CN101337184A - Composite electrocatalyst capable of increasing cathode mass-transfer performance of fuel cell - Google Patents

Composite electrocatalyst capable of increasing cathode mass-transfer performance of fuel cell Download PDF

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CN101337184A
CN101337184A CNA2008100417391A CN200810041739A CN101337184A CN 101337184 A CN101337184 A CN 101337184A CN A2008100417391 A CNA2008100417391 A CN A2008100417391A CN 200810041739 A CN200810041739 A CN 200810041739A CN 101337184 A CN101337184 A CN 101337184A
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fuel cell
preparation
presoma
transfer performance
composite electrocatalyst
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CN101337184B (en
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林瑞
马建新
李冰
王晓蕾
杨代军
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Tongji University
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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
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    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

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Abstract

The invention discloses a Pt-Ce-M-O/C complex electrocatalyst which can improve the cathode mass transfer performance of a fuel cell, and the preparation method thereof. Aiming at the phenomena that the cathode of the fuel cell adopts air as the oxygen source, and the diffusion, the transfer and the reduction of oxygen influence the performance of the fuel cell, the invention provides a novel solution. The complex electrocatalyst comprises carriers, active ingredients and an auxiliary agent, wherein, the carriers adopt black carbon materials including acetylene black, Vulcan XC-72, Ketjen black, graphite nano-fiber, carbon nano-horn, carbon nano-zeolite, etc.; the precursors of the active ingredients and the auxiliary agent are respectively soluble salts of Pt, Ce and M (M is composed of more than one element from Zr, Y and rare earth elements). The Pt-Ce-M-O/C complex electrocatalyst of the invention is obtained by adopting the single-step precipitation method, and is characterized by simple preparation method, small catalyst particle size, high thermal stability, etc. The complex electrocatalyst is applied to the improvement of the cathode mass transfer performance of the fuel cell, and the fuel cell has higher discharge performance under high current density.

Description

Improve the composite electrocatalyst and the preparation method of cathode mass-transfer performance of fuel cell
Technical field
The invention belongs to catalysis and fuel cell technology field, relate to the technology that improves fuel battery negative pole oxygen enrichment ability, thereby particularly a kind ofly improve Pt-Ce-M-O/C composite electrocatalyst and the preparation method that fuel battery negative pole oxygen enrichment ability is improved cathode mass-transfer performance.
Technical background
Fuel-cell catalyst is the key components of fuel cell membrane electrode assembly, and its performance and characteristic directly determine fuel cell performance.At present, existing fuel-cell catalyst adopts Pt/C or Pt-M/C (M is a transition metal) catalyst mostly, and relevant in recent years Pt-M/C catalyst has many reports.The Pt-M/C catalyst is that other transition metal is mixed on the basis with Pt/C, forms binary or multicomponent reactive component catalyst.Some researchers think that the adding of M (transition metal) can prevent the precious metals pt particle aggregation, improve the stability of catalyst.
In view of fuel battery negative pole generally adopts air is the oxygen source of supply, and lower partial pressure of oxygen has limited the performance of negative electrode.And carrying out with reaction, especially under high current density, inert gases (nitrogen) a large amount of in the air are trapped in the Catalytic Layer, hindered the diffusion of oxygen to Catalytic Layer, influenced the reduction of oxygen, because the reduction (ORR) of negative electrode oxygen is that the rate determining step of cell reaction is rapid, therefore seek more appropriate catalyst and preparation method, be to improve the effective means of battery performance with mass transfer amount that improves negative electrode oxygen or the storage capacity that increases oxygen.
CeO 2Be the good auxiliary agent of oxidation catalyst, have the ability of higher storage and release oxygen, pass through Ce 4+/ Ce 3+Carry out redox reaction, thereby under different atmosphere, play the effect of oxygen supply conditioning agent.CeO 2The middle Zr that adds, Y and La, rare earth elements such as Pr can form cerium-based composite oxides (Ce-M-O), play and improve CeO 2Storage and discharge oxygen and the effect of heat endurance.Because the Ce-M-O composite oxides have excellent storage and discharge the performance of oxygen, Pt combines with the Ce-M-O composite oxides and produces synergy, can increase the oxygen-supplying amount of negative electrode, promote the transmission of oxygen, so the mass-transfer performance of fuel battery negative pole oxygen increase to Catalytic Layer.Especially battery moves under high current density, and is big to the demand of oxygen, so the interpolation of Ce-M-O is more obvious to the raising effect of battery performance.Employing Ce-M-O is an auxiliary agent, and preparation Pt-Ce-M-O/C catalyst and the research that is applied to fuel cell is report as yet at present, and the preparation method is simple, and lower and chemical property of cost and heat endurance all increase.
