CN108682870A - Monatomic loaded catalyst of bimetallic and preparation method thereof - Google Patents
Monatomic loaded catalyst of bimetallic and preparation method thereof Download PDFInfo
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Abstract
The invention discloses monatomic loaded catalysts of a kind of bimetallic and preparation method thereof, and preparation method includes the following steps：S1, using metal-organic framework materials and cyanamide or its aggressiveness as raw material, prepare the Me NC with nucleocapsid, wherein Me derives from the metal in the metal-organic framework materials；S2, the Me NC are added in dispersant, add binder, ultrasonic disperse obtains suspension；S3, it takes the suspension to be uniformly coated on ring-disc electrode, is placed in electrolyte, multiple volt-amperes of cycles are carried out continuously using Pt as to electrode；S4, the material on the ring-disc electrode after volt-ampere recycles is subjected to ultrasonic Separation, washs drying, obtain the monatomic catalyst of nitrating defect carbon supporting Pt Me bimetallics, the as monatomic loaded catalyst of bimetallic.The present invention concentrates Pt and Me atoms the defect area for being dispersed in carbon carrier, the distance between metallic atom smaller than common monatomic Pt catalyst, produces synergistic effect, improves the selectivity of four electron reactions.
Description
Technical field
The present invention relates to electro-catalysis technical field more particularly to a kind of monatomic loaded catalyst of bimetallic and its preparations
Method.
Background technology
Electrocatalytic reaction such as produces hydrogen reaction (HER) and oxygen reduction reaction (ORR), is widely used in New Energy Industry.
HER is the important half-reaction of electrocatalytic decomposition water, and the hydrogen of output has green non-pollution compared to conventional fossil fuel and can
The advantage of Persisting exploitation, be at present in addition to steam reformation produce hydrogen other than most important production hydrogen methods.ORR reactions are then fuel cells
And the important half-reaction of metal-air battery, it is applied to hydrogen-oxygen fuel cell, the various fuel cells such as methanol fuel cell
System and zinc and air cell, the various metal-air battery systems such as aluminum-air battery.
Since beginning of this century new-energy automobile comes out, fuel cell is just as a kind of important energy-provision way by major vapour
Depot quotient is applied in the design of new-energy automobile, with the traditional oil gas energy-provision way of substitution.Compared to petrol engine, fuel cell
Any pernicious gas is not will produce in use, unique emission is harmless water, for solving domestic big city Winter Fog
Haze problem is significant.Currently, platinum (Pt) and its alloy are because it is with good catalytic activity, it is that HER and ORR is most common
Elctro-catalyst.But it is Pt scarcity of resources, expensive, and in direct methanol fuel cell, Pt also suffers from the poison of methanol
Change acts on and loses catalytic activity, these drawbacks greatly hinder the large-scale application of fuel cell.Therefore, exploitation being capable of generation
Material for platinum based catalyst is to make electro-catalysis hydrogen manufacturing, and fuel cell and metal-air battery being capable of large-scale commercial applications
A critical issue.
It is practical to rise since Pt is supported on carbon base body in the form of nano particle in business Pt/C catalyst
The atom of catalytic activity only has the surface atom of Pt particles, and there are the low drawbacks of Pt atom utilization ratios.Monatomic Pt dispersions
It can effectively improve Pt atom utilization ratios on carbon base body, not only improve reactivity, but also reduce the usage amount of Pt.So
And during hydrogen reduction two-electron shift mainly occurs for the monatomic Pt catalyst reported at present, reaction product is dioxygen
Water, reaction efficiency are low.Density functional theory (DFT) calculation shows that, monatomic Pt catalysis oxygen, which carries out four electronic reduction reactions, to be needed
Want huge overpotential.So, how while reducing Pt usage amounts, and four electron reaction paths can be kept just to become and worked as
A preceding important subject.
