CN106807365A - A kind of preparation method of core shell structure elctro-catalyst - Google Patents
A kind of preparation method of core shell structure elctro-catalyst Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of core shell structure elctro-catalyst.Specifically in the solution, it is reducing agent with hydrogen, in a kind of metal nanoparticle surface one or more the metallic element of the reduction comprising platinum group of energy adsorbed hydrogen, the metal nanoparticle of the core shell structure that surface is coated by platinum group metal is obtained.The electrocatalyst materials obtained using the preparation method have huge application prospect in terms of Proton Exchange Membrane Fuel Cells and electrolytic cell.
Description
Technical field
The present invention relates to a kind of preparation method of core shell structure elctro-catalyst.
Background technology
Core shell structure is an effective ways of the noble metal load amount in catalyst that reduces.In catalyst with core-casing structure
In, core is made up of base metal, and shell is made up of noble metal, so that the reactivity of precious metal atom
Site is fully exposed, and improves the decentralization and utilization rate of noble metal, and noble metal contains in reducing catalyst
Amount.At present, the preparation method of noble metal catalyst with core-casing structure mainly has post treatment method, displacement method, owes electricity
Position sedimentation and seed mediated growth method etc..
Adzic et al. (L.Yang et.al., the Journal of Physical Chemistry C, 117
(2013) 1748-1753) using the method for underpotential deposition, individual layer copper is deposited in Ru nano grain surfaces,
Reacted by the displacement between K2PtCl4 and copper, the core shell structure hydrogen reduction for obtaining individual layer platinum cladding Ru is urged
Agent.Because main reaction occurs on electrode, there is certain difficulty in the amplification of preparation technology.Additionally,
The formation of core shell structure is mainly on the basis of existing core to be carried out reducing other elements.Yu et al. (Li
et.al.,Journal of the American Chemical Society,137(2015)7862-7868)
In the case where bromide ion is used as protective agent and etching agent, make H2PtCl6 that displacement occur with Pd nano wires anti-
Should, obtain the core shell structure that platinum coats Pd.Introducing bromide ion increases complex process degree, and to environment
Adversely affect；The Pd that replacement process is sacrificed increases cost.
Chinese patent 201110119977.1 discloses a kind of method, is lived as surface in larger molecular organicses
Property agent exist under conditions of prepare metal nanoparticle with hydrogen.The preparation temperature of different metal nano particle is not
Together, and the preparation temperature of platinum and palladium nano-particles is above 50 DEG C.Prepared metal nanoparticle is not
Carry out electrochemical catalysis performance test.Chinese patent 201210120922.7 discloses a kind of method, uses
High boiling point organic compound ethylene glycol is solvent and protective agent, under conditions of more than 80 DEG C, in the palladium copper of carbon-supported type
Nano grain surface reduces platinum, through past alloy, obtains the carbon supported core-shell copper palladium-platinum catalyst of de- alloy,
But do not provide electrocatalysis characteristic test result.United States Patent (USP) 2009/0114061A1 discloses a kind of method,
By the elctro-catalyst for freezing, drying, anneal, go alloy to obtain core shell structure.Step is relatively complicated, and
And go the metal that alloy lost to increase cost, cause the destruction to environment.United States Patent (USP) 2012/0135862
A1 discloses a kind of method, and using amido organic matter as reducing agent, ether base organic matter is high as solvent
The use of boiling organics brings difficulty to the cleaning process of catalyst；And must contain in the core of core shell structure
The element for having the one kind in palladium, copper or iridium, shell can not limit core shell structure beyond platinum, gold or iridium
Element composition.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of cleaning, simple, low cost, rapidly prepare
The method of core shell structure elctro-catalyst.