Summary of the invention
The cathodic oxygen reduction performance is subjected to the oxygen diffusion-restricted and influences the deficiency of fuel battery performance when the objective of the invention is to be used for fuel cell in view of existing P t/C catalyst, and a kind of Pt-Ce-M-O/C composite electrocatalyst and preparation method of simple, novel raising cathode mass-transfer performance of fuel cell is provided.The catalyst for preparing has the characteristic that particle is little, heat endurance is high, chemical property is excellent.
A kind of preparation method who improves the composite electrocatalyst of cathode mass-transfer performance of fuel cell of the present invention is: the carbon black support of a certain amount of (500mg) is uniformly dispersed into suspension with solvent, then add a certain proportion of Pt that has mixed, (M is Zr for Ce, M, more than one elements in Y and the rare earth element) presoma reduces with reducing agent again.Wherein to account for the mass ratio of C be 20%～60% to Pt, and it is 0～20% that Ce-M accounts for the Pt mol ratio.
Wherein: the active constituent presoma comprises chloroplatinic acid, platinum nitrate etc.; The auxiliary agent presoma comprises the nitrate of Ce and M; Also may comprise oxide, carbonate etc.;
Reducing agent is the solvent of reproducibilities such as ethylene glycol, glycerine, formaldehyde, acetaldehyde, sodium borohydride.Control reaction pH value, reaction temperature and the reaction time.After reacting completely,, through the uniform temperature reduction, can obtain the Pt-Ce-M-O/C composite electrocatalyst again with product filtration, washing, vacuum drying.
This Preparation of catalysts step comprises:
(1), carrier is uniformly dispersed is configured to suspension, suspension one; Pt, Ce, M presoma are mixed.
(2), (1) resulting precursor mixture and suspension one is mixed, mixture two, with reducing agent mixture two is reduced again, the pH value in the control course of reaction is 8-12, reaction temperature is 40～150 ℃, the reaction time is 2～5 hours; Filter then, sediment, to sediment wash, vacuum drying.
(3), the sediment after vacuum drying in (2) is reduced through 80～600 ℃ of temperature, can make the Pt-Ce-M-O/C catalyst; Here adopting hydrogen-nitrogen of 5% is reducing agent.
A kind of composite electrocatalyst that improves cathode mass-transfer performance of fuel cell of described preparation has following advantage:
(a), the preparation method is simple: one step of presoma of Pt, Ce, M joins in the carbon carrier and can make, and " step adding " embodied this point;
(b), the catalyst system novelty, the Pt-Ce-M-O/C catalyst did not have report;
(c), the Pt-Ce-M-O/C catalyst can improve cathode mass-transfer performance of fuel cell and improve fuel cell performance as cathod catalyst;
(d), catalyst has that particle diameter is little, heat endurance is high.
Description of drawings
Fig. 1 is H 2The original position XRD spectra of Pt-Ce-La-O/C catalyst under the atmosphere.
Fig. 2 is the TEM spectrogram of Pt-Ce-La-O/C catalyst.
The specific embodiment
Below by example in detail the present invention is described in detail, but the present invention is not limited to these embodiment.
