CN106784889A - A kind of palladium ferriferous oxide fuel-cell catalyst and preparation method thereof - Google Patents
A kind of palladium ferriferous oxide fuel-cell catalyst and preparation method thereof Download PDFInfo
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- CN106784889A CN106784889A CN201611138558.1A CN201611138558A CN106784889A CN 106784889 A CN106784889 A CN 106784889A CN 201611138558 A CN201611138558 A CN 201611138558A CN 106784889 A CN106784889 A CN 106784889A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9041—Metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention discloses a kind of palladium ferriferous oxide fuel-cell catalyst, Pd and Fe elements are loaded on the activated carbon, structural formula is Pd Fe/C, and the Pd Fe load capacity is 20~50%；The Pd Fe particle diameters are 3.5~4.5nm.The invention also discloses the preparation method of the catalyst.The method comprises the steps of firstly, preparing support type Monodisperse nanocrystals carbon load iron nano-crystalline Fe/C, and spontaneous displacement reaction is carried out with palladium salt solution in aqueous, because the reduction potential power of palladium presoma is higher than ferrous metal potential force, so as to obtain the catalyst of bimetallic Pd Fe/C 1；Then it is thermally treated resulting in the catalyst of Pd Fe/C 2 using high-purity argon gas.The content of metal of catalyst of the present invention is 20~50%, it has the advantages that the catalytic capability stronger to formic acid electrocatalytic oxidation, catalytic efficiency higher, stronger CO tolerance catalysts ability and lower cost, can be used to preparing direct methanoic acid fuel cell catalyst, and method is simple, low consumption, environmental-friendly and efficient.
Description
Technical field
The invention belongs to fuel cell catalyst technical field, and in particular to a kind of palladium ferriferous oxide fuel cell catalyst
Agent.The invention further relates to the preparation method of the palladium ferriferous oxide fuel-cell catalyst.
Background technology
Low-temperature fuel cell has cleaning, efficient, safe, removable, operating condition gently and Mirae Corp. has
The advantages of development potentiality, enjoys the attention of countries in the world, including Proton Exchange Membrane Fuel Cells, DMFC and straight
Connect aminic acid fuel battery etc..Elctro-catalyst, PEM and electrode are low-temperature fuel cell critical materials, and high cost is mesh
The main problem of preceding puzzlement commercializing fuel cells, it is a large amount of wherein in catalyst to use Pt materials so that the cost of catalyst
Account for very big proportion.Nowadays Pd bases catalyst has attracted everybody concern, Pd and Pt have similar property (such as period element,
Allomeric structure, homoatomic size), and the price of Pd is that the storage level of 1/3, Pd of Pt is but 50 times of Pt.Gone out according to this
Hair point, we can contemplate and adulterate second metallic element (for example by Pd：Au, Pt, Ir, Pb, Sn, Co, Ni etc.) carry
The activity of Pd bases catalyst high, to substitute the application in a fuel cell of Pt bases catalyst with Pd bases catalyst.It is Chinese special
Sharp CN 101664685A disclose a kind of two steps chemical reduction method and are prepared for PdFe@Pt/C catalyst with core-casing structure, in 0.4V
(Ag/AgCl) the oxygen reduction activity electric current of PdFe@Pt/C catalyst unit platinum quality is 0.126A mg when-1 Pt, its catalysis efficiency
About 4 times of business Pt/C catalyst.Although introducing Pd and Fe to reduce catalyst cost, catalysis activity is still suffered from
The problem of not high and cost control difference.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of low cost and the combustion of the palladium ferriferous oxide with high catalytic activity
Material cell catalyst.The invention solves the problems that another technical problem be to provide one kind and prepare the palladium ferriferous oxide fuel cell and urge
The preparation method of agent.
The present invention solves above-mentioned technical problem by following technological means,
A kind of palladium ferriferous oxide fuel-cell catalyst, it is characterised in that load Pd and Fe elements, structure on the activated carbon
Formula is Pd-Fe/C, and the Pd-Fe load capacity is 20~50%；The Pd-Fe particle diameters are 3.5~4.5nm.