Invention content
The technical problem to be solved in the present invention is, it is monatomic to provide a kind of bimetallic improving four electron reactions selectivity
The preparation method of loaded catalyst and the monatomic loaded catalyst of bimetallic obtained.
The technical solution adopted by the present invention to solve the technical problems is：A kind of monatomic supported catalyst of bimetallic is provided
The preparation method of agent, includes the following steps：
S1, using metal-organic framework materials and cyanamide or its aggressiveness as raw material, prepare the Me- with nucleocapsid
NC, wherein Me derive from the metal in the metal-organic framework materials；
S2, the Me-NC is added in dispersant, adds binder, ultrasonic disperse obtains suspension；
S3, it takes the suspension to be uniformly coated on ring-disc electrode, is placed in electrolyte, using platinum filament as continuous to electrode
Carry out multiple volt-amperes of cycles；
S4, the material on the ring-disc electrode after volt-ampere recycles is subjected to ultrasonic Separation, washs drying, obtained nitrating and lack
Fall into the monatomic catalyst of carbon supporting Pt Me bimetallics, the as monatomic loaded catalyst of bimetallic.
Preferably, in step S1, by the metal-organic framework materials and cyanamide or its aggressiveness with 1:The matter of (1-20)
Amount is than mixing, and under inert gas atmosphere, 750 DEG C of -950 DEG C of calcinations 1-3 hours make the complete carbon of the metal-organic framework materials
Change, obtains the Me-NC with nucleocapsid.
Preferably, the aggressiveness of the cyanamide is dicyandiamide or melamine.
Preferably, the Me is Fe, Co or Ni.
Preferably, in the Me-NC, core is metal, and the shell for coating core is graphite linings.
Preferably, in step S2, the dispersant is ethanol water；The binder is naphthols.
Preferably, in the volt-ampere cycle, voltage window 0.1V-1.1V, electrolyte is the sulfuric acid solution of 0.5M.
Preferably, the volt-ampere cycle is carried out continuously 2000-12000.
Preferably, in step S4, the material after ultrasonic Separation is washed using ethanol solution.
The present invention also provides a kind of monatomic loaded catalysts of bimetallic, using the preparation method described in any of the above item
It is made.
Beneficial effects of the present invention：Pt and Me atoms concentrated to the defect area for being dispersed in carbon carrier, between metallic atom
Distance it is smaller than common monatomic Pt catalyst, therefore synergistic effect is produced, to improve the selectivity of four electron reactions.
Electrochemical activation uses one-step method, while manufacturing defect on carbon base body, by metallic atom reduction in carbon defects, prevents
The reunion of metallic atom ultimately forms the stable monatomic loaded catalyst of PtMe bimetallics, and it is anti-to be suitable for four electronics ORR
It answers.
The monatomic loaded catalyst of bimetallic produced by the present invention, the load capacity of Pt is in 1wt% hereinafter, having more than quotient
The ORR of industry Pt/C catalyst (load capacity of Pt is 20wt%) and HER performances, at the same also ensure in ORR reactions mainly into
Four electronic reduction reaction of row.Due to the synergistic effect of metallic atom and metallic atom, collaboration of the metallic atom with coordination nitrogen-atoms
The synergistic effect of effect and metallic atom and carbon carrier, the electronic structure reacted at position is optimised, to improve four electronics
The selectivity of reaction.
Description of the drawings
Present invention will be further explained below with reference to the attached drawings and examples, in attached drawing：
Fig. 1 is the monatomic loaded catalyst preparation method flow chart of bimetallic of the present invention；
Fig. 2 is the lens electron microscope of the monatomic loaded catalyst of bimetallic made from embodiment 1 in the present invention；
Fig. 3 is the X ray diffracting spectrum in embodiment 1 before and after product electrochemical activation in the present invention；
Fig. 4 is the performance comparison figure of product and commercial catalysts in embodiment 1 in the present invention；
Fig. 5 is the performance comparison figure of product and commercial catalysts in embodiment 2 in the present invention；
Fig. 6 is the lens electron microscope of the monatomic loaded catalyst of bimetallic made from embodiment 3 in the present invention；
Performance map of the product in soda acid electrolyte in embodiment 3 in Fig. 7 present invention；
Fig. 8 is the lens electron microscope of the monatomic loaded catalyst of bimetallic made from embodiment 4 in the present invention；
Performance map of the product in soda acid electrolyte in embodiment 4 in Fig. 9 present invention.
