CN108767277A - A kind of Fe-Pd bases nano-porous materials and preparation method thereof - Google Patents
A kind of Fe-Pd bases nano-porous materials and preparation method thereof Download PDFInfo
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Abstract
A kind of nano-porous materials and preparation method thereof, belong to new material technology field.The catalysis material is using Fe-Pd-P non-crystaline amorphous metals as presoma alloy, under room temperature acidic environment, using the de- alloying technology of chemistry, the nano-porous materials with uniform reticular structure are prepared, the Fe-Pd bases nano-porous materials of acquisition have excellent electrocatalysis characteristic to formic acid etc..The nano-porous materials of acquisition are made into electrode material, hence it is evident that improve the electrocatalysis characteristic to formic acid.For the present invention compared with traditional metal materials, the nano-porous materials structure of preparation is uniform, and specific surface area is high, and stability is good, and occurs to being poisoned without CO during formic acid electro-catalysis;Chemistry is de-, and alloyage is at low cost, is simple and efficient, easily realizes industrialized production;The nano-porous materials of preparation are widely used in the new energy electrode material such as fuel cell field.
Description
Technical field
The invention belongs to field of new materials, more particularly to a kind of Fe-Pd base noncrystal alloys prepare nano-porous materials and its
Preparation method.
Background technology
Nano-porous materials are field of new materials research hotspots, and compared to traditional metal materials, nano porous metal material has
High-specific surface area and special surface criticality, are widely used in the fields such as fuel cell, capacitor, sensor, catalysis.
The method for preparing nano-porous materials has de- alloyage, template, sintering process, layer-by-layer etc..Wherein,
The de- alloyage of chemistry is chemical corrosion process, and in the solution, corrosion dissolution occurs for more active element in alloy, and inert element expands
Bulk weight group forms nano-porous structure.De- alloyage is at low cost, be simple and efficient, easily realizes industrialized production, therefore, takes off alloyage
Show one's talent in numerous preparation methods.
The key that de- alloyage prepares nano porous metal material is that the selection of presoma alloy, presoma will meet conjunction
The feature that golden ingredient is uniform and monophase field ingredient is wide, which has limited the multicomponent alloy system ranges that de- alloyage is applicable in.Currently, selection
Presoma alloy system be concentrated mainly on Ni bases, Cu bases, Mn bases, Mg bases, Zn bases, Al based alloys etc., to Fe based alloys, system grinds
Study carefully less.Compared to the amorphous alloy material that conventional crystal material, rapid cooling are formed, have chemical composition uniform, nodeless mesh,
The advantages such as the defects of dislocation occurs, and component adjustability is larger, and component range of choice is wider.Therefore, non-crystaline amorphous metal is to prepare
The excellent persursor material of polynary nanometer porous metals expands the applicable alloy system range of de- alloyage.
Currently, global energy and environment challenge getting worse, it is further urgent to the exploitation of new energy.It is led in fuel cell
Domain, mainly using Pt base catalysis materials, Pt is expensive and low memory, limits the development and application of fuel cell,
The research and development of cause rather than Pt base catalysis materials are very necessary.However the price of Pd is the half of Pt, and it is straight during Catalyzed by Formic Acid
It connects dehydration and generates CO2, no CO poisonings appearance;Transition-metal Fe element contains vacant electron orbit and not pairs of electronics, with
After Pd forms alloy, the electronic structure of Pd is improved, Pd can be improved to formic acid electrocatalysis characteristic;The addition of nonmetallic P can be improved
Precious metals pd is to the electro catalytic activity and stability of formic acid, in consideration of it, by Fe-Pd-P non-crystaline amorphous metals by the de- alloy treatment of chemistry
It can get efficient nano-porous materials.Research efficiently prepares the Fe-Pd base nano-porous materials with excellent electrocatalysis characteristic
The development of new energy field is of great significance to.
Invention content
The technical problem to be solved in the present invention:De- alloyage is overcome to be applicable in the limitation of alloy system and be difficult to efficiently make
The problems such as standby nano-porous materials with excellent electrocatalysis characteristic, it is more to provide a kind of Fe-Pd base noncrystal alloys preparation nanometer
The method of Porous materials.Using the de- alloyage of chemistry, using principle of oxidation and reduction, Fe elements are rotten in Fe-Pd-P non-crystaline amorphous metals
Erosion dissolving, the recombination of Pd elements diffusions, form the nano-porous materials with three-dimensional uniformly reticular structure, and have studied Fe-Pd bases
Electrocatalysis characteristic of the nano-porous materials in formic acid solution provides new method and think of for the electrode catalytic materials of fuel cell
Road.