The invention solves the problems that another technical problem be to provide one kind and prepare the palladium ferriferous oxide fuel-cell catalyst
Preparation method,
A kind of palladium ferriferous oxide fuel-cell catalyst preparation method, step is as follows,
(1) activated carbon of 10mg is scattered in the aqueous solution of 6mL, and 60~120min of ultrasound；
(2) continue to stir and be passed through 30~120min of inert atmosphere in ultrasonic procedure, to remove the dissolved oxygen in solution；
(3) under ultrasound, stirring and inert atmosphere protection, the hydroboron of metering is added；
(4) the soluble ferrite wiring solution-forming that will be measured；After adding hydroboron to terminate 30~120min, dropwise add
Enter the soluble ferrite solution of metering, so that Fe2+It is reduced into Fe0, 15~60min is stirred, obtain Fe/C solution；
(5) the soluble palladium compound wiring solution-forming that will be measured, and it is added dropwise to the Fe/C solution of step (4) preparation
In, then persistently stir 20~60min；
(6) filter and be washed with deionized, filter residue is vacuum dried 4~6h at 50~70 DEG C of vacuum drying chamber, that is, make
Obtain Pd-Fe/C-1 catalyst.
As optimization, after step (6), by the Pd-Fe/C-1 catalyst, the tube furnace of internal diameter 6cm 100cm long is placed on
In, protective atmosphere is passed through with 200mL/min and drives within 15 minutes air in tube furnace, then adjusted above-mentioned protection is passed through with 20mL/min
Atmosphere and intensification, and 200~500 DEG C of 2~4h of calcining in protective atmosphere, are cooled to room temperature in protective atmosphere, that is, Pd- is obtained
Fe/C-2 catalyst；
Used as optimization, the protective atmosphere is in high-purity argon gas, high pure nitrogen, high-purity helium, high-purity carbon dioxide gas
One kind；
As optimization, oxide PdO and Fe are contained through the Pd-Fe/C-2 catalyst after Overheating TreatmentxOy, wherein x=2~
3, y=2~4.
Used as optimization, activated carbon described in step (1) is Vulan XC-72R, particle diameter 30nm, specific surface area SBET=
237m2·g-1；
Used as optimization, inert atmosphere described in step (2) is nitrogen, carbon dioxide or argon gas；
Used as optimization, hydroboron described in step (3) is sodium borohydride and/or potassium borohydride；
Used as optimization, the Pd-Fe load capacity of the Pd-Fe/C-1 catalyst and Pd-Fe/C-2 catalyst is 20~50%；
The Pd-Fe particle diameters are 3.5~4.5nm；
Used as optimization, the concentration of the soluble ferrite solution is 0.09mol/L；Soluble palladium compound solution it is dense
It is 1g/100mL to spend；
Used as optimization, the soluble ferrite is one or more group in ferrous sulfate, frerrous chloride, ferrous nitrate
Close；
Used as optimization, the soluble palladium compound is palladium bichloride, the acid of chlorine palladium, palladium nitrate；
Used as optimization, the ferro element in the soluble ferrite is with the mol ratio of the palladium element of soluble palladium compound
15~5:1；
Used as optimization, it is 1.2~3 that the hydroboration is closed with the ferro element thing mol ratio in the soluble ferrite:1.
The method comprises the steps of firstly, preparing support type Monodisperse nanocrystals-carbon load iron nano-crystalline Fe/C, and in aqueous with palladium
Salting liquid carries out spontaneous displacement reaction, because the reduction potential power of palladium presoma is higher than ferrous metal potential force, so as to obtain double gold
Category Pd-Fe/C-1 catalyst；Then it is thermally treated resulting in Pd-Fe/C-2 catalyst using high-purity argon gas.The gold of catalyst of the present invention
Category load capacity is 20~50%, and it has the catalytic capability stronger to formic acid electrocatalytic oxidation, catalytic efficiency higher, stronger
The advantages of CO tolerance catalysts ability and lower cost, can be used to prepare direct methanoic acid fuel cell catalyst, and method is simple, low
Consumption, it is environmental-friendly and efficient.
Brief description of the drawings
Fig. 1 is the TEM figures of Pd-Fe/C-1 catalyst prepared by the embodiment of the present invention 1；
Fig. 2 is the TEM figures of Pd-Fe/C-2 catalyst prepared by the embodiment of the present invention 2；
Fig. 3 is the XRD of catalyst prepared by the embodiment of the present invention 1 and 2；
Fig. 4 is the cyclic voltammetry curve that embodiment 1 and 2 prepares catalyst.
