CN105870467A - Oxygen reduction La(OH)3/reduced graphene oxide composite catalyst as well as preparation method and application thereof - Google Patents
Oxygen reduction La(OH)3/reduced graphene oxide composite catalyst as well as preparation method and application thereof Download PDFInfo
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- CN105870467A CN105870467A CN201610327533.XA CN201610327533A CN105870467A CN 105870467 A CN105870467 A CN 105870467A CN 201610327533 A CN201610327533 A CN 201610327533A CN 105870467 A CN105870467 A CN 105870467A
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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
- H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- H01M4/88—Processes of manufacture
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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
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Abstract
The invention discloses an oxygen reduction La(OH)3/reduced graphene oxide composite catalyst as well as a preparation method and application thereof. The composite catalyst is prepared from a La(OH)3 nanorod loaded on a reduced graphene oxide (rGO) slice layer. The preparation method comprises the following steps: dispersing potassium hydroxide, lanthanum nitrate and graphene oxide into water, performing thermal treatment at first and then hydrothermal reaction, and cooling, centrifugating and freeze-drying a reaction product to obtain the composite catalyst. The preparation method of the composite catalyst is simple, low in cost and favorable for industrial production. When applied to a fuel cell, the prepared composite catalyst is higher in activity and excellent in stability.
Description
Technical field
The present invention relates to a kind of hydrogen reduction (ORR) catalyst and methods for making and using same thereof, use particularly to one
Hydrogen reduction La (OH) in fuel cell3/ redox graphene (rGO) composite catalyst and preparation method,
Belong to electro-catalysis technical field.
Technical background
All the time, cheap commercially viable ORR catalyst is developed for accelerating negative electrode ORR mistake slowly
Journey is development fuel cell and a key problem of other electrochemical energy equipment.Recent two decades comes, in non-noble
Although the research and development aspect of metal ORR catalyst makes some progress, but there is also one from reality application
Fixed distance.
In recent years, in addition to transition metal oxide, the compound of rare earth metal is urged as base metal ORR
Agent is also subject to the people's attention, but equally exists mass activity and the low defect of electrical conductivity.By its physics chi
Very little be reduced to nanoscale and compound with the functional material of bigger serface high conductivity be to solve the two defect
Effective way.Since within 2004, finding, Graphene relies on its high conductivity, bigger serface, enriches
The unique performance such as sandwich arouse widespread concern in the world, started rapidly one
" graphene thermal ".Rare earth compound is combined with Graphene, is expected to improve it as fuel cell ORR
The combination property of catalyst.
Summary of the invention
Activity is there is as ORR catalyst low with electrical conductivity for single rare earth metallic compound in prior art
Defect, one of the object of the invention is to be to provide a kind of Novel oxygen reduction with excellent comprehensive catalytic performance
La(OH)3/ rGO composite catalyst, catalytic performance is substantially better than La (OH)3Catalyst.
Second object of the present invention is to be to provide a kind of simple to operate, low cost to prepare described hydrogen reduction
La(OH)3The method of/rGO composite catalyst；The method can make La (OH)3Generate with rGO mono-step and the most multiple
Closing, technique is simple, meets industrial production application requirement.
Third object of the present invention is to provide described hydrogen reduction La (OH)3/ rGO composite catalyst is at fuel
Application in battery, in alkaline medium, catalytic performance is better than La (OH)3。
In order to realize above-mentioned technical purpose, the invention provides a kind of hydrogen reduction La (OH)3/ rGO composite catalyzing
Agent, this composite catalyst is by La (OH)3Nanometer rods is carried on rGO lamella composition.
Preferably scheme, La (OH) in composite catalyst3The mass percent of nanometer rods and rGO consists of
(80% 95%): (5% 20%).La (OH) in composite catalyst3Nanometer rods and the mass percent of rGO
Composition is more preferably (85% 92%): (8% 15%).
Present invention also offers a kind of hydrogen reduction La (OH)3The preparation method of/rGO composite catalyst, this preparation side
Method is potassium hydroxide, lanthanum nitrate and graphene oxide to be dispersed in water, and carries out heat at a temperature of 60 100 DEG C
After process, being transferred in hydrothermal reaction kettle, carry out hydro-thermal reaction at a temperature of 120 180 DEG C, hydro-thermal reaction is produced
Thing cooling, centrifugal and freeze-drying, to obtain final product.