The present invention adopts the following technical scheme that:
A kind of nano-porous materials, using Fe-Pd-P non-crystaline amorphous metals as presoma alloy, under room temperature acidic environment, using change
It learns and takes off alloying technology, prepare the nano-porous materials with uniform reticular structure, the Fe-Pd base nano-porous materials of acquisition are to first
Acid etc. have excellent electrocatalysis characteristic.Wherein, transition-metal Fe element can improve the electrocatalysis characteristic of Pd.Fe-Pd bases are non-
Peritectic alloy ingredient is uniform, and zero defect occurs, and is excellent persursor material.
The nano-porous materials are that the three-dimensional that aperture size is 40 ~ 180nm, hole wall size is 15 ~ 30nm is uniformly netted
Structure.
A kind of method that Fe-Pd base noncrystal alloys prepare nano-porous materials, specifically includes following steps:
Step 1, amorphous alloy component is determined:Using the Fe of high-purity(99.9mass%),Fe3P(99.5mass%),Pd
(99.9mass%)Element and compound press FeaPdbPcComposition of alloy is at assignment system, wherein and 50≤a≤70,0 < b≤
30,0 c≤30 <, and+c=100 a+b;The atomic percent of Fe is bigger in Fe-Pd-P alloy systems, easier formation
Nano-porous structure.
Step 2, non-crystaline amorphous metal master alloy ingot is prepared:Above-mentioned alloy raw material is positioned in induction melting device, is vacuumized
To 8 × 10-3 Pa is hereinafter, and in high-purity argon gas(Purity is 99.99%)Master alloy ingot is made in abundant melting 0.5h under protection;
Step 3, it gets rid of band method using chilling and prepares amorphous alloy ribbon:In chilling gets rid of carrying device, suction less than 2.0 ×
10-3Pa hereinafter, and be filled with high-purity argon gas protection(Purity is 99.99%), master alloy is added using electromagnetic induction effect
Heat sprays master alloy melt to high-speed rotating water-cooled copper roller to after 2000 DEG C, and the rotating speed of copper roller is 2000 revs/min,
It is quickly cooled down obtained amorphous alloy ribbon;
Step 4, nano-porous materials are prepared using the de- alloyage of chemistry:In salpeter solution environment, amorphous alloy ribbon is taken off
Alloy treatment 1 ~ 5h, Fe element corrosion dissolution, Pd elements build up recombination, obtain nano-porous materials, fully clear with deionized water
After washing dry to get.
The non-alloyed strip width of the step 3 is 1 ~ 2mm, thickness is 15 ~ 40 μm.
The salpeter solution of the step 4 is the solution of mass fraction 40 ~ 65%.
Compared with prior art, the present invention advantage is:
The present invention expands the application field of Fe base noncrystal alloys using Fe-Pd base noncrystal alloys as presoma, has also widened de-
The applicable multi-element alloy system range of alloyage;
The present invention prepares nano-porous materials with the de- alloyage of chemistry, and preparation process is simple and efficient, with short production cycle, material cost
Low, applicability is extensive, is easy to industrialized production;
The uniform netted nano-porous materials of three-dimensional prepared by the present invention, aperture size is 40 ~ 180nm, hole wall size be 15 ~
30nm, stable structure, ingredient are adjustable with pattern;
Fe-Pd bases nano-porous materials prepared by the present invention have excellent electrocatalysis characteristic to formic acid etc., can be used as electrode and urge
Change application of the material in electro-catalysis field.
Description of the drawings
Fig. 1 is Fe in the embodiment of the present invention 170Pd20P10The stereoscan photograph figure of amorphous alloy ribbon sample surfaces.
Fig. 2 is the nano-porous materials surface scan electromicroscopic photograph figure that in the embodiment of the present invention 1 prepared by the de- alloy of chemistry.
Fig. 3 be in the embodiment of the present invention 1 amorphous original strip and nano-porous materials to the cyclic voltammetry curve figure of formic acid.
Fig. 4 is the nano-porous materials surface scan electromicroscopic photograph figure that in the embodiment of the present invention 2 prepared by the de- alloy of chemistry.
Fig. 5 is the nano-porous materials surface scan electromicroscopic photograph figure that in the embodiment of the present invention 3 prepared by the de- alloy of chemistry.
Specific implementation mode
Below with reference to accompanying drawings and embodiments, the present invention is described in further detail.