Specific embodiment
Embodiment 1
A kind of palladium ferriferous oxide fuel-cell catalyst preparation method, step is as follows,
(1) activated carbon of 10mg is scattered in the aqueous solution of 6mL, and 60~120min of ultrasound；The activated carbon is
Vulan XC-72R, particle diameter 30nm, SBET=237m2·g-1；
(2) continue to stir and be passed through 30~120min of Ar atmosphere in ultrasonic procedure to remove the dissolved oxygen in solution；
(3) it is being stirred continuously with Ar atmosphere protections, is disposably adding the NaBH of 9.8mg4(total 0.26mmol)；
(4) FeSO that will be measured4It is made into the 0.09mol/L aqueous solution；Add NaBH4After terminating 30~120min, it is added dropwise over
2mL concentration is the FeSO of 0.09mol/L4Solution (total 0.18mmol), so that Fe2+It is reduced into Fe0, 15~60min is stirred,
Obtain Fe/C solution；
(5) by the PdCl of 2.13mg2Wiring solution-forming (total 0.012mmol), and be added dropwise in above-mentioned Fe/C solution,
20~60min of stirring；PdCl2The concentration of solution is 1g/100mL；Fe:Pd mol ratios are 15:1；
(6) filter and be washed with deionized soluble ferrite and soluble palladium compound are can't detect into cleaning solution
Anion, such as Cl-And SO4 2-, filter residue is vacuum dried 4~6h at 50~70 DEG C of vacuum drying chamber, that is, Pd-Fe/C-1 is obtained
Catalyst；Pd-Fe load capacity is 50%, Pd-Fe particle diameters, 3.5~4.5nm.
Electrochemical results show (Fig. 4), and the Pd-Fe/C-1 catalyst shows electro catalytic activity (table 1),
Peak current under 0.21V spike potentials is 0.76A mg-1, its catalysis efficiency is about 24 times of business Pt/C catalyst；TEM photos
(Fig. 1) shows that the catalyst is uniformly dispersed on the carbon carrier.
Embodiment 2
A kind of palladium ferriferous oxide fuel-cell catalyst preparation method, step is as follows,
(1) the Pd-Fe/C-1 catalyst for preparing embodiment 1, is placed in the tube furnace of internal diameter 6cm 100cm long, with
200mL/min is passed through high-purity argon gas and drives within 15 minutes air in tube furnace, then adjusts and be passed through high-purity argon gas and liter with 20mL/min
Temperature, 200~500 DEG C of 2~4h of calcining, are cooled to room temperature in protective atmosphere in high-purity argon gas atmosphere, that is, Pd-Fe/C-2 is obtained
Catalyst；Pd-Fe load capacity 50%, 3.5~4.5nm of Pd-Fe particle diameters.
Electrochemical results show (Fig. 4), and the Pd-Fe/C-2 catalyst shows electro catalytic activity (table 1),
Peak current under 0.21V spike potentials is 3.68A mg-1, it is 4.8 times of Pd-Fe/C-1 catalyst before heat treatment, its catalysis efficiency
About 116 times of business Pt/C catalyst.TEM photos (Fig. 2) show that the catalyst is uniformly dispersed on the carbon carrier.
XRD spectrum (Fig. 3) display Pd-Fe/C-1 catalyst only has the crystallographic plane diffraction peak of Pd, and Pd-Fe/C-2 catalyst is same
When have the crystallographic plane diffraction peak of Pd and PdO.
Embodiment 3
A kind of palladium ferriferous oxide fuel-cell catalyst preparation method, step is as follows,
(1) activated carbon of 10mg is scattered in the aqueous solution of 6mL, and 60~120min of ultrasound；The activated carbon is
Vulan XC-72R, particle diameter 30nm, SBET=237m2·g-1；
(2) continue to stir and be passed through N in ultrasonic procedure230~120min of atmosphere is removing the dissolved oxygen in solution；
(3) it is being stirred continuously and N2Under atmosphere protection, the KBH of disposable addition 11.65mg4(total 0.216mmol)；
(4) FeCl that will be measured2It is made into the aqueous solution of 0.09mol/L；Add KBH4After terminating 30~120min, dropwise add
Enter the FeCl that 2mL concentration is 0.09mol/L2Solution (total 0.18mmol), so that Fe2+It is reduced into Fe0, stirring 15~
60min, obtains Fe/C solution；
(5) by the H of 4.51mg2PdCl4Wiring solution-forming (total 0,018mmol), and it is added dropwise to above-mentioned Fe/C solution
In, stir 20~60min；H2PdCl4The concentration of solution is 1g/100mL；Fe:Pd mol ratios are 10:1；
(6) filter and be washed with deionized, filter residue is vacuum dried 4~6h at 50~70 DEG C of vacuum drying chamber, that is, make
Obtain Pd-Fe/C-1 catalyst；
(7) by Pd-Fe/C-1 catalyst obtained above, it is placed in the tube furnace of internal diameter 6cm 100cm long, with 200mL/
Min is passed through high pure nitrogen and drives within 15 minutes air in tube furnace, then adjusts and be passed through high pure nitrogen and intensification with 20mL/min, in height
200~500 DEG C of 2~4h of calcining, are cooled to room temperature in protective atmosphere in pure nitrogen gas atmosphere, that is, Pd-Fe/C-2 catalyst is obtained；
