CN104907068A - Method for preparing stepped Pt-Au core-shell structural catalyst - Google Patents

Method for preparing stepped Pt-Au core-shell structural catalyst Download PDF

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CN104907068A
CN104907068A CN201510285002.4A CN201510285002A CN104907068A CN 104907068 A CN104907068 A CN 104907068A CN 201510285002 A CN201510285002 A CN 201510285002A CN 104907068 A CN104907068 A CN 104907068A
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catalyst
electrode
core
stepped
ultra
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张生
许慧鑫
尹鸽平
周亚威
杜磊
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Harbin Institute of Technology
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    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

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Abstract

The present invention discloses a method for preparing a stepped Pt-Au core-shell structural catalyst, and the stepped single atomic shell Pt-Au core-shell structural catalyst can be prepared by two-step underpotential deposition and two-step nonuniformity chemical in-situ displacement. Compared with a Pt-Au alloy structure catalyst, the Pt utilization rate can be effectively improved by single Pt; compared with a conventional single-layer core-shell structure Pt catalyst, by the stepped surface structure, each Pt atom is adjacent to Au atoms, Au can play electronic effects; and Pt sites are blocked by the Au atoms, Au can also play the overall effect; compared with a conventional sub-monolayer shell structure Pt catalyst, the complete Pt layer surface structure can improve the stability of the catalyst. The method not only can achieve a high Pt shell atom utilization rate, and reduces toxic intermediate products, and the catalytic reaction is performed towards the most favorable path.

Description

A kind of preparation method of stepped Pt-Au catalyst with core-casing structure
Technical field
The present invention relates to a kind of preparation method of Pt-Au binary catalyst of the high Pt utilization rate for new catalytic type battery.
Background technology
Catalyst is the factor of restriction catalytic type battery performance most critical.In all eurypalynous catalyst, the catalytic activity of noble metal catalyst is wherein the most outstanding.In order to break through cost restriction, people are devoted to the catalyst studying low noble metal carrying capacity height catalytic efficiency always.Take noble metal as shell, the more cheap metal catalyst with core-casing structure that is core because of its efficient noble metal utilisation and the intermetallic electronic effect of allosome, get more and more people's extensive concerning.At present, prepare catalyst with core-casing structure mainly by chemical method, as colloid method, thermal decomposition method, chemical replacement method etc., these method preparation process are loaded down with trivial details, and the individual layer not easily realizing shell metallic covers, and are therefore difficult to realize the highest noble metal utilisation.In recent years, underpotential deposition method is adopted to be subject to the extensive favor of people in conjunction with the catalyst with core-casing structure that chemical original position displacement method prepares monatomic shell.
Summary of the invention
The object of this invention is to provide a kind of preparation method of stepped Pt-Au catalyst with core-casing structure, replaced by two step underpotential deposition methods and two step nonuniformities chemistry original position, gained Pt-Au nucleocapsid structure catalytic nanoparticles has stair-stepping surface topography.
The object of the invention is to be achieved through the following technical solutions:
A preparation method for stepped Pt-Au catalyst with core-casing structure, comprises the steps:
One, Au/C catalyst is prepared
The technology of Kaolinite Preparation of Catalyst mainly contains immersion reduction method, glycol method, colloid method, electrochemical process and Physical etc., and in the present invention, the preparation of Au/C is by immersion reduction method, and concrete steps are as follows:
(1) early-stage preparations: by 40mgXC-72R carbon black (this place can comprise the carrier materials such as all material with carbon elements such as CNT, Graphene and oxide) ultrasonic disperse 30min in ultra-pure water; Take sodium borohydride 19.22mg to be dissolved in the natrium citricum ice water solution of 0.508mL0.1mol/L.
(2) in 150mL ultra-pure water, first add the natrium citricum ultra-pure water solution 1.015mL of 0.1mol/L, stir; Then in solution, add the gold chloride ultra-pure water solution 4.335mL of 0.0117mol/L, stir; Add the sodium borohydride solution configured, stir 30min; Finally add the carbon black that dispersion treatment is good, ultrasonic process 5h.
