CN110048132A - A kind of three-dimensional preparation method for propping up forked Pt-Cu-Mn alloy nanoparticle - Google Patents
A kind of three-dimensional preparation method for propping up forked Pt-Cu-Mn alloy nanoparticle Download PDFInfo
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- CN110048132A CN110048132A CN201910352322.5A CN201910352322A CN110048132A CN 110048132 A CN110048132 A CN 110048132A CN 201910352322 A CN201910352322 A CN 201910352322A CN 110048132 A CN110048132 A CN 110048132A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- H—ELECTRICITY
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- 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
- H01M4/92—Metals of platinum group
- H01M4/921—Alloys or mixtures with metallic elements
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- H—ELECTRICITY
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- H01M4/90—Selection of catalytic material
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Abstract
The invention discloses a kind of three-dimensional preparation methods for propping up forked Pt-Cu-Mn alloy nanoparticle.The present invention is using chloroplatinic acid, copper chloride and manganese chloride as raw material, and using NaI as structure directing agent, using specific glycine and ethylene glycol additional amount, baking oven auxiliary synthesizes a kind of higher three-dimensional forked Pt-Cu-Mn alloy nano particle of branch of selectivity.Easy to operate, nontoxic, repeatability is strong, and cost is relatively low.The three-dimensional of acquisition props up forked Pt-Cu-Mn alloy nano particle alloying level with higher and the low coordination atom density in surface, shows outstanding durability and CO tolerance catalysts ability, is with a wide range of applications.
Description
Technical field
The invention belongs to function nano field of material technology.Specifically, the present invention is prepared using solvent-thermal process method
A kind of three-dimensional forked Pt-Cu-Mn alloy nano particle of branch.
Background technique
Precious metals pt nano-structured calalyst is widely used in the fields such as petrochemical industry, bionic, photoelectrocatalysis, because
It has excellent catalytic activity.Unfortunately, the problem of Pt base catalyst material still has easy poisoning and deactivation, in order to solve
Pt and cheap transition metal element can be formed alloy catalyst at present, such as Co, Ni, Fe, Cu, Cr, Mn by these problems
Deng.Alloying can also improve the oxidizing potential of Pt, to enhance the endurance quality of catalyst, promote oxygen in the desorption on the surface Pt,
Promote the activity of its hydrogen reduction.Most importantly transition metal mostly inexpensively, partially replaces Pt with it, it is possible to reduce Pt's
Dosage, so that the cost of film electrode component of proton exchange film fuel battery be greatly reduced.
Pt base catalyst poisoning is that the strong interaction of the CO substance and Pt active site generated by centre causes, and leads
The rapid deactivation for causing Pt catalyst, to reduce the activity of catalyst.The formation of more metal alloys not only improves catalytic performance, also
It can be reduced the load capacity of Pt, to reduce the cost of catalyst.There are many kinds of methods to prepare PtCu alloy nano at present
Particle, such as Liao et al. using one pot of solvent structure be prepared for PtCu nanoparticle (J. Phys. Chem. C 2016,
120,19,10476-10484.).These methods are that have irritation using n,N-Dimethylformamide and ethylene glycol as solvent
Smell and there is certain toxicity, and the problems such as PtCu nanoparticle will appear aggregation and support corrosion, is unable to fully embody
The activity of PtCu alloy.A kind of method for preparing the three-dimensional forked Pt-Cu-Mn alloy nano particle of branch that the present invention develops, operation
Simply, nontoxic, repeatability is strong, and improves the utilization rate of Pt, substantially increases the anti-poisoning capability of catalyst, increases
The stability of Pt-Cu-Mn alloy.
In face of the continuous quick exhaustion deteriorated with fossil fuel of environment, Proton Exchange Membrane Fuel Cells is converted because of its energy
High-efficient, disposal of pollutants is low, and device manufacturing is simple, stores the advantages that facilitating with processing method and receives more and more attention.
So far, Pt base catalyst is the catalyst that catalytic performance is best in Proton Exchange Membrane Fuel Cells.But Pt in catalyst
Easily CO is caused to be poisoned during the reaction, the serious activity and stability for reducing catalyst strongly limits proton exchange
The extensive use of membrane cell.Therefore the utilization rate and anti-toxicity energy of Pt are improved, the catalytic activity for improving Pt is extremely urgent.