Pd-Fe load capacity 20%, 3.5~4.5nm of Pd-Fe particle diameters.Embodiment 4
A kind of palladium ferriferous oxide fuel-cell catalyst preparation method, step is as follows,
(1) activated carbon of 10mg is scattered in the aqueous solution of 6mL, and 60~120min of ultrasound；The activated carbon is
Vulan XC-72R, particle diameter 30nm, SBET=237m2·g-1；
(2) continue to stir and be passed through 30~120min of carbon dioxide atmosphere in ultrasonic procedure to remove the dissolving in solution
Oxygen；
(3) it is being stirred continuously with carbon dioxide atmosphere protection, is disposably adding the NaBH of 10.21mg4It is (total
0.27mmol) with the KBH of 14.56mg4(total 0.27mmol)；
(4) Fe (NO that will be measured3)2It is made into the aqueous solution of 0.09mol/L；Add NaBH4And KBH4Terminate 30~120min
Afterwards, the Fe (NO that 2mL concentration is 0.09mol/L are added dropwise over3)2Solution (total 0.18mmol), so that Fe2+It is reduced into Fe0,
15~60min of stirring, obtains Fe/C solution；
(5) by the Pd (NO of 8.30mg3)2Wiring solution-forming (total 0.036mol), and it is added dropwise to above-mentioned Fe/C solution
In, continue to stir 20~60min after completion of dropwise addition；Pd(NO3)2The concentration of solution is 1g/100mL；Fe:Pd mol ratios are 5:1；
(6) filter and be washed with deionized, filter residue is vacuum dried 4~6h at 50~70 DEG C of vacuum drying chamber, that is, make
Obtain Pd-Fe/C-1 catalyst；
(7) by Pd-Fe/C-1 catalyst obtained above, it is placed in the tube furnace of internal diameter 6cm 100cm long, with 200mL/
Min is passed through high-purity helium or high-purity carbon dioxide drives air in tube furnace for 15 minutes, then adjust be passed through with 20mL/min it is above-mentioned
Protective atmosphere and intensification, 200~500 DEG C of 2~4h of calcining, are cooled to room in protective atmosphere in above-mentioned protective atmosphere atmosphere
Temperature, that is, be obtained Pd-Fe/C-2 catalyst；Pd-Fe load capacity 35%, 3.5~4.5nm of Pd-Fe particle diameters.
The electro-chemical test of embodiment 5
What electro-chemical test was determined in the three-electrode system of standard.With a diameter of 5mm and difference load embodiment 1 and reality
Apply example 2 and prepare the glass-carbon electrode of catalyst for working electrode, with platinum piece be to electrode, with calomel electrode as reference electrode,
Carry out electro-chemical test.Electrolytic cell concentrated sulfuric acid hydrogen peroxide digestion, and cleaned up with ultra-pure water.To explore catalyst to formic acid
Electrocatalytic oxidation property, electrolyte for 0.1mol/L HClO4, the HClO of 0.1mol/L4The HCOOH solution of+0.5mol/L.
Before electro-chemical test, in order to exclude influence of the oxygen to electrochemical reaction in air, various electrolyte solutions are respectively with high-purity
Nitrogen excludes the air in solution.The electric potential scanning scope of cyclic voltammetry is 0~1.0V, and sweep speed is 50mV s-1,
Laboratory temperature is 25 ± 1 DEG C.
Table 1 is the form of the corresponding peak current density of the catalyst curve of the embodiment of the present invention 1 and 2 and spike potential.
Claims (10)
1. a kind of palladium ferriferous oxide fuel-cell catalyst, it is characterised in that load Pd elements and Fe elements, knot on the activated carbon
Structure formula is Pd-Fe/C, and the Pd-Fe load capacity is 20~50%；The Pd-Fe particle diameters are 3.5~4.5nm.
2. palladium ferriferous oxide fuel-cell catalyst preparation method as claimed in claim 1, step is as follows,
(1) activated carbon of 10mg is scattered in the aqueous solution of 6mL, and 60~120min of ultrasound；
(2) continue to stir and be passed through 30~120min of inert atmosphere in ultrasonic procedure, to remove the dissolved oxygen in solution；
(3) under ultrasound, stirring and inert atmosphere protection, the hydroboron of metering is added；
(4) the soluble ferrite wiring solution-forming that will be measured；After adding hydroboron to terminate 30~120min, meter is added dropwise over
The soluble ferrite solution of amount, so that Fe2+It is reduced into Fe0, 15~60min is stirred, obtain Fe/C solution；
(5) the soluble palladium compound wiring solution-forming that will be measured, and be added dropwise in the Fe/C solution of step (4) preparation, then
Persistently stir 20~60min；
(6) filter and be washed with deionized, filter residue is vacuum dried 4~6h at 50~70 DEG C of vacuum drying chamber, that is, Pd- is obtained
Fe/C-1 catalyst.
