CN106207206A - A kind of nitrogen-doped graphene Pt-supported catalyst - Google Patents
A kind of nitrogen-doped graphene Pt-supported catalyst Download PDFInfo
- Publication number
- CN106207206A CN106207206A CN201610576692.3A CN201610576692A CN106207206A CN 106207206 A CN106207206 A CN 106207206A CN 201610576692 A CN201610576692 A CN 201610576692A CN 106207206 A CN106207206 A CN 106207206A
- Authority
- CN
- China
- Prior art keywords
- nitrogen
- doped graphene
- parts
- catalyst
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- H01M4/92—Metals of platinum group
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
- H01M4/926—Metals of platinum group supported on carriers, e.g. powder carriers on carbon or graphite
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of nitrogen-doped graphene Pt-supported catalyst, it is mainly prepared by the raw material of following weight portion: nitrogen-doped graphene 60~90 parts, PdCl215~30 parts, potassium borohydride 300~320 parts;The invention also discloses the preparation method of a kind of nitrogen-doped graphene Pt-supported catalyst.The catalyst that the present invention prepares has bigger desorption peaks area;Catalysis activity is more excellent, has higher redox catalysis performance, stability and bigger catalyst electrochemical active surface;Increase the dispersibility of Pd nanoparticle, decrease the reunion of Pd particle.
Description
Technical field
The present invention relates to catalyst and catalyst synthesis technology field, especially relate to a kind of nitrogen-doped graphene load P d and urge
Agent.
Background technology
Along with the fast development of science, the consumption of the energy is increasingly severe, and the pollution caused is the most increasing, and we are urgent
Ground needs to find a kind of to integrate environmental protection, energy-conservation, efficient clean energy resource.And the high conversion that fuel cell possesses, pollute
Property is little, and the scope of application is wide and valuing researches.The wherein Proton Exchange Membrane Fuel Cells manufacturing cost mistake with hydrogen as fuel
Height, thus cannot be carried out commercially producing;Although DMFC uses simple, cost is suitable, but because methanol has
Stronger volatility, and there is toxicity, not environmentally, the most not ideal enough.In recent years, by nonhazardous, and possesses methanol fuel cell
The aminic acid fuel battery of advantage is shown one's talent, and being recognized as by the public is the ideal source of portable type electronic product.
Along with our further investigation to direct methanoic acid fuel cell, it has been found that formic acid anion and nafion film
In sulfonic acid group there is bigger electrostatic influence, mutually exclusive, permeability is low, so its electrochemical oxidation is relatively good;With
And its theoretical potential and proton conductivity also higher than direct formic acid fuel.Thus, direct methanoic acid fuel cell will have one
Individual wide business development space, is also to solve the one of mankind's fuel contamination to wish greatly.
Such as Chinese patent publication No. CN105597743A, patent disclosure day is on May 23rd, 2016, discloses a kind of oxidation
The preparation method of alumina supporter Pt-supported catalyst, catalyst prepared by the method is alumina support Pt-supported catalyst, although
This method has prepared the Pd catalyst with good catalytic activity under relatively low content of beary metal, but this kind of catalyst
There is alumina support hinders the situations such as catalytic efficiency lifting, Pd skewness in the carrier to exist simultaneously so that utilize the party
The heavy metal Pd catalyst that method prepares still suffers from the situations such as catalytic efficiency is relatively low.
Summary of the invention
For solving the problems referred to above, the invention provides one and there is high catalytic activity, dispersibility, stability and antitoxin performance
Excellent nitrogen-doped graphene Pt-supported catalyst.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of nitrogen-doped graphene Pt-supported catalyst, is prepared by the raw material of following weight portion: nitrogen-doped graphene 60~90 parts,
PdCl215~30 parts, potassium borohydride 300~320 parts.Graphene be at present the thinnest be also the hardest nano material,
There is resistivity low, the advantages such as electron transfer speed is fast, play important role in emerging electrochmical power source, Graphene is as urging
The carrier of agent has the advantages such as bigger specific surface area, good electrical conductivity and mechanical performance, is possible not only to reduce noble metal
The load capacity of Pd, reduces cost, moreover it is possible to be effectively improved the catalysis activity of catalyst;After Graphene nitrating, to oxygen reduction reaction
Demonstrate higher catalysis activity and cyclical stability.
As preferably, nitrogen-doped graphene Pt-supported catalyst is prepared by the raw material of following weight portion: nitrogen-doped graphene 80 parts,
PdCl225 parts, potassium borohydride 317 parts.
As preferably, nitrogen-doped graphene is prepared by following methods: add in the graphene oxide that weight portion is 30~35 parts
Enter the ammonia that weight portion is 2700~2800 parts, supersound process sufficiently long time so that it is in ink-like;By ink-like product with
Weight portion is that the ammonia of 2650~2750 parts is put in hydrothermal reaction kettle, reacts 4~6 hours at a temperature of 200~240 DEG C, system
Obtain nitrogen-doped graphene basic products;Nitrogen-doped graphene basic products is reacted 6~7 hours at 300~600 DEG C, prepares nitrating graphite
Alkene.