Summary of the invention
In view of the above technical problems, the present invention solves the technologies such as expensive and easy poisoning existing for current Pt catalyst
Problem prepares a kind of three-dimensional forked Pt-Cu-Mn alloy nano particle of branch, improves the performance of Pt nano-structured calalyst.
To achieve the above object, the present invention is achieved by the following technical solutions.
A kind of three-dimensional experimental procedure for propping up forked Pt-Cu-Mn alloy nano particle preparation method is as follows:
150 mg glycine, 200 mg polyvinylpyrrolidones are weighed, 150 mgNaI are subsequently added into 2.0 mL chlorine in beaker
Platinic acid (19.3 mmol/L), 1.0 mL copper chlorides (20 mmol/L), 1.0 mL manganese chlorides (20 mmol/L) aqueous solution and 1.0
Dissolution is sufficiently stirred with magnetic stirring apparatus in the ethylene glycol solution of mL, is then added in reaction kettle, 200 DEG C of baking oven 4 h of reaction, instead
By processing steps such as ethyl alcohol centrifuge washing, freeze-dryings after answering, the three-dimensional forked Pt-Cu-Mn alloy nanoparticle of branch is obtained
Son.
Preferably, reducing agent is ethylene glycol.
Preferably, it is synthesized using solvent thermal reaction, synthesis temperature is 150-250 DEG C, more preferably 200 DEG C.
Wherein: the study found that NaI is structure directing agent, dosage has decisive significance to Pt-Cu-Mn crystal morphology, only
Have in the case that the additional amount of NaI is 150 mg, can just obtain three-dimensional of the invention and prop up forked Pt-Cu-Mn alloy nanoparticle
Son.
Preferably, the amount ranges of glycine are 100-200 mg, more preferably 150 mg.
It is received further, it should be noted that present invention three-dimensional is heated and synthesized using baking oven and props up forked Pt-Cu-Mn alloy
The essential factor of rice corpuscles is stablized due to baking oven and heats up, and is conducive to the crystal that growth defect is few, has been orientated, and close
At Nanoalloy particle crystallization degree is high, easily controllable size and is evenly distributed, avoid alloy particle hard aggregation, could obtain
Forked Pt-Cu-Mn alloy nano particle is propped up to three-dimensional of the invention.
Beneficial effects of the present invention: the present invention is oriented to using chloroplatinic acid, copper chloride and manganese chloride as raw material by pattern of NaI
The higher three-dimensional forked Pt-Cu-Mn alloy of branch of selectivity is prepared using specific glycine and ethylene glycol additional amount in agent
Nanoparticle, whole process energy conservation and environmental protection.The three-dimensional of acquisition props up the forked higher alloying journey of Pt-Cu-Mn alloy nano particle
Coordination atom density low with surface is spent, outstanding durability and CO tolerance catalysts is shown, is with a wide range of applications.
Detailed description of the invention
Fig. 1 is the XRD spectrum that the three-dimensional that embodiment 1 is prepared props up forked Pt-Cu-Mn alloy nano particle.
Fig. 2 is the TEM map that the three-dimensional that embodiment 1 is prepared props up forked Pt-Cu-Mn alloy nano particle.
Fig. 3 is that the three-dimensional that embodiment 1 is prepared props up forked Pt-Cu-Mn alloy nano particle and business Pt/C as first
The cyclic voltammetry curve comparison diagram of alcohol electro-oxidizing-catalyzing agent.
Fig. 4 is that the three-dimensional that embodiment 1 is prepared props up forked Pt-Cu-Mn alloy nano particle and business Pt/C as first
The cyclic voltammetry curve comparison diagram of sour electro-oxidizing-catalyzing agent.
Fig. 5 is the TEM map for the Pt-Cu-Mn alloy nano particle that comparative example 1 is prepared.
Fig. 6 is the TEM map for the Pt-Cu-Mn alloy nano particle that comparative example 2 is prepared.
Fig. 7 is the TEM map for the Pt-Cu-Mn alloy nano particle that comparative example 3 is prepared.
Specific embodiment
Below by way of the implementation and possessed beneficial effect of specific embodiment the present invention will be described in detail technical solution, but not
It can regard as any restriction to enforceable range of the invention.