Embodiment 1
Preparation Pt-Ce-La-O/C catalyst (Pt: Ce: the La mol ratio is 20: 1: 1): the Vulcan XC-72R carbon black that takes by weighing 500mg adds ethylene glycol solution, fully stirs.Add pre-configured Pt, Ce, La mixed solution, wherein the presoma of Pt, Ce and La adopts chloroplatinic acid respectively, and the mass percent that cerous nitrate and lanthanum nitrate, Pt account for C is 40%.Drip ethylene glycol solution in above-mentioned solution, control pH value is about 10, and reaction temperature is 150 ℃, and the reaction time is 3 hours.After question response is complete, cool off, be filtered to no Cl -Deng impurity.After the vacuum drying, characterize the heat endurance of Pt-Ce-La-O/C catalyst by original position XRD.Respectively through 30,80,200,300,400,500 and 600 ℃ of in-situ reducing, after each temperature spot stops half an hour, the analysis of catalyst particle size is with the variation (Fig. 1) of reduction temperature, and the grain size of Pt-Ce-La-O/C catalyst under relevant temperature is respectively 4.8,4.9,5.7,6.1,6.8,8.7 and 11.0nm.
Embodiment 2
Change the Pt among the embodiment 1: Ce: La mol ratio, preparation Pt-Ce-La-O/C (Pt: Ce: the La mol ratio is 100: 5: 1) catalyst.Detailed preparation process is as follows: the Vulcan XC-72R carbon black that takes by weighing 500mg adds ethylene glycol solution, fully stirs.Add pre-configured Pt, Ce, La mixed solution, wherein the presoma of Pt, Ce and La adopts chloroplatinic acid respectively, and the mass percent that cerous nitrate and lanthanum nitrate, Pt account for C is 40%.Drip ethylene glycol solution in above-mentioned solution, control pH value is about 10, and reaction temperature is 150 ℃, and the reaction time is 3 hours.After question response is complete, cool off, be filtered to no Cl -Deng impurity.After the vacuum drying, the microscopic appearance of catalyst characterizes by transmission electron microscope (TEM).Fig. 2 is the TEM photo of the Pt-Ce-La-O/C eelctro-catalyst for preparing, amplifies 80,000 times.As seen from the figure, the size of Pt particle evenly disperses better not reunite substantially, and particle mean size is 4.5nm.
Embodiment 3
Change the reaction temperature among the embodiment 1, preparation Pt-Ce-La-O/C (Pt: Ce: the La mol ratio is 20: 1: 1) catalyst.Detailed preparation process is as follows: the Vulcan XC-72R carbon black that takes by weighing 500mg adds ethylene glycol solution, fully stirs.Add pre-configured Pt, Ce, La mixed solution, wherein the presoma of Pt, Ce and La adopts chloroplatinic acid respectively, and the mass percent that cerous nitrate and lanthanum nitrate, Pt account for C is 40%.Drip ethylene glycol solution in above-mentioned solution, control pH value is about 10, and reaction temperature is 80 ℃, and the reaction time is 3 hours.After question response is complete, cool off, be filtered to no Cl -Deng impurity.After the vacuum drying, it is 4.2nm that the microscopic appearance of catalyst is observed Pt particle average grain diameter by transmission electron microscope (TEM).
Embodiment 4:
Change the carbon carrier among the embodiment 1, preparation Pt-Ce-La-O/C catalyst (Pt: Ce: the La mol ratio is 20: 1: 1): take by weighing the 500mg Graphite Nano Fiber and add ethylene glycol solution, fully stirred 1 hour.Add pre-configured Pt, Ce, La mixed solution, wherein the presoma of Pt, Ce and La adopts platinum nitrate respectively, and the mass percent that cerous nitrate and lanthanum nitrate, Pt account for C is 40%.Drip ethylene glycol solution in above-mentioned solution, control pH value is about 10, and reaction temperature is 150 ℃, and the reaction time is 3 hours.After question response is complete, cool off, be filtered to no Cl -Deng impurity.After the vacuum drying, observing Pt particle average grain diameter by transmission electron microscope (TEM) is 5.2nm.
Embodiment 5:
Change the reducing agent among the embodiment 1, the detailed preparation process of Pt-Ce-La-O/C catalyst (Pt: Ce: the La mol ratio is 20: 1: 1): take by weighing 500mg Vulcan XC-72R carbon black, add glycerine solution, fully stirred 1 hour.Add pre-configured Pt, Ce, La mixed solution, wherein the presoma of Pt, Ce and La adopts platinum nitrate respectively, and the mass percent that cerous nitrate and lanthanum nitrate, Pt account for C is 40%.Drip excessive glycerine solution in above-mentioned solution, control pH value is about 8, and reaction temperature is 150 ℃, and the reaction time is 3 hours.After question response is complete, cool off, be filtered to no Cl -Deng impurity.After the vacuum drying, observing Pt particle average grain diameter by transmission electron microscope (TEM) is 4.5nm.