Specific implementation mode
For a clearer understanding of the technical characteristics, objects and effects of the present invention, now control attached drawing is described in detail
The specific implementation mode of the present invention.
With reference to figure 1, the preparation method of the monatomic loaded catalyst of bimetallic of the invention, it may include following steps：
S1, using metal-organic framework materials (MOFs) and cyanamide or its aggressiveness as raw material, preparing has nucleocapsid
Me-NC, wherein Me derive from metal-organic framework materials in metal.
Wherein, metal-organic framework materials optionally have：The organic framework material (Co-MOF) of cobalt, the organic backbone material of iron
Expect the organic framework material (Ni-MOF) etc. of (Co-MOF), nickel.The optional type of metal-organic framework materials includes that (next watt uncommon by MILs
Your framework material), ZIFs (class zeolitic imidazolate framework material) etc..The aggressiveness of cyanamide includes dicyandiamide and melamine.
Specifically, in step S1, by metal-organic framework materials and cyanamide (dicyandiamide or melamine) with 1:(1-
20) mass ratio mixing, can be placed in tube furnace, under inert gas (such as nitrogen) atmosphere, 750 DEG C of -950 DEG C of calcination 1-3 are small
When, make metal-organic framework materials carbonization, obtains the Me-NC with nucleocapsid.In Me-NC, according to the organic bone of metal
The selection of frame material, Me Fe, Co or Ni.
In Me-NC structures, core is metal (Me), and the shell for coating core is graphite linings.
S2, Me-NC is added in dispersant, adds binder, ultrasonic disperse obtains suspension.
Dispersant is ethanol water.In 1mL ethanol waters, ethyl alcohol 0.2mL, water 0.8mL.With 1mL ethanol waters
For solution, the Me-NC of addition is no more than 8mg；The binder 0.05-0.15mL of addition.
Naphthols can be selected in binder.Ultrasonic disperse half an hour.
S3, it takes suspension to be uniformly coated on ring-disc electrode, is placed in electrolyte, using platinum filament (Pt) as continuous to electrode
Carry out multiple volt-amperes of cycles (CV cycles).
In volt-ampere cycle, voltage window 0.1V-1.1V, electrolyte is the sulfuric acid solution of 0.5M.Volt-ampere cycle continuously into
Row 2000-12000.For the ring-disc electrode of diameter 4mm, the suspension of 5-20 μ L is can use, is evenly coated on ring-disc electrode.
The step is mainly activation process.In activation process, agraphitic carbon is aoxidized in the graphite linings of Me-NC, makes stone
Layer of ink produces crack, and electrolyte is able to penetrate into interior metal core from crack, and metallic core is dissolved.Meanwhile by
In electrochemical oxidation process, to the Pt on electrode by oxidation dissolution to electrolyte.When the Me in electrolyte passes through with Pt ions
It will be captured by the carbon defects at graphite linings edge when graphite linings crack, form monatomic Me and Pt.N atoms replace at carbon defects
Part C atoms.
S4, the material on the ring-disc electrode after volt-ampere recycles is subjected to ultrasonic Separation, washs drying, obtained nitrating and lack
Fall into carbon supporting Pt Me bimetallics monatomic catalyst (A-MePt-NC, A：Activation is activated), as bimetallic is monatomic
Loaded catalyst.
Washing uses ethanol solution.
The monatomic loaded catalyst of bimetallic of the present invention is made using above-mentioned preparation method.