Preferably scheme, potassium hydroxide, lanthanum nitrate and graphene oxide mass percent consist of
(30% 45%): (45% 65%): (3% 10%).
Preferably scheme, composite catalyst is by La (OH)3Nanometer rods is carried on rGO lamella composition；Wherein,
La(OH)3The mass percent of nanometer rods and rGO consists of (80% 95%): (5% 20%).It is combined and urges
La (OH) in agent3The mass percent of nanometer rods and rGO forms more preferably (85% 92%):
(8% 15%).
Preferably scheme, heat treatment temperature is 70 90 DEG C.
Preferably scheme, hydrothermal temperature is 140 160 DEG C.
More preferably scheme, heat treatment time is 5 20h.
More preferably scheme, the hydro-thermal reaction time is 10 40h.
Present invention also offers a kind of described Novel oxygen reduction La (OH)3The application of/rGO composite catalyst,
La(OH)3/ rGO composite catalyst is applied to fuel cell.
Hinge structure, the Advantageous Effects that technical scheme is brought:
1, the hydrogen reduction La (OH) of the present invention3/ rGO composite catalyst is by having ORR catalysis activity
La(OH)3The rGO of nanometer rods and bigger serface high conductivity is composited, Synergistic between various materials
Substantially, catalytic performance is substantially better than La (OH) in effect3。
2, the hydrogen reduction La (OH) of the present invention3/ rGO method for preparing composite catalyst is simple, low cost, favorably
In industrialized production.
3, the hydrogen reduction La (OH) of the present invention3/ rGO composite catalyst is generated by reaction in-situ, La (OH)3
Nanometer rods uniformly, is stably supported on rGO lamella, and physicochemical stability is good.
4, the hydrogen reduction La (OH) of the present invention3/ rGO composite catalyst is applied to fuel cell, shows higher
Activity and good stability, relative to La (OH)3, there is more preferable combination property.
Accompanying drawing explanation
[Fig. 1] is La (OH) in embodiment 1 and comparative example 13/ rGO and La (OH)3XRD, show
La(OH)3Containing La (OH) in/rGO composite3And Graphene；
[Fig. 2] is La (OH) in embodiment 13SEM (a) and TEM (b and the c) figure of/rGO, shows diameter 10 20
Nm, the La (OH) of long 50 150nm3Nanometer rods is carried on rGO lamella equably；
[Fig. 3] is La (OH) in embodiment 1 and comparative example 13/ rGO and La (OH)3Linear sweep voltammetry curve
Figure, rotating speed is 1600rpm；
[Fig. 4] (a) is La (OH) in embodiment 13/ rGO linear sweep voltammetry curve map under different rotating speeds；
B () is with La (OH) in embodiment 13/ rGO is the electron transfer number figure during catalyst ORR；
[Fig. 5] is La (OH) in embodiment 1 and comparative example 13/ rGO and La (OH)3Chronoa mperometric plot figure.
Detailed description of the invention
It is more fully described present invention by embodiment below, but is not limiting as the protection of the claims in the present invention
Scope.
Embodiment 1
La(OH)3The preparation of/rGO is divided into two steps, specific as follows:
(1) preparation of graphene oxide (GO)
GO uses the Hummers method synthesis improved.Weigh 1g graphite powder and 5g NaCl, both are mixed
Grinding 30min, vacuum filtration is dried, is transferred in 250mL round-bottomed flask, is slowly added to 23mL dense
Sulfuric acid, and stir 24h.Round-bottomed flask is transferred in 35 DEG C of water-baths, adds 0.5g NaNO3And continue
Stirring.Treat NaNO3After dissolving, extremely it is slowly added into 3g KMnO4, more continuously stirred 120min.Slow
Slow addition 46mL deionized water, is transferred in 98 DEG C of water-baths heat 30min, and removal is cooled to normal temperature not
Disconnected stirring, is sequentially added into 140mL deionized water and 10mL 30% hydrogen peroxide stirring 5min respectively.Adopt
The GO in suspension is collected with centrifugal method.In centrifugal process (rotating speed is 8000 revs/min), first with 5%
Hydrochloric acid solution washes twice, then is washed with deionized repeatedly, until mixed liquor is neutrality.Finally, by GO
Being scattered in the aqueous solution and obtain GO suspension, the content of GO is about 2.43mg/mL.