Embodiment 1
150 mg glycine, 200 mg polyvinylpyrrolidones are weighed, 150 mgNaI are subsequently added into 2.0 mL chlorine in beaker
Platinic acid (19.3 mmol/L), 1.0 mL copper chlorides (20 mmol/L), 1.0 mL manganese chlorides (20 mmol/L) and 1.0 ml second two
Dissolution is sufficiently stirred with magnetic stirring apparatus in alcoholic solution, is then added in reaction kettle, 200 DEG C of baking oven 4 h of reaction, after reaction
By processing steps such as ethyl alcohol centrifuge washing, freeze-dryings, three-dimensional forked Pt-Cu-Mn alloy nano particle (such as Fig. 2 of branch is obtained
It is shown).
The test of methanol (formic acid) electroxidation: anodic oxidation performance test is using conventional three-electrode system, in CHI650D
It is carried out on type electrochemical workstation.It is a platinum filament to electrode with saturated calomel electrode (SCE) for reference electrode, and the electricity that works
Extremely diameter be 3 mm glass-carbon electrode (GC).A certain amount of catalyst suspension (holding metal quality is 4 μ g) is taken to drip to GC electricity
It is dry under infrared lamp on the surface of pole, then there is one end of sample against UV ozone lamp (launch wavelength working electrode drop
For 185 nm and 254 nm, power is 10 W) it is separated by 5 mm irradiation, 12 h to remove the organic molecule of sample surfaces (such as
PVP).Then the 0.5 wt% Nafion solution (ethyl alcohol dilution) of upper 2 μ L is dripped on the surface of working electrode.Catalyst electrochemistry
Active area is tested with 0.5 M H2SO4Solution first leads to the high-purity N of 30 min as electrolyte before experiment2To electrolyte deoxygenation,
Then cyclic voltammetric (CV) scanning is carried out with 50 mV/s rates, the scanning range of setting is 0.24~1.0 V.In experimentation
Holding superjacent is N2Atmosphere.The test of methanol (formic acid) electroxidation is in 0.5 M H2SO4 + 2 M CH3OH(0.5 M
H2SO4+ 0.25 M HCOOH) it carries out in electrolyte, before CV test, lead to high-purity N230 min are purged to be used to remove electrolyte
In dissolved oxygen, the scanning range set as 0.24~1.0 V, determine scanning speed be 50 mV/s.Current density is to work
Unit catalyst electrochemical activation area (cm on electrode2) on electric current indicate.Each working electrode is followed with the rate of 50 mV/s
Ring scan process 50 encloses obtained stable CV curve.Prepared by the three-dimensional forked Pt-Cu-Mn nanoparticle of branch for embodiment 1, it
The size just swept the current density that peak is normalized on electrochemical surface area ECSA and represent the latent active of catalyst, from figure
It is 4.69 that 3 and Fig. 4, which can be seen that the three-dimensional highest current density for propping up forked Pt-Cu-Mn nanoparticle in methanol electro-oxidizing,
mA cm-2, the highest current density in the experiment of formic acid electroxidation is 1.17mA cm-2, methanol highest much higher than commercial Pt/C
Current density is 0.55 mA cm-2, formic acid highest current density is 0.29 mA cm-2.As can be seen from Figure 3 Pt-Cu-Mn
Positive scanning peak value be significantly larger than than the numerical value of inverse scan peak value Pt/C peak ratio, illustrate CO tolerance catalysts ability improve, urge
The activity of agent is significantly improved with stability.