The preparation method of described nitrogen-doped graphene Pt-supported catalyst, comprises the following steps:
A) nitrogen-doped graphene joins supersound process in distilled water make it be uniformly dispersed to obtain nitrogen-doped graphene solution;
B) by PdCl2It is dissolved in enough distilled water and prepares PdCl2Solution, makes PdCl2The concentration of solution is 0.05mol/L,
By PdCl after supersound process2The pH value of solution is adjusted to 7~8;
C) potassium borohydride is joined in enough distilled water and make its positive good dissolving prepare solution of potassium borohydride;
D) PdCl that the nitrogen-doped graphene solution prepared by step a is prepared with step b2Solution mixes, and will mix molten
Liquid is heated to 50~60 DEG C;
E) mixed solution after processing through step d is slowly added to solution of potassium borohydride;
F) mixed solution after adding potassium borohydride reacts 6~8 hours at 50~60 DEG C;
G) by reacted for step f product through sucking filtration, washing, dried prepared nitrogen-doped graphene Pt-supported catalyst.
As preferably, in step e, the mixed solution after processing through step d is slowly added to solution of potassium borohydride, makes every
The addition of minute potassium borohydride is 30 weight portions.
As preferably, the reaction in step f is carried out in a nitrogen atmosphere.
As preferably, in step g, it is dried at a temperature of 70~80 DEG C after product washing.
Therefore, the method have the advantages that
(1) there is bigger desorption peaks area;
(2) catalysis activity is more excellent, has higher redox catalysis performance, stability and bigger catalyst electrification
Learn active surface area;
(3) increase the dispersibility of Pd nanoparticle, decrease the reunion of Pd particle.
Accompanying drawing explanation
Fig. 1 is three battery structure schematic diagrams;
Fig. 2 is the XRD spectra of different embodiment gained catalyst;
Fig. 3 is the SEM figure of embodiment 2 and embodiment 3 gained catalyst;
Fig. 4 is that the EDX of embodiment 3 can spectrogram;
Fig. 5 is the cyclic voltammetry curve that each embodiment prepares that catalyst electrode surface sweeping speed in the electrolytic solution is 20mV/s;
Fig. 6 is the cyclic voltammetry curve that each embodiment prepares that catalyst electrode surface sweeping speed in the electrolytic solution is 50mV/s;
Fig. 7 is the cyclic voltammetry curve that each embodiment prepares that catalyst electrode surface sweeping speed in the electrolytic solution is 2mV/s
Fig. 8 is the cyclic voltammetry curve that each embodiment prepares that catalyst electrode surface sweeping speed in the electrolytic solution is 10mV/s
Fig. 9 is that each embodiment prepares catalysis electrode current of polarization curve under 0.4V constant potential;
Figure 10 is the PVI curve that each embodiment prepares under catalyst electrode 0.1mA constant current in the electrolytic solution;
Figure 11 is the PVI curve that embodiment 3 prepares under catalyst electrode different constant currents in the electrolytic solution;
Figure 12 is that to prepare catalyst electrode scanning speed in 0.5mol/L sulfuric acid solution be following of 50mV/s to each embodiment
Ring volt-ampere curve.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is further illustrated.
Embodiment 1
A kind of nitrogen-doped graphene Pt-supported catalyst, is prepared by the raw material of following weight portion: nitrogen-doped graphene 60 parts,
PdCl215 parts, potassium borohydride 300 parts;
Wherein, nitrogen-doped graphene is prepared by following methods:
Adding the ammonia that weight portion is 2700 parts in the graphene oxide that weight portion is 30 parts, supersound process is sufficiently long
Time so that it is in ink-like;The ammonia that ink-like product and weight portion are 2650 parts is put in hydrothermal reaction kettle, at 200 DEG C
At a temperature of react 4 hours, prepare nitrogen-doped graphene basic products;Nitrogen-doped graphene basic products is reacted 6 hours at 300 DEG C, system
Obtain nitrogen-doped graphene;
Additionally graphene oxide is prepared by hummer method.
The preparation method of a kind of nitrogen-doped graphene Pt-supported catalyst, comprises the following steps:
A) nitrogen-doped graphene joins supersound process in distilled water make it be uniformly dispersed to obtain nitrogen-doped graphene solution;
B) by PdCl2It is dissolved in enough distilled water and prepares PdCl2Solution, makes PdCl2The concentration of solution is 0.05mol/L,
By PdCl after supersound process2The pH value of solution is adjusted to 7;
C) potassium borohydride is joined in enough distilled water and make its positive good dissolving prepare solution of potassium borohydride;
D) PdCl that the nitrogen-doped graphene solution prepared by step a is prepared with step b2Solution mixes, and will mix molten
Liquid is heated to 50 DEG C;
E) mixed solution after processing through step d is slowly added to solution of potassium borohydride, makes potassium borohydride per minute
Addition is 30 weight portions;
F) mixed solution after adding potassium borohydride reacts 6 hours under 50 DEG C of nitrogen atmospheres;
G) by reacted for step f product through sucking filtration, washing, the dried nitrogen-doped graphene Pt-supported catalyst for preparing, dry
Dry carry out at a temperature of 70 DEG C.