Embodiment 1:Fe70Pd20P10Non-crystaline amorphous metal chemistry takes off alloy treatment and prepares nano-porous materials.
Step 1:Dispensing
According to Fe70Pd20P10The atomic percent of alloying component is converted into weight percent, using the Fe of high-purity
(99.9mass%),Fe3P(99.5mass%),Pd(99.9mass%)Element and compound are weighed by composition of alloy ingredient.
Step 2:Master alloy melting ingot.
The raw metal of preparation is positioned over new skill of Japanese day to grind in NEV-SM04 type vacuum induction melting devices, is vacuumized
It spends to 8 × 10-3 Pa is hereinafter, and in high-purity argon gas(Purity is 99.99%)Abundant melting obtains master alloy ingot under protection.
Step 3:Amorphous alloy ribbon prepares and characterization.
NEV-SM04 type vacuum chillings are ground using new skill of Japanese day and get rid of band device, and suction is less than 2.0 × 10-3Pa with
Under, and it is filled with the argon gas protection of high-purity(Purity is 99.99%), master alloy is positioned over to the quartz of fast cooling device after broken
After master alloy is heated to 2000 DEG C using electromagnetic induction effect, master alloy melt is sprayed to high-speed rotating water cooling by Guan Zhong
On copper roller, the rotating speed of copper roller is 2000 revs/min, is quickly cooled down the amorphous alloy thin that obtained width is 2mm, thickness is 25 μm
Band;Amorphous alloy ribbon material phase analysis, Cu are carried out using the Xpert powder type X-ray diffractometers of Dutch Panaco company
K α radiation, λ 0.15406nm, 2 θ of scanning range are 30 ° ~ 90 °, can test to obtain Fe70Pd20P10Alloy sample is without apparent crystallization
Peak occurs, and has non crystalline structure;Using the Zeiss- Σ IGMA HD type field emission scanning electron microscopes of Zeiss, Germany company to preparation
Amorphous alloy ribbon carries out sample topography observation, and Fe is observed that in stereoscan photograph70Pd20P10Alloy sample ingredient is equal
It is even, the defects of nodeless mesh, dislocation, as shown in Fig. 1.
Step 4:The de- alloy of chemistry prepares nano-porous materials and characterization.
Using the supersonic wave cleaning machine of model JP-020 type bench-top laboratories, by 25 μm of wide 2mm × thickness
Fe70Pd20P10Amorphous alloy ribbon is placed in alcoholic solution after ultrasonic cleaning 5min, using the non-crystaline amorphous metal after cleaning as
The persursor material of the de- alloy of chemistry, be placed on 25 DEG C, the mass fraction of 0.1L be 65% concentrated nitric acid solution in take off at alloy 3h
Reason, salpeter solution are Sinopharm Chemical Reagent Co., Ltd.'s production, are fully cleaned with deionized water after the de- alloy 3h of chemistry
It is spontaneously dried after sample and obtains nano-porous materials;It is scanned using the Zeiss- Σ IGMA HD type Flied emissions of Zeiss, Germany company
Electronic Speculum carries out sample topography observation to the nano-porous materials of preparation, is observed that aperture size is 40 in stereoscan photograph
The uniform netted nano-porous materials of three-dimensional that ~ 80nm, hole wall size are 15 ~ 30nm, as shown in Fig. 2.
Step 5:Nano-porous materials electrocatalysis characteristic is tested.
Cyclic voltammetry curve test, work are carried out using the CHI660 electrochemical workstations of Shanghai Hua Chen Instrument Ltd.
Battery is glass-carbon electrode, with nafion solution by the nano-porous materials and Fe of width 2mm70Pd20P10Amorphous alloy ribbon is distinguished
It is adhered to electrode surface, reference electrode is mereurous sulfate, is platinum filament to electrode.In 25 DEG C, the 0.5mol/L H of 0.01L2SO4+
Nano-porous materials are tested in 0.5mol/L HCOOH electrolyte to formic acid electrocatalysis characteristic;The sweep speed of cyclic voltammetry curve
For 0.1V/s, scanning range is -0.8V ~ 0.8V, as shown in Fig. 3;Through electro-chemical test, Fe70Pd20P10Amorphous alloy ribbon
The oxidation spike potential of formation is 0.1V, and oxidation peak current density is 640 A/m2, the chemical nano-porous materials taken off after alloy 3h
It is -0.09V to form oxidation spike potential, and oxidation peak current density is 1200 A/m2, compared with former strip, oxidation spike potential is negative to be moved
0.19V, oxidation peak current density improve 560A/m2, show Fe70Pd20P10Amorphous alloy ribbon takes off through chemistry at alloy
The nano-porous materials that reason 3h is obtained can improve the electrocatalysis characteristic to formic acid.
