is made up of the PtSi compound; Stability Analysis of Structures also can effectively lower the consumption of Pt; Have than the better electrochemical stability of simple substance Pt nanoparticle catalyst, and PtSi has the better catalytic action of methyl alcohol than simple substance Pt, can be used as methanol fuel cell anode catalyzer; Need not supported, electrochemical catalysis is active high.Owing to the existence of Si in the material, effectively reduced the consumption of precious metals pt, reduced material cost.
2, nanoporous PtSi preparation methods of the present invention makes the compound of separating out 3-D nano, structure in the alloy through rapid solidification, dissolves away matrix with chemistry or electrochemical method, obtains need not the nano-porous materials of supported.Its technical process is simple, and equipment requirements is low, and used process equipment mainly contains vacuum melting furnace, gets rid of carrying device, electrochemical workstation and electrolysis tank etc., and its process route is simple, and process cycle is short, and environmentally safe and technology versatility are good in the preparation process.
Description of drawings
Fig. 1 is the Pt that gets rid of the preparation of band method in the embodiment of the invention 1 30Si 70The X-ray diffraction of foundry alloy band (XRD) collection of illustrative plates.
Fig. 2 is Pt in the embodiment of the invention 1 30Si 70The ESEM microphoto of foundry alloy band.
Fig. 3 is the ESEM microphoto of the nanoporous PtSi material that makes in the embodiment of the invention 1.
Fig. 4 is Pt in the embodiment of the invention 2 30Si 70The ESEM microphoto of foundry alloy band.
Fig. 5 is the ESEM microphoto of the nanoporous PtSi material that makes in the embodiment of the invention 2.
Fig. 6 is the Pt for preparing in the Comparative Examples of the present invention 30Si 70The ESEM microphoto of foundry alloy band.
Fig. 7 be in the embodiment of the invention 2 nanoporous PtSi material and commercial Pt nanoparticle catalyst to methyl alcohol catalytic action correlation curve sketch map.
Fig. 8 is the volt-ampere curve correlation curve sketch map after the volt-ampere circulation for the first time of nanoporous PtSi material circulates with 500 volt-ampere in the embodiment of the invention 2.
Fig. 9 is the volt-ampere curve correlation curve sketch map after the volt-ampere circulation for the first time of commercial Pt nanoparticle catalyst circulates with 500 volt-ampere in the embodiment of the invention 2.
Embodiment
Below will combine Figure of description and specific embodiment that the present invention is explained further details.
Embodiment 1:
A kind of nanoporous PtSi material of the present invention mainly comprises the PtSi compound, and it is laminar that outward appearance is.Be evenly equipped with the nanoaperture of three-dimensional communication in the nanoporous PtSi material, the aperture is that (wherein the element of PtSi compound composition is generally Pt to 800 nm～2000 nm 30Si 70).
The nanoporous PtSi material of present embodiment mainly prepares through following steps:
(1) melting Pt 30Si 70Foundry alloy:
High-purity platinized platinum (99.98%) and polycrystalline silica flour (99.998%), ethanol are placed in the crucible after cleaning; Under high-purity argon gas atmosphere, place induction heating vacuum furnace heating and melting, be incubated 30 minutes to melt evenly after; Cool to room temperature under high-purity argon gas atmosphere makes Pt 30Si 70Foundry alloy.
(2) get rid of the band legal system and be equipped with Pt 30Si 70The foundry alloy band:
With Pt 30Si 70Foundry alloy melts under high-purity argon gas atmosphere again, adopts single roller to get rid of the band legal system and is equipped with Pt 30Si 70Foundry alloy band, roller rotating speed are 4000 r/min; The Pt that makes 30Si 70The foundry alloy beam thickness is 20 μ m, width 1 mm～2mm.This Pt 30Si 70The ESEM microphoto of foundry alloy band is as shown in Figure 2, and visible by Fig. 2, its structure is a distributed network shape PtSi precipitate in the black Si matrix; Its X-ray diffraction (XRD) collection of illustrative plates is as shown in Figure 1, visible Pt 30Si 70It is PtSi compound and Si matrix mutually that the foundry alloy band is formed.
(3) electrochemical method selective dissolution Si matrix:
With 0.1ml/L hydrofluoric acid is electrolyte, and platinum black electrode is to electrode, and silver electrode or silver chloride electrode are reference electrode, Pt 30Si 70The foundry alloy band is a work electrode, sets up electrochemical workstation.Adopt cyclic voltammetry to confirm that the anodised current potential of Si is 0.7v, the voltage that on the foundry alloy band, loads 0.7v then is with Pt 30Si 70Si matrix dissolving in the foundry alloy band, dissolution time obtains nanoporous PtSi material for being about 1000s.
The ESEM microphoto of the above-mentioned nanoporous PtSi material that obtains is as shown in Figure 3, and visible Si matrix is removed fully, obtains porous PtSi material, and its composition is the PtSi compound, and the aperture is 800 nm～2000 nm.
Embodiment 2:
A kind of nanoporous PtSi material of the present invention, it mainly comprises the PtSi compound, it is laminar that outward appearance is.Be evenly equipped with the nanoaperture of three-dimensional communication in the nanoporous PtSi material, the aperture is 80 nm～200 nm.
Nanoporous PtSi material of the present invention mainly prepares through following steps:
(1) melting Pt 30Si 70Foundry alloy:
High-purity platinized platinum (99.98%) and polycrystalline silica flour (99.998%), ethanol are placed in the crucible after cleaning; Under high-purity argon gas atmosphere, place induction heating vacuum furnace heating and melting, be incubated 30 minutes to melt evenly after; Cool to room temperature under high-purity argon gas atmosphere makes Pt 30Si 70Foundry alloy.
(2) get rid of the band legal system and be equipped with Pt 30Si 70The foundry alloy band:
With Pt 30Si 70Foundry alloy melts under high-purity argon gas atmosphere again, adopts single roller to get rid of the band legal system and is equipped with Pt 30Si 70The foundry alloy band, the roller rotating speed is 6000 r/min, the Pt that makes 30Si 70The foundry alloy beam thickness is 20 μ m, width 1 mm～2mm.This Pt 30Si 70The ESEM microphoto of foundry alloy band is as shown in Figure 4, and visible by Fig. 4, the foundry alloy structure is a distributed network shape PtSi precipitate in the black Si matrix, and precipitate is evenly tiny.
(3) electrochemical method selective dissolution Si matrix:
With 0.1ml/L hydrofluoric acid is electrolyte, and platinum black electrode is to electrode, and silver electrode or silver chloride electrode are reference electrode, Pt 30Si 70The foundry alloy band is a work electrode, sets up electrochemical workstation.Adopt cyclic voltammetry to confirm that the anodised current potential of Si is 0.7v, the voltage that on the foundry alloy band, loads 0.7v then is with Pt 30Si 70Si matrix dissolving in the foundry alloy band, dissolution time is about 1000s, obtains nanoporous PtSi material.
The ESEM microphoto of the above-mentioned nanoporous PtSi material that obtains is as shown in Figure 5, and visible Si matrix dissolves fully, obtains porous PtSi material, and its composition is the PtSi compound, and the aperture is 80 nm～200 nm.
Above-mentioned nanoporous PtSi material that obtains and existing commercial Pt nanoparticle catalyst are carried out methyl alcohol catalytic action contrast test, and the gained result is as shown in Figure 7.Can find out that nanoporous PtSi material is lower to methyl alcohol anodic oxidation current potential, explain that nanoporous PtSi material of the present invention has than commercial Pt nanoparticle catalyst the better electrocatalysis of methyl alcohol.
Above-mentioned nanoporous PtSi material that obtains and existing commercial Pt nanoparticle catalyst (Pt/C catalyst) are carried out the electrochemical stability contrast test; Experiment is an electrolyte with 1mol/L sulfuric acid; Volt-ampere curve after circulating with volt-ampere circulation for the first time and 500 volt-ampere is to the electrochemical stability of assessment material recently, gained result such as Fig. 8, shown in Figure 9.Fig. 8 is above-mentioned porous PtSi material volt-ampere first time circulation that obtains and the volt-ampere curve contrast after 500 volt-ampere circulations; Fig. 9 is the volt-ampere curve contrast after the volt-ampere circulation for the first time of commercial Pt nanoparticle catalyst and 500 the volt-ampere circulations.Visible by figure, porous PtSi compound obviously has than the much higher electrochemical stability of commercial Pt nanoparticle catalyst.Be furnished with the nanoporous PtSi material of the nanoaperture of three-dimensional communication, its composition is the PtSi compound.
Comparative Examples:
A kind of Comparative Examples of the present invention, carry out following steps successively:
(1) melting Pt 30Si 70Foundry alloy: step is identical with embodiment 1.
(2) get rid of the band legal system and be equipped with Pt 30Si 70The foundry alloy band:
With Pt 30Si 70Foundry alloy melts under high-purity argon gas atmosphere again, adopts single roller to get rid of the band legal system and is equipped with Pt 30Si 70Foundry alloy band, roller rotating speed are 2000 r/min; The Pt that makes 30Si 70The foundry alloy beam thickness is 20 μ m, width 1 mm～2mm.
The above-mentioned Pt that obtains 30Si 70The ESEM microphoto of foundry alloy band is as shown in Figure 6, and is visible by Fig. 6, and visible low owing to getting rid of tape speed by Fig. 6, alloy liquid setting rate is slow, and the PtSi compound of separating out is very thick, does not also form three-dimensional connected porous tissue.Therefore, can not be used to prepare nanoporous PtSi material of the present invention.
In sum, nanoporous PtSi material preparation process process of the present invention is simple, and equipment requirements is low, and is simple, and process cycle is short, environmentally safe in the preparation process.PtSi material of the present invention is made up of the PtSi compound, has than the better electrochemical stability of simple substance Pt nanoparticle catalyst; And PtSi has the better catalytic action of methyl alcohol than simple substance Pt; As methanol fuel cell anode catalyzer, need not supported, electrochemical catalysis is active high.Simultaneously, the present invention can also study the porous silicon compound for preparing other noble metals to those skilled in the art research direction and enlightenment are provided.
Below only be preferred implementation of the present invention, protection scope of the present invention also not only is confined to the foregoing description, and the various process programs of conceiving no substantial differences with the present invention are all in protection scope of the present invention.