3. palladium ferriferous oxide fuel-cell catalyst preparation method as claimed in claim 2, it is characterised in that after step (6),
The Pd-Fe/C-1 catalyst is placed in the tube furnace of internal diameter 6cm 100cm long, 15 points of protective atmosphere is passed through with 200mL/min
Clock drives air in tube furnace, then adjusts and be passed through above-mentioned protective atmosphere and intensification with 20mL/min, and 200 in protective atmosphere~
500 DEG C of 2~4h of calcining, are cooled to room temperature in protective atmosphere, that is, Pd-Fe/C-2 catalyst is obtained.
4. palladium ferriferous oxide fuel-cell catalyst preparation method as claimed in claim 3, it is characterised in that the protective atmosphere
It is the one kind in high-purity argon gas, high pure nitrogen, high-purity helium, high-purity carbon dioxide gas.
5. palladium ferriferous oxide fuel-cell catalyst preparation method as claimed in claim 2, it is characterised in that institute in step (1)
Activated carbon is stated for Vulan XC-72R, particle diameter 30nm, specific surface area SBET=237m2·g-1。
6. palladium ferriferous oxide fuel-cell catalyst preparation method as claimed in claim 2, it is characterised in that institute in step (3)
Hydroboron is stated for sodium borohydride and/or potassium borohydride.
7. palladium ferriferous oxide fuel-cell catalyst preparation method as claimed in claim 2, it is characterised in that described soluble sub-
Molysite is one or more combination in ferrous sulfate, frerrous chloride, ferrous nitrate.
8. palladium ferriferous oxide fuel-cell catalyst preparation method as claimed in claim 2, it is characterised in that the soluble palladium
Compound is palladium bichloride, the acid of chlorine palladium, palladium nitrate.
9. palladium ferriferous oxide fuel-cell catalyst preparation method as claimed in claim 2, it is characterised in that described soluble sub-
Ferro element and the mol ratio of the palladium element of soluble palladium compound in molysite are 15~5:1.
10. palladium ferriferous oxide fuel-cell catalyst preparation method as claimed in claim 2, it is characterised in that the hydroboration
It is 1.2~3 to close with the ferro element thing mol ratio in the soluble ferrite:1.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109148904A (en) * | 2018-09-20 | 2019-01-04 | 宁波高新区诠宝绶新材料科技有限公司 | A kind of preparation method of proton exchange membrane direct methanoic acid fuel cell catalyst |
| CN110729485A (en) * | 2019-09-12 | 2020-01-24 | 东南大学 | Preparation method and application of porous carbon-coated PdFe/C alloy nano-frame |
| US20210252488A1 (en) * | 2020-02-18 | 2021-08-19 | United States Government, as represented by the Administrator of the U.S. EPA | Synthesis of metallic materials imbedded in activated carbon to degrade chlorinated and fluorinated organic pollutants |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102903939A (en) * | 2012-10-17 | 2013-01-30 | 厦门大学 | Fuel-cell catalyst with non-platinum core-shell structure and preparation method of fuel-cell catalyst |
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2016
- 2016-12-12 CN CN201611138558.1A patent/CN106784889A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102903939A (en) * | 2012-10-17 | 2013-01-30 | 厦门大学 | Fuel-cell catalyst with non-platinum core-shell structure and preparation method of fuel-cell catalyst |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109148904A (en) * | 2018-09-20 | 2019-01-04 | 宁波高新区诠宝绶新材料科技有限公司 | A kind of preparation method of proton exchange membrane direct methanoic acid fuel cell catalyst |
| CN110729485A (en) * | 2019-09-12 | 2020-01-24 | 东南大学 | Preparation method and application of porous carbon-coated PdFe/C alloy nano-frame |
| US20210252488A1 (en) * | 2020-02-18 | 2021-08-19 | United States Government, as represented by the Administrator of the U.S. EPA | Synthesis of metallic materials imbedded in activated carbon to degrade chlorinated and fluorinated organic pollutants |
| US11701642B2 (en) * | 2020-02-18 | 2023-07-18 | United States Government, as represented by the Administrator of the U.S. EPA, Waashington DC | Synthesis of metallic materials imbedded in activated carbon to degrade chlorinated and fluorinated organic pollutants |
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