Embodiment 2:Fe70Pd20P10Non-crystaline amorphous metal increases the chemistry de- alloy time and prepares nano-porous materials to 5h
With embodiment 1, difference is method:
(1)By 25 μm of Fe of wide 2mm × thickness70Pd20P10Amorphous alloy ribbon be placed on 25 DEG C, the mass fraction of 0.1L be 65%
Alloy 5h processing is taken off in concentrated nitric acid solution prepares nano-porous materials.
(2)It is uniform it to be prepared for the three-dimensional that aperture size is 55 ~ 90nm, hole wall size is 10 ~ 30nm after the de- alloy 5h of chemistry
The nano-porous materials of reticular structure;As shown in Fig. 4.
(3)Increase the chemistry de- alloy time to 5h, promotes Fe70Pd20P10Amorphous alloy ribbon chemistry take off alloying into
Corrosion dissolution persistently occurs for row, Fe elements, and the aperture size of nano-porous materials, which is persistently corroded, to become larger.Illustrate in acid solution
In, increase the chemistry de- alloy time, promotes Fe element etchant solutions, be conducive to the state of tending towards stability.
Embodiment 3:Fe60Pd20P20Non-crystaline amorphous metal chemistry takes off alloy treatment 5h and prepares nano-porous materials
With embodiment 1, difference is method:
(1)By Fe60Pd20P20The melting of nominal composition dispensing and vacuum chilling are got rid of is prepared into 30 μm of wide 2mm × thickness with alloy
Fe60Pd20P20Amorphous alloy ribbon;
(2)By 30 μm of Fe of wide 2mm × thickness60Pd20P20The dense nitre that amorphous alloy ribbon is 65% in the mass fraction of 25 DEG C, 0.1L
In acid solution after the de- alloy 5h of chemistry, sample forms the corrosion cracking structure that a large amount of width are 50 ~ 180nm, as shown in Fig. 5.
(3)Fe60Pd20P20Amorphous alloy ribbon and Fe70Pd20P10Non-crystaline amorphous metal is compared, due to the reduction of Fe elements, 25
DEG C, in the concentrated nitric acid solution that the mass fraction of 0.1L is 65%, Fe70Pd20P10It is molten that non-crystaline amorphous metal is easier generation Fe elements corrosion
Solution, Pd elements diffusions recombinate to form three-dimensional uniform netted nano-porous structure.Illustrate the atom hundred of Fe in Fe-Pd-P alloy systems
Divide ratio bigger, it is easier to form nano-porous structure.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, any made by repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of Fe-Pd bases nano-porous materials, which is characterized in that using Fe-Pd-P non-crystaline amorphous metals as presoma alloy, in room
Under warm acidic environment, using the de- alloying technology of chemistry, the nano-porous materials with uniform reticular structure are prepared.
2. a kind of Fe-Pd bases nano-porous materials according to claim 1, which is characterized in that the nano-porous materials
It is 40 ~ 180nm for aperture size, the uniform reticular structure of three-dimensional that hole wall size is 15 ~ 30nm.
3. a kind of Fe-Pd bases nano-porous materials according to claim 1, which is characterized in that the nano-porous materials
With excellent electrocatalysis characteristic.
4. a kind of a kind of preparation method of Fe-Pd bases nano-porous materials as described in claim 1, which is characterized in that the system
Preparation Method specifically includes following steps:
Step 1, amorphous alloy component is determined:Using the Fe of high-purity(99.9mass%),Fe3P(99.5mass%),Pd
(99.9mass%)Element and compound press FeaPdbPcComposition of alloy is at assignment system, wherein and 50≤a≤70,0 < b≤
30,0 c≤30 <, and+c=100 a+b;The atomic percent of Fe is bigger in Fe-Pd-P alloy systems, easier formation
Nano-porous structure;
Step 2, non-crystaline amorphous metal master alloy ingot is prepared:Above-mentioned alloy raw material is positioned in induction melting device, it is evacuated to 8 ×
10-3 Pa is hereinafter, and in high-purity argon gas(Purity is 99.99%)Master alloy ingot is made in abundant melting 0.5h under protection;
Step 3, it gets rid of band method using chilling and prepares amorphous alloy ribbon:In chilling gets rid of carrying device, suction is less than 2.0 × 10-3Pa hereinafter, and be filled with high-purity argon gas protection(Purity is 99.99%), master alloy is heated using electromagnetic induction effect
To after 2000 DEG C, master alloy melt is sprayed to high-speed rotating water-cooled copper roller, the rotating speed of copper roller is 2000 revs/min, soon
Amorphous alloy ribbon is but made in quickly cooling;
Step 4, nano-porous materials are prepared using the de- alloyage of chemistry:In salpeter solution environment, amorphous alloy ribbon is taken off
Alloy treatment 1 ~ 5h, Fe element corrosion dissolution, Pd elements build up recombination, obtain nano-porous materials, fully clear with deionized water
After washing dry to get.