Claims (9)

1. a nanoporous PtSi material is characterized in that, said nanoporous PtSi material mainly comprises the PtSi compound, is evenly equipped with the nanoaperture of three-dimensional communication in the said nanoporous PtSi material.
2. nanoporous PtSi material according to claim 1 is characterized in that, the aperture of said nanoaperture is 50 nm～2000 nm.
3. nanoporous PtSi material according to claim 1 and 2 is characterized in that, said nanoporous PtSi material profile is laminar.
4. nanoporous PtSi preparation methods may further comprise the steps:
(1) melting Pt mSi 100-mFoundry alloy: platinized platinum and silica flour are placed heating and melting under the inert gas atmosphere, be incubated 30 minutes～60 minutes to melt evenly after, cool to room temperature makes Pt mSi 100-mFoundry alloy; Wherein, m is 10～40;
(2) preparation Pt mSi 100-mFoundry alloy band: with said Pt mSi 100-mThe foundry alloy refuse is adopted single roller to get rid of the band legal system and is equipped with Pt mSi 100-mFoundry alloy band, roller rotating speed are 3000 r/min～6000 r/min;
(3) selective dissolution Si matrix: with the Pt that makes mSi 100-mThe foundry alloy band is a work electrode, adopts three-electrode method to set up electrochemical workstation, adopts anode oxidation method with said Pt mSi 100-mThe dissolving of Si matrix obtains said nanoporous PtSi material in the foundry alloy band.
5. nanoporous PtSi preparation methods according to claim 4 is characterized in that, said electrochemical workstation is to be electrolyte with hydrofluoric acid, is to electrode with platinum black electrode, is reference electrode with silver electrode/silver chloride electrode.
6. nanoporous PtSi preparation methods according to claim 5; It is characterized in that; Before setting up behind the said electrochemical workstation and adopting said anode oxidation method dissolving Si; Adopt cyclic voltammetry to confirm anodised current potential earlier, the voltage that on said work electrode, loads this current potential of formation then is to dissolve said Si matrix.
7. nanoporous PtSi preparation methods according to claim 6 is characterized in that the voltage of said loading is 0.5v～0.8v, and the dissolving duration is 500s～2000s.
8. according to each described nanoporous PtSi preparation methods in the claim 4～7, it is characterized in that the Pt that said step (2) makes mSi 100-mThe foundry alloy beam thickness is 10 μ m～50 μ m, width 1 mm～2mm.
9. according to each described nanoporous PtSi preparation methods in the claim 4～7, it is characterized in that said Pt mSi 100-mM in the foundry alloy gets 30.
CN201210067748.4A 2012-03-15 2012-03-15 Nano-porous PtSi material and preparation method thereof Expired - Fee Related CN102593476B (en)

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Cited By (3)

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CN104525218A (en) * 2014-12-12 2015-04-22 江苏大学 Preparation method of efficient Pt-CoSi2/graphene composite electric catalyst
CN110724995A (en) * 2019-11-14 2020-01-24 中国科学院理化技术研究所 Method for improving photoelectric conversion efficiency of water decomposed by p-Si/PtSi photocathode
CN111509236A (en) * 2019-01-31 2020-08-07 华中科技大学 One-dimensional porous platinum-containing alloy nanowire catalyst and preparation method thereof

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CN110724995A (en) * 2019-11-14 2020-01-24 中国科学院理化技术研究所 Method for improving photoelectric conversion efficiency of water decomposed by p-Si/PtSi photocathode

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