(2)La(OH)3The preparation of/rGO
Measure 5mL 0.5mol/L La (NO3)3Solution, above 10mL 1mol/L KOH solution and 30mL
The GO suspension prepared, is transferred in 250mL round-bottomed flask, adds 75mL deionized water.
After ultrasonic 30min, heat in 80 DEG C of water-baths and stir 12h, mixed liquor being divided equally and is transferred to two 100
In the reactor of mL, at 150 DEG C, react 24h.Centrifugal method is used to collect product, at centrifugal process
In (rotating speed is 6000 revs/min), respectively with absolute ethyl alcohol and deionized water repeatedly wash to cleaning solution be neutrality.
Finally, the product after centrifugal is carried out freeze-drying, obtains La (OH)3/ rGO composite.La(OH)3Matter
Amount degree is about 89%, and rGO mass percentage content is about 11%.
Employing X-ray diffractometer (XRD, Rigaku-D/Max 2550, Cu-K α,40kV,
300mA) product is carried out material phase analysis；By SEM (SEM, FEI Quanta-200,20kV)
With the pattern that product observed by transmission electron microscope (TEM, JEOL-2010,200kV).
Test specimens in three-electrode system is stood in through CHI760D electrochemical operation by rotating disk electrode (r.d.e) (RDE)
The limiting current density of product evaluates its ORR activity.The preparation of working electrode: weigh 4mg testing sample,
It is scattered in the 1mL mixed liquor of ethanol, water and 5%nafion solution (volume ratio is 16:8:1), ultrasonic 1h,
Obtaining 4mg/mL dispersion liquid, liquid-transfering gun draws 20 μ L hanging drops and is added to the glass-carbon electrode of diameter 5.6mm
On, 60 DEG C are dried to be measured.In test process, being platinum electrode to electrode, reference electrode is Hg/HgO
Electrode.When evaluating the ORR activity of sample, electrolyte is the 0.1M KOH solution that oxygen is saturated, rotating speed
For 1600rpm, sweep speed is 10mV/s, and scanning voltage scope is 0.2V to-1.0V (vs.Hg/HgO).
Under different speed conditions, by electron transfer number during the calculating hydrogen reduction of Koutechy-Levich formula.
Compared the stability of sample ORR catalysis by chronoamperometry, test voltage is-0.2V (vs.Hg/HgO),
Electrolyte is the 0.1M KOH solution that oxygen is saturated.
La(OH)3/ rGO compound as the take-off potential of ORR catalyst be-0.16V (vs.Hg/HgO),
Half wave potential is-0.29V (vs.Hg/HgO), and limiting current density is-3.06mA/cm2.-0.5 to-0.6
The hydrogen reduction average electron transfer number of V (vs.Hg/HgO) potential region is about 3.40, trends towards 4 electro transfer
Approach.In evaluating when galvanometer, after 6800s continuously runs, current density conservation rate is about 80%.
Embodiment 2
As described in Example 1, at La (OH)3The preparation of/rGO adds 35mL GO suspension.
The evaluation method of catalytic performance is with embodiment 1.
La(OH)3/ rGO compound is-0.18V (vs.Hg/HgO) as the take-off potential of ORR catalyst,
Half wave potential is-0.33V (vs.Hg/HgO), and limiting current density is-3.01mA/cm2.In the galvanometer news commentary
In valency, after 6800s continuously runs, current density conservation rate is about 83%.
Comparative example 1
As described in Example 1, at La (OH)3The preparation of/rGO is not added with GO suspension, preparation La (OH)3。
The evaluation method of catalytic performance is with embodiment 1.
La(OH)3As the take-off potential of ORR catalyst be-0.37V (vs.Hg/HgO), half wave potential be
-0.65V (vs.Hg/HgO), limiting current density is-1.2mA/cm2.In evaluating when galvanometer, through 6800
After s continuously runs, current density conservation rate is about 65%.
Claims (10)
1. a hydrogen reduction La (OH)3/ redox graphene composite catalyst, it is characterised in that: by La (OH)3
Nanometer rods is carried on redox graphene lamella composition.