Embodiment 6:
Change the reducing agent among the embodiment 1, the detailed preparation process of Pt-Ce-La-O/C catalyst (Pt: Ce: the La mol ratio is 20: 1: 1): add pre-configured Pt, Ce, La mixed solution, wherein the presoma of Pt, Ce and La adopts platinum nitrate respectively, the mass percent that cerous nitrate and lanthanum nitrate, Pt account for C is 40%.Drip excessive formalin in above-mentioned solution, control pH value is about 8, and reaction temperature is 150 ℃, and the reaction time is 3 hours.After question response is complete, cool off, be filtered to no Cl -Deng impurity.After the vacuum drying, observing Pt particle average grain diameter by transmission electron microscope (TEM) is 5.2nm.
Embodiment 7:
The detailed preparation process of Pt/C catalyst: take by weighing 500mg Vulcan XC-72R carbon black, add ethylene glycol solution, fully stirred 1 hour.Add platinum nitrate, the mass percent that Pt accounts for C is 40%.Drip excessive ethylene glycol solution in above-mentioned solution, control pH value is about 8, and reaction temperature is 150 ℃, and the reaction time is 5 hours.After question response is complete, cool off, be filtered to no Cl -Deng impurity.After the vacuum drying, heat endurance by original position XRD performance characterization Pt/C catalyst, respectively through 30,80,200,300,400,500 and 600 ℃ of in-situ reducing, after each temperature spot stops half an hour, carry out the variation of original position XRD material phase analysis catalyst particle size size, the Pt/C grain size is respectively 3.8,4.2,5.9,6.9,7.4,8.1 and 13.4nm.Comparing embodiment 1 and embodiment 7, as seen with the raising of reduction temperature, Pt-Ce-La-O/C is little than the growth of Pt/C catalyst particle size, has higher heat endurance, and handles the synergy that can strengthen between Pt and Ce, the La at high temperature.
Embodiment 8:
The detailed preparation process of Pt-Ce-Zr-O/C catalyst: the Vulcan XC-72R carbon black that takes by weighing 500mg adds ethylene glycol solution, fully stirs.Add pre-configured Pt, Ce and the mixed solution of Zr (Pt: Ce: the Zr molar concentration rate is 20: 1: 1), wherein the presoma of Pt, Ce and Zr adopts platinum nitrate, cerous nitrate and zirconium nitrate, and the mass percent that Pt accounts for C is 40%.Drip ethylene glycol solution in above-mentioned solution, control pH value is about 10, and reaction temperature is 150 ℃, and the reaction time is 3 hours.After question response is complete, cool off, be filtered to no Cl -Deng impurity.After the vacuum drying, observing Pt particle average grain diameter by transmission electron microscope (TEM) is 4.5nm.
Embodiment 9:
The detailed preparation process of Pt-Ce-Y-O/C catalyst: the Vulcan XC-72R carbon black that takes by weighing 500mg adds ethylene glycol solution, fully stirs.Add pre-configured Pt, Ce and the mixed solution of Y, wherein the presoma of Pt, Ce and Y adopts platinum nitrate, cerous nitrate and yttrium nitrate.Pt: Ce: the Y molar concentration rate is 20: 1: 1, and the mass percent that Pt accounts for C is 40%.Drip ethylene glycol solution in above-mentioned solution, control pH value is about 10, and reaction temperature is 150 ℃, and the reaction time is 3 hours.After question response is complete, cool off, be filtered to no Cl -Deng impurity.After the vacuum drying, observing Pt particle average grain diameter by transmission electron microscope (TEM) is 4.0nm.The Pt-Ce-Y-O/C catalyst is used to prepare membrane electrode cathode, and wherein the carrying capacity of anode and cathode Pt respectively is 0.4mg/cm 2,, under constant current (20A) pattern, carry out by electrochemical impedance (EIS) test.After adding Ce-Y-O in the Pt catalyst, the ohmage of fuel cell increases to some extent, but greatly reduces in the impedance of low frequency range mass transfer, and visible Ce-Y-O is added with enrichment and the transmission that is beneficial to oxygen.