Below by way of specific embodiment, the invention will be further described.
Embodiment 1：
The nitrating defect carbon monatomic catalyst A-CoPt-NC of supporting Pt Co bimetallics is prepared, alkalinity ORR is used for：
0.2g cobalt nitrates, 0.21g trimesic acids and 0.02g 4,4- bipyridyls are dissolved in 8.47 milliliters of dimethyl methyl
In amide solution, and 1 ml deionized water, 7.18 milliliters of glycerine are added, stir 2 hours, is uniformly mixed.Then solution is turned
Move in baking oven, 65 DEG C holding 48 hours, after centrifugation obtain the organic framework material (Co-MOF) of cobalt.
By Co-MOF and dicyandiamide with 1:It is put into tube furnace after 16 mass ratio mixing, in a nitrogen atmosphere, 850 DEG C burn
Two hours are burnt, the Co-NC with nucleocapsid is obtained.The Co-NC of 4mg is dispersed in ethanol water (ethyl alcohol 0.2mL, water
In 0.8mL), and the naphthols of 0.08mL is added, ultrasonic disperse half an hour, obtains suspension.The suspension of 10 μ L is taken, is uniformly applied
On the ring-disc electrode of diameter 4mm.Electrode is placed in the sulfuric acid solution of 0.5M, is made to electrode of Pt, with 0.1V to 1.1V
Voltage window, 8000 CV cycles of continuous activation.Finally by the material ultrasonic Separation on ring-disc electrode, washed with ethanol solution
After dry, obtain the monatomic catalyst A-CoPt-NC of nitrating defect carbon supporting Pt Co bimetallics.
The lens electron microscopic picture of the monatomic catalyst of nitrating defect carbon supporting Pt Co bimetallics obtained is as shown in Figure 2.Fig. 2
In (a) be angle of elevation annular dark field figure, (b) be corresponding light field figure；White bright spot is Pt metal and Co atoms in figure, it can be seen that
Metallic atom with monoatomic fractions distribution graphite linings indentation, there (figure (b) in dashed circle part).(b) upper right corner is small in
In figure, dot is metallic atom, and arc dotted portion indicates that graphite linings, metallic atom are distributed in the indentation, there of graphite linings.
Fig. 3 is the X ray diffracting spectrum before and after 1 products obtained therefrom electrochemical activation of embodiment；Curve 1 is Co-NC, curve 2
For A-CoPt-NC.It can be seen that after activation, the peak of metal Co disappears, and illustrates that metal cobalt granule is dissolved in activation.
Graphite peaks, which come to a point, illustrates that degree of graphitization improves, and amorphous carbon is aoxidized in activation, forms notch, and metal Co cores are dissolved,
It is flowed out from indentation, there.
Fig. 4 is the ORR of A-CoPt-NC (line 3), Co-NC (line 2) and business Pt/C (line 1) catalyst in embodiment 1
It can comparison diagram.The half wave potential (0.96V) of A-CoPt-NC is better than business Pt/C (0.87V) as can be seen from Figure.A- simultaneously
The limiting current density of CoPt-NC is also best, has reached 5.7mA/cm2。
Embodiment 2：
The nitrating defect carbon monatomic catalyst A-CoPt-NC of supporting Pt Co bimetallics is prepared, acidity HER is used for：Specific side
Method reference implementation example 1.
Fig. 5 is the HER of A-CoPt-NC (line 3), Co-NC (line 2) and business Pt/C (line 1) catalyst in embodiment 2
It can comparison diagram.Have before the performance ratio activation of A-CoPt-NC as can be seen from Figure and greatly improve, and has been more than business Pt/C catalysis
Agent.Current density is in 60mA/cm2When, it is only necessary to the overpotential of 0.06V is less than the 0.08V of Pt/C.