The present invention is comprised the steps of：
To voluntarily prepare or commercialized loaded/non-supported metal M1 nano particles are distributed to water, have
Among machine solvent or the mixture of the two, at a certain temperature, hydrogen, in addition platinum group metal one are passed through
Kind or more than two kinds of soluble metallic salt, react the regular hour under a reducing atmosphere, be centrifuged, wash,
The M1@M2 metal nanoparticles of the core shell structure that drying to obtain surface is coated by platinum group metal；
Preparation method of the present invention, it is characterised in that：Metal M1 be can the Mo of adsorbed hydrogen, Rh,
One or two or more kinds in Pt, Ti, Co, Ni, Fe, Cr, Pd.
Preparation method of the present invention, it is characterised in that：Organic solvent be methyl alcohol, ethanol, isopropanol,
One or two or more kinds in ethylene glycol, polyethylene glycol etc..
Preparation method of the present invention, it is characterised in that：Reaction temperature is 0-160 DEG C, and the reaction time is
0.1-24 hours；The purity of hydrogen is 0-100%, and flow velocity is 0.1-500mL min-1.
Preparation method of the present invention, it is characterised in that：Described platinum group metal is Pt, Pd, Ir, Ru
In one or two or more kinds；Described platinum group metal precursor be Pt, Pd, Ir, Ru in one kind or
One or two or more kinds in more than two kinds of sulfate, nitrate, halide, halogen acids or halogen acid salt.
The preparation method of the elctro-catalyst of loaded M1@M2 core shell structures of the present invention, using environment
Friendly hydrogen is made without using surfactant as reducing agent, preparation process without larger molecular organicses
It is solvent or reducing agent, it is not necessary to which the post processing such as high temperature can obtain the elctro-catalyst of surface cleaning, simplifies and prepares
Technique, reduces preparation cost, is easy to large-scale production；Prepare core shell structure process and be provided without sacrificing element,
Belong to atom economy type preparation method；Element species that the core of core shell structure can be selected with shell and composition are more
Extensively, making the present invention has the larger scope of application.
Brief description of the drawings
The TEM figures of the Pd/C that Fig. 1 is used by the embodiment of the present invention one；
Fig. 2 is the particle diameter distribution histogram of Pd nano particles corresponding with Fig. 1.The particle diameter of Pd nano particles
It is mainly distributed between 2.5-4.5nm, average grain diameter is 3.4nm, and is uniformly dispersed on the carbon carrier.
Fig. 3 is the TEM figures of Pd@Pt/C prepared by the embodiment of the present invention one；
Fig. 4 is the particle diameter distribution histogram of Pd@Pt nano particles corresponding with Fig. 3.Pd@Pt nano particles
Particle diameter be mainly distributed between 3.0-7.0nm, average grain diameter is 4.9nm, and is disperseed on the carbon carrier
Uniformly.
Fig. 5 is the TEM figures of Pt/C prepared by comparative example of the present invention；
Fig. 6 is the particle diameter distribution histogram of Pt nano particles corresponding with Fig. 5.The particle diameter of Pt nano particles
It is mainly distributed between 2.0-14.0nm, average grain diameter is 7.6nm, disperses uneven on the carbon carrier.
Fig. 7 is respectively Pd@Pt/C, the Pd/C that is used and the system of comparative example one of the preparation of the embodiment of the present invention one
Standby Pt/C tests the cyclic voltammetry curve figure for obtaining by rotating disk electrode (r.d.e) (RDE)；
The Pt/C that the Pd@Pt/C that Fig. 8 is respectively the preparation of the embodiment of the present invention one are prepared with comparative example one passes through
The polarization curves of oxygen reduction figure that rotating disk electrode (r.d.e) (RDE) test is obtained.Cyclic voltammetry electrolyte
It is the 0.1mol/L HClO4 aqueous solution of N2 saturations, sweeps speed for 50mV/s.Polarization curves of oxygen reduction is tested
With the 0.1mol/L HClO4 aqueous solution that electrolyte is O2 saturations, speed is swept for 10mV/s, forward scan,
RDE rotating speeds are 1600rpm.Test is carried out at room temperature, and metal load amount is 19 μ g/cm2 on electrode.