Hydrogen reduction La (OH) the most according to claim 13/ redox graphene composite catalyst, its feature
It is: La (OH) in described composite catalyst3The mass percent composition of nanometer rods and redox graphene
For (80% 95%): (5% 20%).
Hydrogen reduction La (OH) the most according to claim 1 and 23/ redox graphene composite catalyst, its
It is characterised by: La (OH) in described composite catalyst3Nanometer rods and the mass percent of redox graphene
Consist of (85% 92%): (8% 15%).
4. a hydrogen reduction La (OH)3The preparation method of/redox graphene composite catalyst, it is characterised in that:
Potassium hydroxide, lanthanum nitrate and graphene oxide are dispersed in water, are heat-treated at a temperature of 60 100 DEG C
After, it is transferred in hydrothermal reaction kettle, at a temperature of 120 180 DEG C, carries out hydro-thermal reaction, hydro-thermal reaction product warp
Cooling, centrifugal and freeze-drying, to obtain final product.
Hydrogen reduction La (OH) the most according to claim 43The preparation side of/redox graphene composite catalyst
Method, it is characterised in that: potassium hydroxide, lanthanum nitrate and graphene oxide mass percent consist of (30% 45%):
(45% 65%): (3% 10%).
Hydrogen reduction La (OH) the most according to claim 43The preparation side of/redox graphene composite catalyst
Method, it is characterised in that: described composite catalyst is by La (OH)3Nanometer rods is carried on redox graphene sheet
Constitute on layer；Wherein, La (OH)3The mass percent of nanometer rods and redox graphene consists of
(80% 95%): (5% 20%).
Hydrogen reduction La (OH) the most according to claim 63The preparation side of/redox graphene composite catalyst
Method, it is characterised in that: La (OH)3The mass percent of nanometer rods and redox graphene consists of
(85% 92%): (8% 15%).
Hydrogen reduction La (OH) the most according to claim 43The preparation side of/redox graphene composite catalyst
Method, it is characterised in that: heat treatment temperature is 70 90 DEG C；Hydrothermal temperature is 140 160 DEG C.
9. according to the hydrogen reduction La (OH) described in claim 4 or 83The system of/redox graphene composite catalyst
Preparation Method, it is characterised in that: heat treatment time is 5 20h；The hydro-thermal reaction time is 10 40h.
10. the hydrogen reduction La (OH) described in a claim 1 or 23Answering of/redox graphene composite catalyst
With, it is characterised in that: it is applied to fuel cell.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108568284A (en) * | 2017-03-10 | 2018-09-25 | 厦门稀土材料研究所 | It is a kind of to be removed using the graphene-based material of support type210The method of Po aerosols |
| CN110026153A (en) * | 2019-01-18 | 2019-07-19 | 闽南师范大学 | A kind of synthetic method and absorption property of graphene oxide-samaric hydroxide composite material |
| CN110026152A (en) * | 2019-01-18 | 2019-07-19 | 闽南师范大学 | A kind of graphene oxide-europium hydroxide composite material, preparation method and applications |
| CN111545211A (en) * | 2020-04-26 | 2020-08-18 | 闽南师范大学 | Graphene oxide-lanthanum oxide-cobalt hydroxide composite material, and synthesis method and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108568284A (en) * | 2017-03-10 | 2018-09-25 | 厦门稀土材料研究所 | It is a kind of to be removed using the graphene-based material of support type210The method of Po aerosols |
| CN108568284B (en) * | 2017-03-10 | 2021-05-18 | 厦门稀土材料研究所 | Removal by using supported graphene-based material210Po aerosol method |
| CN110026153A (en) * | 2019-01-18 | 2019-07-19 | 闽南师范大学 | A kind of synthetic method and absorption property of graphene oxide-samaric hydroxide composite material |
| CN110026152A (en) * | 2019-01-18 | 2019-07-19 | 闽南师范大学 | A kind of graphene oxide-europium hydroxide composite material, preparation method and applications |
| CN111545211A (en) * | 2020-04-26 | 2020-08-18 | 闽南师范大学 | Graphene oxide-lanthanum oxide-cobalt hydroxide composite material, and synthesis method and application thereof |
| CN111545211B (en) * | 2020-04-26 | 2023-01-10 | 闽南师范大学 | Graphene oxide-lanthanum oxide-cobalt hydroxide composite material, and synthesis method and application thereof |
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