Embodiment 3：
The monatomic catalyst A-FePt-NC of nitrating defect carbon supporting Pt Fe bimetallics is prepared for HER：
0.32g iron chloride and 0.33g terephthalic acid (TPA)s are dissolved in 10 milliliters of dimethyl formamide solution, stirring 2
Hour, it is uniformly mixed.Then solution is transferred in baking oven, 150 DEG C of 24 hours of holding.After centrifugation having for iron can be obtained
Machine metallic framework (Fe-MOF).
By Fe-MOF and dicyandiamide with 1:It is put into tube furnace after 16 mass ratio mixing, in a nitrogen atmosphere, 850 DEG C burn
Two hours are burnt, the Fe-NC with nucleocapsid is obtained.The Fe-NC of 4mg is dispersed in ethanol water (ethyl alcohol 0.2mL, water
In 0.8mL), and the naphthols of 0.08mL is added, ultrasonic disperse half an hour, obtains suspension.The suspension of 10 μ L is taken, is uniformly applied
On the ring-disc electrode of diameter 4mm.Electrode is placed in the sulfuric acid solution of 0.5M, is made to electrode of Pt, with 0.1V to 1.1V
Voltage window, 8000 CV cycles of continuous activation.Finally by the material ultrasonic Separation on electrode, done after being washed with ethanol solution
It is dry, obtain the monatomic catalyst A-FePt-NC of nitrating defect carbon supporting Pt Fe bimetallics.
The lens Electronic Speculum of the monatomic catalyst A-FePt-NC of nitrating defect carbon supporting Pt Fe bimetallics made from embodiment 3
Picture is as shown in Figure 6.(a) is transmission electron microscope photo in Fig. 6, is (b) angle of elevation annular dark field photo；As can be seen from the figure Fe gold
Belong to core to be completely dissolved, Fe atoms are embedded in the form of monatomic (white bright spot in figure) in graphite linings.
Fig. 7 is HER performance of the A-FePt-NC catalyst in acid (line 1) and alkaline (line 2) electrolyte in embodiment 3
Figure.A-FePt-NC has good HER soda acids compatibility as can be seen from Figure.Current density is in 10mA/cm2When, acidic electrolysis
The overpotential of 75mV is needed in liquid, and the overpotential of 89mV is needed in alkaline electrolyte.
Embodiment 4：
The monatomic catalyst A-NiPt-NC of nitrating defect carbon supporting Pt Ni bimetallics is prepared for HER：
The nickel nitrate of the 2,5- dihydric para-phthalic acids of 0.5g and 1.5g are dissolved in 70 milliliters of dimethylformamide
In solution, and 70 milliliters of ethyl alcohol are added, 70 milliliters of water stir 2 hours, are uniformly mixed.Then solution is transferred in baking oven,
100 DEG C of 66 hours of holding.After centrifugation the organometallic skeletal (Ni-MOF) of nickel can be obtained.
By Ni-MOF and dicyandiamide with 1:It is put into tube furnace after 16 mass ratio mixing, in a nitrogen atmosphere, 850 DEG C burn
Two hours are burnt, the Ni-NC with nucleocapsid is obtained.The Ni-NC of 4mg is dispersed in ethanol water (ethyl alcohol 0.2mL, water
In 0.8mL), and the naphthols of 0.08mL is added, ultrasonic disperse half an hour, obtains suspension.The suspension of 10 μ L is taken, is uniformly applied
On the ring-disc electrode of diameter 4mm.Electrode is placed in the sulfuric acid solution of 0.5M, is made to electrode of Pt, with 0.1V to 1.1V
Voltage window, 8000 CV cycles of continuous activation.Finally by the material ultrasonic Separation on electrode, done after being washed with ethanol solution
It is dry, obtain the monatomic catalyst A-NiPt-NC of nitrating defect carbon supporting Pt Ni bimetallics.