(3) with the freeze drying of 2L ultra-pure water (being no less than 2L herein) filtering and washing final vacuum, Au/C catalyst is obtained.
Two, Au/C membrane electrode and electrode activation is prepared
The preparation of Au/C membrane electrode adopts conventional method, and concrete steps are as follows:
(1), before the preparation of catalyst rete electrode, catalyst slurry need be configured.A certain amount of catalyst fines is taken in reagent bottle with electronic balance, ultra-pure water and absolute ethyl alcohol (1:1) is added in reagent bottle, be configured to the slurries of 1mg/mL, in sonic oscillation machine, ultrasonic disperse 30min(catalyst slurry preparation herein also comprises with the dispersion of Nafion ethanolic solution).
(2) glass-carbon electrode needs to carry out pretreatment to its surface before the use.Select the Al of 50nm and 30nm successively 2o 3polishing powder, on polishing cloth, carry out polishing by the wetting action of ultra-pure water to electrode, carry out ultrasonic cleaning 10 ~ 20s after polishing completes in ultra-pure water, rear ultrapure water is clean.
(3) measure 7.5uL slurry drops in glassy carbon electrode surface with microlitre pipettor, allow slurries freely sprawl and naturally to dry; Backward electrode surface drips 5uL0.05mass%Nafion ethanolic solution, has namely prepared Au/C membrane electrode after naturally drying.
(4) experiment front activating is carried out, namely at 0.5M H to the Au/C membrane electrode prepared 2sO 4carry out cyclic voltammetry scan in solution, scanning potential range is that 0.05 ~ 1.7V(is all relative to RHE), sweep speed is 1 ~ 100mV/s, and the number of turns is 50 ~ 100.Activation completes in standard three electrode electrolyser, and working electrode is the glass-carbon electrode that load has catalyst, and auxiliary electrode is Pt sheet, and reference electrode is Hg/Hg 2sO 4electrode, involved electrode potential is all relative to RHE.
Three, first step underpotential deposition
First step underpotential deposition and follow-up second step underpotential deposition all complete in three electrode electrolysers, and working electrode is the glass-carbon electrode that load has catalyst, and auxiliary electrode is Pt silk, and reference electrode is Hg/Hg 2sO 4electrode, involved electrode potential is all relative to RHE.
(1) current potential of underpotential deposition is determined: the load activated in step 2 is had the glass-carbon electrode of catalyst rete at the saturated 10 ~ 50mMH of Ar gas 2sO 4+ 10 ~ 50mM CuSO 4in carry out cyclic voltammetry scan, scanning potential range is 0.302 ~ 1.2V, and sweep speed is arbitrary scan speed between 1 ~ 50mV/s.At 1.1 ~ 1.3V constant potential process, 120 ~ 720s after end.
(2) selecting 0.372 ~ 0.352V for stopping current potential, adopting 1 ~ 50 mV/s sweep speed to be that take-off potential carries out linear voltammetric scan with OCP, at termination current potential place potentiostatic electrodeposition 60 ~ 240s after terminating.
Four, first step chemistry original position displacement
First step chemical replacement is carried out under Ar atmosphere is enclosed, and concrete steps are as follows:
(1) glass-carbon electrode step 3 handled well transfers to 1 ~ 5mMHAuCl under Ar atmosphere is enclosed 4in the aqueous solution, carry out the chemical original position displacement reaction of 5 ~ 10min.
(2) rear taking-up electrode has been replaced, with ultra-pure water by clean for the liquid rinse of glassy carbon electrode surface remnants.
Five, second step underpotential deposition
The same step 3 of second step underpotential deposition step, that is:
(1) by the glass-carbon electrode for preparing in step 4 at the saturated 10 ~ 50mMH of Ar gas 2sO 4+ 10 ~ 50mM CuSO 4in carry out cyclic voltammetry scan, scanning potential range is 0.302 ~ 1.2V, and sweep speed is 1 ~ 50mV/s.At 1.1 ~ 1.3V constant potential process, 120 ~ 720s after end.