Fig. 9 is Pd Pt/C prepared by the embodiment of the present invention one and the Pt/C of the preparation of comparative example one is through more than half electricity
The hydrogen reduction catalytic quantity specific activity comparison diagram that pond test is obtained.
Figure 10 is that Pd@Pt-2/C prepared by the embodiment of the present invention two are tested by rotating disk electrode (r.d.e) (RDE)
The cyclic voltammetry curve for obtaining；
Figure 11 is that Pd@Pt-2/C prepared by the embodiment of the present invention two are tested by rotating disk electrode (r.d.e) (RDE)
The polarization curves of oxygen reduction for obtaining.
Figure 12 is the TEM figures of Pd@Ir/C prepared by the embodiment of the present invention two；
Figure 13 is the particle diameter distribution histogram of Pd@Ir nano particles corresponding with Figure 12.Pd@Ir nanometers
The particle diameter of grain is mainly distributed between 3.0-6.0nm, and average grain diameter is 4.4nm, and is divided on the carbon carrier
Dissipate uniform.
Figure 14 is that Rh@Pt/C prepared by the embodiment of the present invention two are tested by rotating disk electrode (r.d.e) (RDE)
The cyclic voltammetry curve for arriving；
Figure 15 is that Rh@Pt/C prepared by the embodiment of the present invention two are tested by rotating disk electrode (r.d.e) (RDE)
The polarization curves of oxygen reduction for arriving.
Figure 16 is that Ir@Pt/C prepared by the embodiment of the present invention two are followed in rotating disk electrode (r.d.e) (RDE) test
Ring volt-ampere curve；
Figure 17 is that Ir@Pt/C prepared by the embodiment of the present invention two are analysed in rotating disk electrode (r.d.e) (RDE) test
Oxygen reaction polarization curve map.Cyclic voltammetry electrolyte is that the 0.5mol/L H2SO4 of N2 saturations are water-soluble
Liquid, sweeps speed for 50mV/s, sweep limits 0-1.45V vs.RHE.The test of oxygen evolution reaction polarization curve is used
Electrolyte is the 0.5mol/L H2SO4 aqueous solution of N2 saturations, sweeps speed for 5mV/s, forward scan, RDE
Rotating speed is 1600rpm.Test is carried out at room temperature, and metal load amount is 19 μ g/cm2 on electrode.
Figure 18 is that Ni@Pt/C prepared by the embodiment of the present invention three are followed in rotating disk electrode (r.d.e) (RDE) test
Ring volt-ampere curve；
Figure 19 be the embodiment of the present invention three prepare Ni@Pt/C rotating disk electrode (r.d.e) (RDE) test in oxygen
Reduction reaction polarization curve.
Specific embodiment
Embodiment one：
1. 50mg Pd/C (BASF) are taken in there-necked flask, and wherein the mass fraction of Pd is 20%；
The mixed solution of 50.0mL deionized waters and ethanol is added, its reclaimed water is 3 with the volume ratio of ethanol:1；Stir
Mix and ultrasound is dispersed in the solution to Pd/C.
2. it is the H of 100mL/min to flow velocity is passed through in above-mentioned solution2/N2Mixed gas, wherein H2With
N2Volume ratio be 5:95, while being stirred at room temperature 1 hour；Add the 50.0mM's of 1300 μ L
H2PtCl6The aqueous solution, in H2/N2Reacted 24 hours under mixed atmosphere, be centrifuged, wash, dry, obtain Pd@Pt/C
Catalyst.
The TEM figures of the Pd/C that Fig. 1 is used by embodiment one；Fig. 2 is the grain of corresponding Pd nano particles
Footpath distribution histogram.
Fig. 3 is the TEM figures of Pd@Pt/C prepared by embodiment one；Fig. 4 is corresponding Pd@Pt nano particles
Particle diameter distribution histogram.
Comparative example one：
1. 50mg XC-72 are taken in there-necked flask, add the mixing of 50.0mL deionized waters and ethanol
Solution, its reclaimed water is 3 with the volume ratio of ethanol:1；Stir and ultrasound is dispersed in the solution to XC-72.