5. a kind of preparation method of Fe-Pd bases nano-porous materials according to claim 4, which is characterized in that the step
Rapid 3 non-alloyed strip width is 1 ~ 2mm, thickness is 15 ~ 40 μm.
6. a kind of preparation method of Fe-Pd bases nano-porous materials according to claim 4, which is characterized in that the step
Rapid 4 salpeter solution is the solution of mass fraction 40 ~ 65%.
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Cited By (7)
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CN109518215A (en) * | 2018-11-16 | 2019-03-26 | 佛山科学技术学院 | A kind of nano-meter porous amorphous state electro catalytic electrode and its preparation method and application |
CN110224148A (en) * | 2019-05-24 | 2019-09-10 | 华中科技大学 | The porous PdFe intermetallic compound and the preparation method and application thereof of Pt or Au modification |
CN111068647A (en) * | 2020-01-02 | 2020-04-28 | 南京工程学院 | Nano TiO (titanium dioxide)2-SnO2Preparation method of solid solution photocatalytic material |
CN111118523A (en) * | 2020-01-16 | 2020-05-08 | 暨南大学 | Method for improving catalytic activity of Fe-based amorphous alloy for hydrogen evolution by electrolysis water through dealloying treatment |
CN114192132A (en) * | 2021-12-15 | 2022-03-18 | 合肥工业大学 | Method for simultaneously obtaining nano-porous strip and nano-fiber powder |
CN114724861A (en) * | 2022-04-18 | 2022-07-08 | 东南大学 | Method for preparing flexible sandwich type amorphous alloy composite electrode |
CN115537622A (en) * | 2022-06-08 | 2022-12-30 | 湖南大学 | Transition metal atom modified nanoporous ReSe 2 Material and method for the production thereof |
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CN109518215A (en) * | 2018-11-16 | 2019-03-26 | 佛山科学技术学院 | A kind of nano-meter porous amorphous state electro catalytic electrode and its preparation method and application |
CN109518215B (en) * | 2018-11-16 | 2021-06-15 | 佛山科学技术学院 | Nano porous amorphous electrocatalytic electrode and preparation method and application thereof |
CN110224148A (en) * | 2019-05-24 | 2019-09-10 | 华中科技大学 | The porous PdFe intermetallic compound and the preparation method and application thereof of Pt or Au modification |
CN111068647A (en) * | 2020-01-02 | 2020-04-28 | 南京工程学院 | Nano TiO (titanium dioxide)2-SnO2Preparation method of solid solution photocatalytic material |
CN111068647B (en) * | 2020-01-02 | 2022-12-09 | 南京工程学院 | Nano TiO (titanium dioxide) 2 -SnO 2 Method for preparing solid solution photocatalytic material |
CN111118523A (en) * | 2020-01-16 | 2020-05-08 | 暨南大学 | Method for improving catalytic activity of Fe-based amorphous alloy for hydrogen evolution by electrolysis water through dealloying treatment |
CN114192132A (en) * | 2021-12-15 | 2022-03-18 | 合肥工业大学 | Method for simultaneously obtaining nano-porous strip and nano-fiber powder |
CN114192132B (en) * | 2021-12-15 | 2024-03-05 | 合肥工业大学 | Method for simultaneously obtaining nano porous strip and nano fiber powder |
CN114724861A (en) * | 2022-04-18 | 2022-07-08 | 东南大学 | Method for preparing flexible sandwich type amorphous alloy composite electrode |
CN115537622A (en) * | 2022-06-08 | 2022-12-30 | 湖南大学 | Transition metal atom modified nanoporous ReSe 2 Material and method for the production thereof |
CN115537622B (en) * | 2022-06-08 | 2023-09-26 | 湖南大学 | Transition metal atom modified nanoporous ReSe 2 Material and preparation method thereof |
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