(2) selecting 0.372 ~ 0.352V for stopping current potential, adopting 1 ~ 50 mV/s sweep speed to be that take-off potential carries out linear voltammetric scan with OCP, at termination current potential place potentiostatic electrodeposition 60 ~ 240s after terminating.
Six, second step chemistry original position displacement
The displacement of second step chemistry original position is carried out under Ar atmosphere is enclosed, and concrete steps are as follows:
(1) glass-carbon electrode step 5 handled well transfers to the saturated 1 ~ 5mM H of Ar gas under Ar atmosphere is enclosed 2ptCl 4+ 10 ~ 50mMH 2sO 4in the aqueous solution, carry out the chemical original position displacement reaction of 5 ~ 10min.
(2) rear taking-up electrode has been replaced, with ultra-pure water, the liquid rinse of glassy carbon electrode surface remnants is clean, obtain the Pt-Au/C catalyst with core-casing structure with step-like surface structure.
Tool of the present invention has the following advantages:
1, compared with the catalyst of PtAu alloy structure, individual layer Pt effectively can improve the utilization rate of Pt.
2, compared with common Pt individual layer catalyst with core-casing structure, this stair-stepping surface texture not only makes each Pt atom adjacent with Au atom, and Au can play electronic effect; And Pt site is all intercepted by Au atom, Au can play group effect simultaneously.
3, compared with common subband structures Pt individual layer catalyst with core-casing structure, this complete Pt layer surface texture, makes the stability of catalyst get a promotion.
4, the present invention can be used for the utilization rate of raising Pt and improves catalyst CO tolerance catalysts performance and stability simultaneously.
5, the catalyst with core-casing structure with Au core and Pt shell that prepared by the method can be used for new catalytic type battery as in fuel cell (anode and cathode), lithium-air battery, to improve electro-chemical activity and stability.
6, the present invention adopts two step underpotential depositions and the displacement of two step nonuniformities chemistry original position to prepare the Pt-Au catalyst with core-casing structure of stepped monatomic shell, not only achieve the high usage of Pt shell atom, and decrease the generation of toxic intermediates, catalytic reaction is carried out towards best path.
Accompanying drawing explanation
Fig. 1 is experiment schematic diagram;
Fig. 2 is the Oxidation of Formic Acid curve (50mV/s of stepped Pt-Au/C and Pt/C; The 0.5MH that Ar is saturated 2sO 4+ 0.5MHCOOH);
Fig. 3 is mechanism figure (for catalytic oxidation formic acid molecule).
Detailed description of the invention
Below in conjunction with accompanying drawing, technical scheme of the present invention is further described; but be not limited thereto; everyly technical solution of the present invention modified or equivalent to replace, and not departing from the spirit and scope of technical solution of the present invention, all should be encompassed in protection scope of the present invention.
The invention provides a kind of preparation method of the stepped Pt-Au nucleocapsid structure anode catalyst for direct methanoic acid fuel cell, concrete implementation step is as follows:
One, Au/C catalyst is prepared:
The preparation of Au/C is by immersion reduction method, and concrete steps are as follows:
(1) early-stage preparations: by 40mgXC-72R carbon black ultrasonic disperse 30min in ultra-pure water; Take sodium borohydride 19.22mg to be dissolved in the natrium citricum ice water solution of 0.508mL, 0.1mol/L.
(2) in 150mL ultra-pure water, first add the natrium citricum ultra-pure water solution 1.015mL of 0.1mol/L, stir; Then in solution, add the gold chloride ultra-pure water solution 4.335mL of 0.0117mol/L, stir; Add sodium borohydride, stir 30min; Finally add carbon black, ultrasonic process 5h.
(3) with the freeze drying of 4L ultra-pure water filtering and washing final vacuum, Au/C catalyst is obtained.