2. it is the H of 100mL/min to flow velocity is passed through in above-mentioned solution2/N2Mixed gas, wherein H2With
N2Volume ratio be 5:95, while being stirred at room temperature 1 hour；Add the 50.0mM's of 1300 μ L
H2PtCl6The aqueous solution, in H2/N2Reacted 24 hours under mixed atmosphere, be centrifuged, wash, dry, obtain Pt/C
Catalyst.
Fig. 5 is the TEM figures of Pt/C prepared by comparative example one；Fig. 6 is the particle diameter of corresponding Pt nano particles
Distribution histogram.
Fig. 7 is respectively the Pd@Pt/C of the preparation of embodiment one, the Pd/C that is used with the preparation of comparative example one
Pt/C tests the cyclic voltammetry curve figure for obtaining by rotating disk electrode (r.d.e) (RDE)；Fig. 8 is respectively reality
The Pd@Pt/C and the Pt/C of the preparation of comparative example one for applying the preparation of example one are tested by rotating disk electrode (r.d.e) (RDE)
The polarization curves of oxygen reduction figure for obtaining.Cyclic voltammetry electrolyte is N2The 0.1mol/L HClO of saturation4
The aqueous solution, sweeps speed for 50mV/s.Polarization curves of oxygen reduction test electrolyte is O2The 0.1mol/L of saturation
HClO4The aqueous solution, sweeps speed for 10mV/s, and forward scan, RDE rotating speeds are 1600rpm.Test is in room
Carried out under temperature, metal load amount is 19 μ g/cm on electrode2。
Fig. 9 is that the Pt/C that Pd@Pt/C prepared by embodiment one are prepared with comparative example one is tested by half-cell
The hydrogen reduction catalytic quantity specific activity comparison diagram for obtaining.
Embodiment two：
1. 70mg Pd/C (BASF) are taken in there-necked flask, and wherein the mass fraction of Pd is 20%；
Add 50.0mL ethylene glycol；Stir and ultrasound is dispersed in the solution to Pd/C.
2. it is the H of 400mL/min to flow velocity is passed through in above-mentioned solution2/ Ar mixed gas, wherein H2With
The volume ratio of Ar is 50:50, while being stirred 0.5 hour at 100 DEG C；Add the 50.0mM of 2600 μ L
K2PtCl4The aqueous solution, in H2Reacted 1 hour under/Ar mixed atmospheres, be centrifuged, wash, dry, obtained
Pd@Pt-2/C catalyst.
The Pd@Pt-2/C that Figure 10 and Figure 11 is respectively the preparation of embodiment two pass through rotating disk electrode (r.d.e) (RDE)
Cyclic voltammetry curve and polarization curves of oxygen reduction that test is obtained.
Embodiment three：
1. 50mg Pd/C (BASF) are taken in there-necked flask, and wherein the mass fraction of Pd is 20%；
Add 50.0mL deionized waters；Stir and ultrasound is dispersed in the solution to Pd/C.
2. it is the H of 20mL/min to flow velocity is passed through in above-mentioned solution2/N2Mixed gas, wherein H2With Ar
Volume ratio be 90:10, while being stirred at room temperature 0.2 hour；Add the 50.0mM's of 1300 μ L
H2IrCl6The aqueous solution, in H2/N2Reacted 1 hour under mixed atmosphere, be centrifuged, wash, dry, obtain Pd@Ir/C
Catalyst.
Figure 12 is the TEM figures of Pd@Ir/C prepared by embodiment two；Figure 13 is corresponding Pd@Ir nanometers
The particle diameter distribution histogram of grain.
Example IV：
1. 50mg Rh/C are taken in there-necked flask, and wherein the mass fraction of Rh is 20%；Add 50.0
ML methyl alcohol；Stir and ultrasound is dispersed in methyl alcohol to Rh/C.