Comparative example 1
100 mg glycine, 200 mg polyvinylpyrrolidones are weighed, 150 mgNaI are subsequently added into 2.0 mL chlorine in beaker
Platinic acid (19.3 mmol/L), 1.0 mL copper chlorides (20 mmol/L), 1.0 mL manganese chlorides (20 mmol/L) and 1 mL ethanol amine
Dissolution is sufficiently stirred with magnetic stirring apparatus in solution, is then added in reaction kettle, 200 DEG C of baking oven 4 h of reaction are passed through after reaction
The processing steps such as ethyl alcohol centrifuge washing, freeze-drying are crossed, are obtained Pt-Cu-Mn alloy nano particle (as shown in Figure 5), and are used
Test condition same as Example 1, obtaining its highest current density in methanol electro-oxidizing is 1.05 mA cm-2, in first
Highest current density in sour electroxidation experiment is 0.33 mA cm-2。
Comparative example 2
150 mg glycine, 200 mg polyvinylpyrrolidones are weighed, 150 mgNaI are subsequently added into 2.0 mL chlorine in beaker
Platinic acid (19.3 mmol/L), 1.0 mL copper chlorides (20 mmol/L), 1.0 mL manganese chlorides (20 mmol/L) and 1 ml ethanol amine
Dissolution is sufficiently stirred with magnetic stirring apparatus in solution, is then added in reaction kettle, 200 DEG C of baking oven 4 h of reaction are passed through after reaction
The processing steps such as ethyl alcohol centrifuge washing, freeze-drying are crossed, are obtained Pt-Cu-Mn alloy nano particle (as shown in Figure 6), and are used
Test condition same as Example 1, obtaining its highest current density in methanol electro-oxidizing is 1.79 mA cm-2, in first
Highest current density in sour electroxidation experiment is 0.89 mA cm-2。
Comparative example 3
100 mg of glycine, 200 mg polyvinylpyrrolidones are weighed, 150 mgNaI are subsequently added into 2.0 mL chlorine in beaker
Platinic acid (19.3 mmol/L), 1.0 mL copper chlorides (20 mmol/L), 1.0 mL manganese chlorides (20 mmol/L) and 1.0 ml second two
Alcoholic solution is sufficiently stirred dissolution with magnetic stirring apparatus, is then transferred in reaction kettle, 200 DEG C of baking oven 4 h of reaction, after reaction
By processing steps such as ethyl alcohol centrifuge washing, freeze-dryings, Pt-Cu-Mn alloy nano particle (as shown in Figure 7) is obtained, and is adopted
With test condition same as Example 1, obtaining its highest current density in methanol electro-oxidizing is 1.65 mA cm-2,
Highest current density in the experiment of formic acid electroxidation is 0.59 mA cm-2。
Moreover, it relates to arrive multiple groups comparative example, it will not enumerate in view of length, be respectively relative to embodiment 1
Change one or more parametric variables, cannot get this hair in the case where changing one or more variable as the result is shown
Bright three-dimensional props up forked Pt-Cu-Mn alloy nano particle, and showing between each technical characteristic of the technical solution of the application has
Synergistic effect, and catalytic activity is far below the catalytic activity of the embodiment of the present invention 1, show the application technical solution no matter from
Unexpected technical effect is reached for alloy pattern or catalytic activity.
Claims (5)
1. a kind of three-dimensional preparation method for propping up forked Pt-Cu-Mn alloy nanoparticle, specific steps are as follows:
150 mg glycine, 200 mg polyvinylpyrrolidones are weighed, it is dense to be subsequently added into 2.0 mL in beaker by 150 mgNaI
Degree is the chloroplatinic acid aqueous solution of 19.3 mmol/L, and 1.0 mL concentration are the copper chloride solution of 20 mmol/L, 1.0 mL concentration
For the manganese chloride of 20 mmol/L and the ethylene glycol solution of 1.0 mL, dissolution is sufficiently stirred with magnetic stirring apparatus, reaction is then added
In kettle, 200 DEG C of baking oven 4 h of reaction obtain three-dimensional after reaction by processing steps such as ethyl alcohol centrifuge washing, freeze-dryings
The forked Pt-Cu-Mn alloy nano particle of branch.
2. a kind of three-dimensional forked Pt-Cu-Mn alloy nano particle preparation method of branch described in claim 1, it is characterised in that: make
With ethanol amine, ethylene glycol, ethyl alcohol, preferably ethylene glycol.
3. a kind of three-dimensional forked Pt-Cu-Mn alloy nano particle preparation method of branch claimed in claims 1-2, it is characterised in that:
It is prepared using solvent-thermal process method, baking oven range of reaction temperature is 150-250 DEG C, preferably 200 DEG C.
4. a kind of three-dimensional forked Pt-Cu-Mn alloy nano particle preparation method of branch described in claim 1-3, it is characterised in that:
The amount ranges of glycine are 100-200 mg, preferably 150 mg.
5. a kind of three-dimensional forked Pt-Cu-Mn alloy nano particle preparation method of branch described in claim 1-4, it is characterised in that:
The amount ranges of NaI are 100-300 mg, preferably 150 mg.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110534756A (en) * | 2019-09-09 | 2019-12-03 | 济南大学 | A kind of preparation method optimizing porous complicated and confused shape Pt-Ru-Ni alloy nanoparticle performance |
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| CN110534756A (en) * | 2019-09-09 | 2019-12-03 | 济南大学 | A kind of preparation method optimizing porous complicated and confused shape Pt-Ru-Ni alloy nanoparticle performance |
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