Two, Au/C membrane electrode and electrode activation is prepared:
The preparation of Au/C membrane electrode adopts conventional method, and concrete steps are as follows:
(1), before the preparation of catalyst rete electrode, catalyst slurry need be configured.Take a certain amount of catalyst fines in reagent bottle with electronic balance, in reagent bottle, add ultra-pure water and absolute ethyl alcohol (1:1), be configured to the slurries of 1mg/mL, ultrasonic disperse 30min in sonic oscillation machine.
(2) glass-carbon electrode needs to carry out pretreatment to its surface before the use.Select the Al of 50nm and 30nm successively 2o 3polishing powder, on polishing cloth, carry out polishing by the wetting action of ultra-pure water to electrode, carry out ultrasonic cleaning 20s after polishing completes in ultra-pure water, rear ultrapure water is clean.
(3) measure 7.5uL slurry drops in glassy carbon electrode surface with microlitre pipettor, allow slurries freely sprawl and naturally to dry; Backward electrode surface drips 5uL, 0.05mass%Nafion ethanolic solution, has namely prepared Au/C membrane electrode after naturally drying.
(4) experiment front activating is carried out, namely at 0.5M H to the Au/C membrane electrode prepared 2sO 4carry out cyclic voltammetry scan in solution, scanning potential range is that 0.05V ~ 1.7V(is all relative to RHE), sweep speed is 50mV/s, and the number of turns is 50.Activation completes in standard three electrode electrolyser, and working electrode is the glass-carbon electrode that load has catalyst, and auxiliary electrode is Pt sheet, and reference electrode is Hg/Hg 2sO 4electrode, involved electrode potential is all relative to RHE.
Three, first step underpotential deposition
First step underpotential deposition and follow-up second step underpotential deposition all complete in three electrode electrolysers, and working electrode is the glass-carbon electrode that load has catalyst, and auxiliary electrode is Pt silk, and reference electrode is Hg/Hg 2sO 4electrode, involved electrode potential is all relative to RHE.
(1) current potential of underpotential deposition is determined: the load prepared in step 2 is had the glass-carbon electrode of catalyst rete at the saturated 50mM H of Ar gas 2sO 4+ 50mM CuSO 4in carry out cyclic voltammetry scan, scanning potential range is 0.302V ~ 1.2V, and sweep speed is 50mV/s.At 1.2V constant potential process 240s after end.
(2) select 0.352V for stopping current potential, the speed of sweeping adopting 1mV/s is that take-off potential carries out linear voltammetric scan with OCP, and at termination current potential 0.352V place potentiostatic electrodeposition 60s.
Four, first step chemistry original position displacement
First step chemical replacement is carried out under Ar atmosphere is enclosed.
(1) glass-carbon electrode step 3 handled well transfers to 1mM HAuCl under Ar atmosphere is enclosed 4in the aqueous solution, carry out the chemical original position displacement reaction of 10min.Chemistry original position displacement reaction is:
3Cu+2Au 3+→2Au+3Cu 2+。
(2) rear taking-up electrode has been replaced, with ultra-pure water by clean for the liquid rinse of glassy carbon electrode surface remnants.
Five, second step underpotential deposition
The same step 3 of second step underpotential deposition step.
Six, second step chemistry original position displacement
The displacement of second step chemistry original position is carried out under Ar atmosphere is enclosed.
(1) glass-carbon electrode step 5 handled well transfers to the saturated 1mM H of Ar gas under Ar atmosphere is enclosed 2ptCl 4+ 50mM H 2sO 4in the aqueous solution, carry out the chemical original position displacement reaction of 10min.Chemistry original position displacement reaction is:
Cu+Pt 2+→Pt+Cu 2+。
(2) rear taking-up electrode has been replaced, with ultra-pure water by clean for the liquid rinse of glassy carbon electrode surface remnants.
(3) prepared by the Pt-Au/C catalyst with core-casing structure so far, with step-like surface structure.
The preparation process simulation drawing of catalyst is as shown in Figure 1 known, and the present invention gets stepped Pt-Au catalyst with core-casing structure in return by two step underpotential deposition methods and two step nonuniformities chemistry original position.