2. to being passed through H in above-mentioned solution2, while being stirred at room temperature 1 hour；Add 1300 μ L's
The K of 50.0mM2PtCl4The aqueous solution, in H2Reacted 24 hours under atmosphere, be centrifuged, wash, dry, obtained
To carbon-supported Rh@Pt/C catalyst.
The Rh@Pt/C that Figure 14 and Figure 15 is respectively the preparation of embodiment two pass through rotating disk electrode (r.d.e) (RDE)
Cyclic voltammetry curve and polarization curves of oxygen reduction that test is obtained.
Embodiment five：
1. 50mg Ir/C are taken in there-necked flask, and wherein the mass fraction of Ir is 20%；Add 50.0
ML ethylene glycol；Stir and ultrasound is dispersed in ethylene glycol to Ir/C.
2. to being passed through H in above-mentioned solution2, while being stirred at room temperature 1 hour；Add 1300 μ L's
50.0
The K of mM2PtCl4The aqueous solution, in H2Reacted 24 hours under atmosphere, be centrifuged, wash, dry,
Obtain Ir@Pt/C catalyst.
The Ir@Pt/C that Figure 16 and Figure 17 is respectively the preparation of embodiment two are surveyed in rotating disk electrode (r.d.e) (RDE)
Cyclic voltammetry curve and oxygen evolution reaction polarization curve in examination.Cyclic voltammetry electrolyte is N2Saturation
0.5mol/L H2SO4The aqueous solution, sweeps speed for 50mV/s, sweep limits 0-1.45V vs.RHE.Analysis oxygen
Reaction polarization curve test electrolyte is N2The 0.5mol/L H of saturation2SO4The aqueous solution, sweeps speed for 5mV/s,
Forward scan, RDE rotating speeds are 1600rpm.Test is carried out at room temperature, and metal load amount is on electrode
19μg/cm2。
Embodiment six：
1. Ni nano particles are prepared.50mL ethylene glycol solutions are taken in there-necked flask, 0.1M NiCl are added2
's
Ethylene glycol solution, makes Ni in solution2+Concentration is 1mM.Solution is stirred vigorously under the conditions of 120 DEG C,
Add the 50mM NaBH containing 5mM NaOH4Ethylene glycol solution, makes NaBH in final solution4Concentration be
8mM.Reaction 2 hours is stirred vigorously under the conditions of 120 DEG C, reaction solution is down to room temperature.
2. carbon-supported Ni@Pt nano particles are prepared.To being passed through H in above-mentioned solution2, while in room temperature
Under
Stirring 1 hour；Add the K of the 50.0mM of 1300 μ L2PtCl4The aqueous solution, in H2Under atmosphere
React 24 hours, add 40mg XC-72 activated carbon, ultrasound 1 hour is centrifuged, washs, does
It is dry, obtain Ni@Pt/C catalyst.
The Ni@Pt/C that Figure 18 and Figure 19 is respectively the preparation of embodiment three are surveyed in rotating disk electrode (r.d.e) (RDE)
Cyclic voltammetry curve and oxygen reduction reaction polarization curve in examination.
Claims (8)
1. a kind of preparation method of core shell structure elctro-catalyst, it is characterised in that comprise the following steps：
By loaded or non-supported metal M1 nano particles be distributed to water, organic solvent or the two
Among mixture, hydrogen is passed through, adds the soluble metallic salt of one or two or more kinds in platinum group metal,
React under a reducing atmosphere, be centrifuged, wash, surface that drying to obtain is loaded or non-supported is by platinum
The M1@M2 metal nanoparticles of the core shell structure of race's metallic cover.
2. preparation method according to claim 1, it is characterised in that：Metal M1 is that can adsorb hydrogen
One or two or more kinds in Mo, Rh, Pt, Ti, Co, Ni, Fe, Cr, Pd of gas.
3. preparation method according to claim 1, it is characterised in that：Organic solvent be methyl alcohol,
One or two or more kinds in ethanol, isopropanol, ethylene glycol, polyethylene glycol etc..