Embodiment 10:
The detailed preparation process of Pt-Ce-Pr-O/C catalyst: the Vulcan XC-72R carbon black that takes by weighing 500mg adds ethylene glycol solution, fully stirs.Add pre-configured Pt, Ce and the mixed solution of Pr, wherein the presoma of Pt, Ce and Pr adopts platinum nitrate, cerous nitrate and praseodymium nitrate.Pt: Ce: the Pr molar concentration rate is 20: 1: 1, and the mass percent that Pt accounts for C is 40%.Drip ethylene glycol solution in above-mentioned solution, control pH value is about 10, and reaction temperature is 150 ℃, and the reaction time is 3 hours.After question response is complete, cool off, be filtered to no Cl -Deng impurity.After the vacuum drying, observing Pt particle average grain diameter by transmission electron microscope (TEM) is 5.0nm
Embodiment 11:
The electrochemical properties of Pt/C, Pt-Ce-Zr-O/C, Pt-Ce-Y-O/C, Pt-Ce-La-O/C and Pt-Ce-Pr-O/C eelctro-catalyst carries out performance test by being prepared into monocell.Specific as follows: as to get a certain amount of Pt/C, Pt-Ce-Zr-O/C, Pt-Ce-Y-O/C, Pt-Ce-La-O/C and Pt-Ce-Pr-O/C eelctro-catalyst, mix sonic oscillation 15min with deionized water, isopropyl alcohol; Add a certain amount of Nafion solution again, continue sonic oscillation 15min, be sprayed on equably on the Nafion film, obtain membrane electrode MEA.MEA is assembled into monocell, and the effective area of monocell is 50cm 2, the fuel at negative and positive the two poles of the earth is respectively air and hydrogen, and utilization rate is respectively 40% and 70%, and the humidification degree is 100%, and wherein the carrying capacity of anode and cathode Pt respectively is 0.4mg/cm 2(＜200mA/cm under low current density 2), the discharge performance of the fuel cell that the discharge performance of the fuel cell that employing Pt/C Preparation of Catalyst obtains makes than adopting Pt-Ce-Zr-O/C, Pt-Ce-Y-O/C, Pt-Ce-La-O/C and Pt-Ce-Pr-O/C catalyst is high slightly, at 200mA/cm 2, the discharge voltage of these catalyst is respectively 0.80,0.76,0.78,0.75 and 0.72V; But along with the increase of current density, catalyst series is at 800mA/cm 2Under the current density, discharge voltage is respectively 0.50,0.56,0.59,0.57 and 0.52V, and wherein the discharge performance with Pt-Ce-Y-O/C is the highest.
The present invention adds rare earth elements such as Ce, M in Pt; Add two kinds of rare earth elements simultaneously; One step is directly synthetic.
As can be seen, Pt-Ce-M-O/C composite catalyst preparation technology of the present invention is simple from the above embodiments, Pt, and Ce, the presoma of M and carrier can make required catalyst through single step reaction; The catalyst system novelty, the Pt-Ce-M-O/C catalyst did not have report; The catalyst particle size for preparing is less, the heat endurance height; Catalyst of the present invention is used for fuel battery negative pole, and cell cathode mass transfer ability is improved, and battery performance improves.
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.The person skilled in the art obviously can easily make various modifications to these embodiment, and needn't pass through performing creative labour being applied in the General Principle of this explanation among other embodiment.Therefore, the invention is not restricted to the embodiment here, those skilled in the art should be within protection scope of the present invention for improvement and modification that the present invention makes according to announcement of the present invention.

Claims (7)

1, a kind of composite electrocatalyst that improves cathode mass-transfer performance of fuel cell, it is characterized in that: composite electrocatalyst comprises C carrier, auxiliary agent and active component; Wherein:
(1), the C carrier is carbon black material, comprises that acetylene black, Vulcan XC-72, Ketjen are black, Graphite Nano Fiber, carbon nanohorn, carbon nano molecular;
(2), auxiliary agent comprises the oxide of Ce, M; Wherein M is Zr, more than one elements in Y and the rare earth element;
(3), active component comprises Pt, solubility Pt.