Fig. 2 is that prepared stepped Pt-Au/C catalyst with core-casing structure is at 0.5M H 2sO 4cyclic voltammetry curve in+0.5M HCOOH, i.e. Oxidation of Formic Acid curve, and contrast with common Pt/C, sweep speed and be 50mV/s.In figure, stepped Pt-Au/C catalyst with core-casing structure is 0.0079A/cm at the direct oxidation pathway peak current density at 0.5V place 2, be 5 times of Pt/C; It is starkly lower than Pt/C at the indirect oxidation approach peak at 0.95V place.Can illustrate that this stepped Pt-Au catalyst with core-casing structure not only has excellent area specific activity, effectively can also avoid the generation of toxic intermediates.
Fig. 3 is the Analysis on Mechanism figure of prepared stepped Pt-Au/C catalyst with core-casing structure catalysis Oxidation of Formic Acid.Each Pt atom is adjacent with Au atom on the one hand, and Au can play electronic effect, makes catalyst possess high area specific activity; On the other hand, Pt site is all intercepted by Au atom, and Au can play group effect simultaneously, thus reduces the generation of toxic intermediates CO.

Claims (5)

1. a preparation method for stepped Pt-Au catalyst with core-casing structure, is characterized in that described method step is as follows:
One, Au/C membrane electrode activation
Experiment front activating is carried out to Au/C membrane electrode, namely at 0.5M H 2sO 4carry out cyclic voltammetry scan in solution, scanning potential range is 0.05 ~ 1.7V, and sweep speed is 1 ~ 100mV/s, and the number of turns is 50 ~ 100;
Two, first step underpotential deposition
(1) current potential of underpotential deposition is determined: the load activated is had the glass-carbon electrode of Au/C catalyst rete at the saturated 10 ~ 50mMH of Ar gas 2sO 4+ 10 ~ 50mM CuSO 4in carry out cyclic voltammetry scan, scanning potential range is 0.302 ~ 1.2V, and sweep speed is 1 ~ 50mV/s, at 1.1 ~ 1.3V constant potential process, 120 ~ 720s after terminating;
(2) selecting 0.372 ~ 0.352V for stopping current potential, adopting 1 ~ 50 mV/s sweep speed to be that take-off potential carries out linear voltammetric scan with OCP, at termination current potential place potentiostatic electrodeposition 60 ~ 240s after terminating;
Three, first step chemistry original position displacement
(1) glass-carbon electrode step 2 handled well transfers to 1 ~ 5mMHAuCl under Ar atmosphere is enclosed 4in the aqueous solution, carry out the chemical original position displacement reaction of 5 ~ 10min;
(2) rear taking-up electrode has been replaced, with ultra-pure water by clean for the liquid rinse of glassy carbon electrode surface remnants;
Four, second step underpotential deposition
(1) by the glass-carbon electrode for preparing in step 3 at the saturated 10 ~ 50mMH of Ar gas 2sO 4+ 10 ~ 50mM CuSO 4in carry out cyclic voltammetry scan, scanning potential range is 0.302 ~ 1.2V, and sweep speed is 1 ~ 50mV/s, at 1.1 ~ 1.3V constant potential process, 120 ~ 720s after terminating;
(2) selecting 0.372 ~ 0.352V for stopping current potential, adopting 1 ~ 50 mV/s sweep speed to be that take-off potential carries out linear voltammetric scan with OCP, at termination current potential place potentiostatic electrodeposition 60 ~ 240s after terminating;
Five, second step chemistry original position displacement
(1) glass-carbon electrode step 4 handled well transfers to the saturated 1 ~ 5mM H of Ar gas under Ar atmosphere is enclosed 2ptCl 4+ 10 ~ 50mMH 2sO 4in the aqueous solution, carry out the chemical original position displacement reaction of 5 ~ 10min;
(2) rear taking-up electrode has been replaced, with ultra-pure water, the liquid rinse of glassy carbon electrode surface remnants is clean, obtain the Pt-Au/C catalyst with core-casing structure with step-like surface structure.