4. preparation method according to claim 1, it is characterised in that：Reaction temperature is 0-160 DEG C,
Reaction time is 0.1-24 hours；The purity of hydrogen is 1-100%, and remaining gas are in N2 and Ar
One or two or more kinds, flow velocity is 0.1-500mL min-1.
5. preparation method according to claim 1, it is characterised in that：Described platinum group metal M2
It is one or two or more kinds in Pt, Pd, Ir, Ru；Described platinum group metal precursor be Pt, Pd,
The sulfate of one or two or more kinds, nitrate, halide, halogen acids or halogen acid salt in Ir, Ru
In one or two or more kinds.
6. preparation method according to claim 1, it is characterised in that：It is loaded or non-supported
Metal M1 nano particles be scattered in mass concentration 0.1-10mg/mL in system.
7. the preparation method according to claim 1,5 or 6, it is characterised in that：Before platinum group metal
Mass concentration 0.1-10mg/mL of the body in system.
8. the preparation method according to claim 1 or 6, it is characterised in that：Loaded metal
M1 nano particles, carrier is the one kind or two in activated carbon, Graphene, CNT or metal nitride
More than kind, M1 load capacity is 1%-80%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109378492A (en) * | 2018-11-27 | 2019-02-22 | 上海交通大学 | Core-shell structure Pd@Pt/C or PdM@Pt/C catalyst and its preparation |
| CN109873175A (en) * | 2017-12-04 | 2019-06-11 | 中国科学院大连化学物理研究所 | A kind of low-temperature fuel cell supports the preparation method of platinum cobalt iridium alloy structure catalyst with nitridation three-dimensional carrier |
| CN114497603A (en) * | 2021-12-17 | 2022-05-13 | 深圳航天科技创新研究院 | Catalyst for fuel cell, preparation method thereof and fuel cell |
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| CN102500365A (en) * | 2011-10-19 | 2012-06-20 | 华南理工大学 | Preparation method of catalyst with core-shell structure for low-temperature fuel cell |
| CN103071486A (en) * | 2012-12-21 | 2013-05-01 | 江苏扬农化工集团有限公司 | Preparation method of palladium-platinum bimetallic catalyst |
| CN103111308A (en) * | 2013-03-05 | 2013-05-22 | 北京大学 | Method for directly synthesizing Pt-Co bimetallic nanoparticles utilizing water phase and application |
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2015
- 2015-11-27 CN CN201510863851.3A patent/CN106807365A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102500365A (en) * | 2011-10-19 | 2012-06-20 | 华南理工大学 | Preparation method of catalyst with core-shell structure for low-temperature fuel cell |
| CN103071486A (en) * | 2012-12-21 | 2013-05-01 | 江苏扬农化工集团有限公司 | Preparation method of palladium-platinum bimetallic catalyst |
| CN103111308A (en) * | 2013-03-05 | 2013-05-22 | 北京大学 | Method for directly synthesizing Pt-Co bimetallic nanoparticles utilizing water phase and application |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109873175A (en) * | 2017-12-04 | 2019-06-11 | 中国科学院大连化学物理研究所 | A kind of low-temperature fuel cell supports the preparation method of platinum cobalt iridium alloy structure catalyst with nitridation three-dimensional carrier |
| CN109873175B (en) * | 2017-12-04 | 2021-05-11 | 中国科学院大连化学物理研究所 | Preparation method of nitrided three-dimensional carrier supported platinum-cobalt-iridium alloy structure catalyst for low-temperature fuel cell |
| CN109378492A (en) * | 2018-11-27 | 2019-02-22 | 上海交通大学 | Core-shell structure Pd@Pt/C or PdM@Pt/C catalyst and its preparation |
| CN114497603A (en) * | 2021-12-17 | 2022-05-13 | 深圳航天科技创新研究院 | Catalyst for fuel cell, preparation method thereof and fuel cell |
| CN114497603B (en) * | 2021-12-17 | 2023-07-11 | 深圳航天科技创新研究院 | Catalyst for fuel cell, preparation method of catalyst and fuel cell |
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Application publication date: 20170609 |