The lens Electronic Speculum of the monatomic catalyst A-NiPt-NC of nitrating defect carbon supporting Pt Ni bimetallics made from embodiment 4
Picture is as shown in Figure 8.(a) is transmission electron microscope photo in Fig. 8, is (b) angle of elevation annular dark field photo；As can be seen from the figure Ni gold
Belong to core to be completely dissolved, Ni atoms are embedded in the form of monatomic (white bright spot in figure) in graphite linings.
Fig. 9 is HER performance of the A-NiPt-NC catalyst in acid (line 1) and alkaline (line 2) electrolyte in embodiment 4
Figure.A-NiPt-NC has good HER soda acids compatibility as can be seen from Figure.Current density is in 10mA/cm2When, acidic electrolysis
The overpotential of 58mV is needed in liquid, and the overpotential of 74mV is needed in alkaline electrolyte.
Example the above is only the implementation of the present invention is not intended to limit the scope of the invention, every to utilize this hair
Equivalent structure or equivalent flow shift made by bright specification and accompanying drawing content is applied directly or indirectly in other relevant skills
Art field, is included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of the monatomic loaded catalyst of bimetallic, which is characterized in that include the following steps：
S1, using metal-organic framework materials and cyanamide or its aggressiveness as raw material, prepare the Me-NC with nucleocapsid,
Middle Me derives from the metal in the metal-organic framework materials；
S2, the Me-NC is added in dispersant, adds binder, ultrasonic disperse obtains suspension；
S3, it takes the suspension to be uniformly coated on ring-disc electrode, is placed in electrolyte, be carried out continuously using platinum filament as to electrode
Multiple volt-amperes of cycles；
S4, the material on the ring-disc electrode after volt-ampere recycles is subjected to ultrasonic Separation, washs drying, obtain nitrating defect carbon
The monatomic catalyst of supporting Pt Me bimetallics, the as monatomic loaded catalyst of bimetallic.
2. preparation method according to claim 1, which is characterized in that in step S1, by the metal-organic framework materials
And cyanamide or its aggressiveness are with 1:（1-20）Mass ratio mixing, under inert gas atmosphere, 750 DEG C of -950 DEG C of calcination 1-3 are small
When, make the metal-organic framework materials carbonization, obtains the Me-NC with nucleocapsid.
3. preparation method according to claim 1, which is characterized in that the aggressiveness of the cyanamide is dicyandiamide or melamine
Amine.
4. preparation method according to claim 1, which is characterized in that the Me is Fe, Co or Ni.
5. preparation method according to claim 1, which is characterized in that in the Me-NC, core is metal, coats core
Shell be graphite linings.
6. preparation method according to claim 1, which is characterized in that in step S2, the dispersant is ethanol water；
The binder is naphthols.
7. preparation method according to claim 1, which is characterized in that in the volt-ampere cycle, voltage window 0.1V-
1.1V, electrolyte are the sulfuric acid solution of 0.5M.
8. preparation method according to claim 1, which is characterized in that the volt-ampere cycle is carried out continuously 2000-12000
It is a.
9. preparation method according to claim 1, which is characterized in that in step S4, using ethanol solution to ultrasonic Separation
Material afterwards is washed.
10. a kind of monatomic loaded catalyst of bimetallic, which is characterized in that use claim 1-9 any one of them systems
Preparation Method is made.
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| CN114522710A (en) * | 2022-01-26 | 2022-05-24 | 大连理工大学 | Ti1Preparation method and application of-NC single-atom catalytic material |
| CN114588907A (en) * | 2022-02-28 | 2022-06-07 | 五邑大学 | Catalyst and preparation method and application thereof |
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| CN115000337B (en) * | 2022-06-13 | 2024-05-03 | 中国科学院苏州纳米技术与纳米仿生研究所 | Defect-rich hydrated vanadium pentoxide nanosheet core-shell structure fiber electrode and preparation method thereof |
| CN115652322A (en) * | 2022-11-09 | 2023-01-31 | 哈尔滨工业大学 | Diatomic catalyst based on electrostatic interaction and preparation method and application thereof |
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