2. the preparation method of stepped Pt-Au catalyst with core-casing structure according to claim 1, it is characterized in that the activation of described Au/C membrane electrode completes in standard three electrode electrolyser, working electrode is the glass-carbon electrode that load has Au/C catalyst, auxiliary electrode is Pt sheet, and reference electrode is Hg/Hg 2sO 4electrode, involved electrode potential is all relative to RHE.
3. the preparation method of stepped Pt-Au catalyst with core-casing structure according to claim 1, is characterized in that described Au/C membrane electrode is prepared from accordance with the following methods:
(1) take a certain amount of Au/C catalyst fines in reagent bottle with electronic balance, in reagent bottle, add ultra-pure water and absolute ethyl alcohol, be configured to the slurries of 1mg/mL, ultrasonic disperse 30min in sonic oscillation machine;
(2) Al of 50nm and 30nm is selected successively 2o 3polishing powder, on polishing cloth, carry out polishing by the wetting action of ultra-pure water to electrode, carry out ultrasonic cleaning 10 ~ 20s after polishing completes in ultra-pure water, rear ultrapure water is clean;
(3) measure 7.5uL slurry drops in glassy carbon electrode surface with microlitre pipettor, allow slurries freely sprawl and naturally to dry; Backward electrode surface drips 5uL, 0.05mass%Nafion ethanolic solution, has namely prepared Au/C membrane electrode after naturally drying.
4. the preparation method of stepped Pt-Au catalyst with core-casing structure according to claim 3, is characterized in that the volume ratio of described ultra-pure water and absolute ethyl alcohol is 1:1.
5. the preparation method of stepped Pt-Au catalyst with core-casing structure according to claim 3, is characterized in that described Au/C catalyst is prepared from by immersion reduction method.
CN201510285002.4A 2015-05-29 2015-05-29 Method for preparing stepped Pt-Au core-shell structural catalyst Pending CN104907068A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106935873A (en) * 2017-04-13 2017-07-07 中国科学院长春应用化学研究所 A kind of platinum cladding gold nanocrystals material and its preparation method and application
CN109225257A (en) * 2018-10-16 2019-01-18 中国科学技术大学先进技术研究院 A kind of monatomic catalyst of support type and preparation method thereof
CN112510220A (en) * 2020-11-19 2021-03-16 武汉大学 Core-shell type platinum-based alloy electrocatalyst with high oxygen reduction performance and preparation method thereof
CN114689651A (en) * 2020-12-31 2022-07-01 长城汽车股份有限公司 Nitrogen-oxygen sensor, nitrogen oxide measuring method and vehicle

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106935873A (en) * 2017-04-13 2017-07-07 中国科学院长春应用化学研究所 A kind of platinum cladding gold nanocrystals material and its preparation method and application
CN106935873B (en) * 2017-04-13 2019-09-13 中国科学院长春应用化学研究所 A kind of platinum cladding gold nanocrystals material and its preparation method and application
CN109225257A (en) * 2018-10-16 2019-01-18 中国科学技术大学先进技术研究院 A kind of monatomic catalyst of support type and preparation method thereof
CN109225257B (en) * 2018-10-16 2021-07-27 中国科学技术大学先进技术研究院 Supported monatomic catalyst and preparation method thereof
CN112510220A (en) * 2020-11-19 2021-03-16 武汉大学 Core-shell type platinum-based alloy electrocatalyst with high oxygen reduction performance and preparation method thereof
CN112510220B (en) * 2020-11-19 2022-02-01 武汉大学 Core-shell type platinum-based alloy electrocatalyst with high oxygen reduction performance and preparation method thereof
CN114689651A (en) * 2020-12-31 2022-07-01 长城汽车股份有限公司 Nitrogen-oxygen sensor, nitrogen oxide measuring method and vehicle

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Application publication date: 20150916