2, the preparation method of the composite electrocatalyst of raising cathode mass-transfer performance of fuel cell according to claim 1, it is characterized in that: active constituent presoma and one step of auxiliary agent presoma are joined in the carrier, through reducing agent reduction, precipitation, filtration, washing, make catalyst.
3, the preparation method of the composite electrocatalyst of raising cathode mass-transfer performance of fuel cell according to claim 2 is characterized in that: wherein
(1), the active constituent presoma comprises chloroplatinic acid, platinum nitrate; (2), the auxiliary agent presoma comprises and the nitrate of Ce and M also comprises oxide, carbonate; (3), reducing agent comprises ethylene glycol, glycerine, formaldehyde, acetaldehyde and sodium borohydride.
4, the preparation method of the composite electrocatalyst of raising cathode mass-transfer performance of fuel cell according to claim 2 is characterized in that: this Preparation of catalysts step comprises:
(1), carbon black support is uniformly dispersed is configured to suspension one;
(2), a certain proportion of active constituent presoma and auxiliary agent presoma are mixed precursor mixture one;
(3), suspension one and precursor mixture one mixed, again with the reducing agent reduction, filter then sediment, again to sediment wash, vacuum drying, dry sediment;
(4), the sediment of drying is reduced through uniform temperature, promptly make the Pt-Ce-M-O/C composite electrocatalyst.
5, the preparation method of the composite electrocatalyst of raising cathode mass-transfer performance of fuel cell according to claim 4, it is characterized in that: to account for the mass ratio of carbon black support be 20%～60% to the active component presoma in the step (2), and the auxiliary agent presoma is that the mol ratio that accounts for the active constituent presoma is 0～20%.
6, the preparation method of the composite electrocatalyst of raising cathode mass-transfer performance of fuel cell according to claim 4, it is characterized in that: the pH value in the step (3) in the control course of reaction is 8-12, reaction temperature is 40～150 ℃, and the reaction time is 2～5 hours, filter then sediment; " uniform temperature " is meant 80～600 ℃ described in the step (4).
7, the preparation method of the composite electrocatalyst of raising cathode mass-transfer performance of fuel cell according to claim 4 is characterized in that: the hydrogen-nitrogen of employing 5% is reducing agent in the step (4).
CN2008100417391A 2008-08-15 2008-08-15 Composite electrocatalyst capable of increasing cathode mass-transfer performance of fuel cell and preparation method Expired - Fee Related CN101337184B (en)

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CN101988206A (en) * 2009-07-31 2011-03-23 拜尔材料科学股份公司 Electrode and electrode coating
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CN109904474A (en) * 2019-03-18 2019-06-18 中国科学技术大学 The platinum based catalyst and its application that the conductive black of a kind of conductive black carrier of sulfur doping and preparation method thereof and sulfur doping loads
CN113224323A (en) * 2021-05-17 2021-08-06 安徽师范大学 Three-dimensional flower-shaped ultrathin two-dimensional Ce and B doped Pt nanosheet and preparation method and application thereof
CN114558604A (en) * 2022-03-09 2022-05-31 昆明理工大学 Method for loading platinum on heteroatom-doped carbon nanohorn, catalyst and application thereof
US11667530B1 (en) 2022-03-09 2023-06-06 Kunming University Of Science And Technology Method for preparing heteroatom-doped CNHs and heteroatom-doped carbon nanohorns supporting platinum, and catalyst
US11981569B2 (en) 2022-03-09 2024-05-14 Kunming University Of Science And Technology Method for preparing heteroatom-doped CNHS
CN115663210A (en) * 2022-11-06 2023-01-31 中国人民解放军国防科技大学 Preparation method of carbon-coated platinum oxygen reduction electrocatalyst
CN115663210B (en) * 2022-11-06 2023-10-13 中国人民解放军国防科技大学 Preparation method of carbon-coated platinum-oxygen reduction electrocatalyst

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