Embodiment 2
A kind of nitrogen-doped graphene Pt-supported catalyst, is prepared by the raw material of following weight portion: nitrogen-doped graphene 80 parts,
PdCl225 parts, potassium borohydride 317 parts;
Wherein, nitrogen-doped graphene is prepared by following methods:
Adding the ammonia that weight portion is 2730 parts in the graphene oxide that weight portion is 35 parts, supersound process is sufficiently long
Time so that it is in ink-like;The ammonia that ink-like product and weight portion are 2730 parts is put in hydrothermal reaction kettle, at 210 DEG C
At a temperature of react 5 hours, prepare nitrogen-doped graphene basic products;Nitrogen-doped graphene basic products is reacted 6 hours at 400 DEG C, system
Obtain nitrogen-doped graphene;
Additionally graphene oxide is prepared by hummer method.
The preparation method of a kind of nitrogen-doped graphene Pt-supported catalyst, comprises the following steps:
A) nitrogen-doped graphene joins supersound process in distilled water make it be uniformly dispersed to obtain nitrogen-doped graphene solution;
B) by PdCl2It is dissolved in enough distilled water and prepares PdCl2Solution, makes PdCl2The concentration of solution is 0.05mol/L,
By PdCl after supersound process2The pH value of solution is adjusted to 7.5;
C) potassium borohydride is joined in enough distilled water and make its positive good dissolving prepare solution of potassium borohydride;
D) PdCl that the nitrogen-doped graphene solution prepared by step a is prepared with step b2Solution mixes, and will mix molten
Liquid is heated to 50 DEG C;
E) mixed solution after processing through step d is slowly added to solution of potassium borohydride, makes potassium borohydride per minute
Addition is 30 weight portions;
F) mixed solution after adding potassium borohydride reacts 6 hours under 50 DEG C of nitrogen atmospheres;
G) by reacted for step f product through sucking filtration, washing, the dried nitrogen-doped graphene Pt-supported catalyst for preparing, dry
Dry carry out at a temperature of 70 DEG C.
Embodiment 3
A kind of nitrogen-doped graphene Pt-supported catalyst, is prepared by the raw material of following weight portion: nitrogen-doped graphene 90 parts,
PdCl230 parts, potassium borohydride 320 parts;
Wherein, nitrogen-doped graphene is prepared by following methods:
Adding the ammonia that weight portion is 2800 parts in the graphene oxide that weight portion is 35 parts, supersound process is sufficiently long
Time so that it is in ink-like;The ammonia that ink-like product and weight portion are 2750 parts is put in hydrothermal reaction kettle, at 240 DEG C
At a temperature of react 6 hours, prepare nitrogen-doped graphene basic products;To react 7 hours at nitrogen-doped graphene basic products 600 DEG C, prepare
Nitrogen-doped graphene;
Additionally graphene oxide is prepared by hummer method.
The preparation method of a kind of nitrogen-doped graphene Pt-supported catalyst, comprises the following steps:
A) nitrogen-doped graphene joins supersound process in distilled water make it be uniformly dispersed to obtain nitrogen-doped graphene solution;
B) by PdCl2It is dissolved in enough distilled water and prepares PdCl2Solution, makes PdCl2The concentration of solution is 0.05mol/L,
By PdCl after supersound process2The pH value of solution is adjusted to 8;
C) potassium borohydride is joined in enough distilled water and make its positive good dissolving prepare solution of potassium borohydride;
D) PdCl that the nitrogen-doped graphene solution prepared by step a is prepared with step b2Solution mixes, and will mix molten
Liquid is heated to 60 DEG C;
E) mixed solution after processing through step d is slowly added to solution of potassium borohydride, makes potassium borohydride per minute
Addition is 30 weight portions;
F) mixed solution after adding potassium borohydride reacts 8 hours under 60 DEG C of nitrogen atmospheres;
G) by reacted for step f product through sucking filtration, washing, the dried nitrogen-doped graphene Pt-supported catalyst for preparing, dry
Dry carry out at a temperature of 80 DEG C.
Embodiment 4
A kind of nitrogen-doped graphene Pt-supported catalyst, is prepared by the raw material of following weight portion: nitrogen-doped graphene 80 parts,
PdCl225 parts, potassium borohydride 317 parts;
Wherein, nitrogen-doped graphene is prepared by following methods:
Adding the ammonia that weight portion is 2730 parts in the graphene oxide that weight portion is 35 parts, supersound process is sufficiently long
Time so that it is in ink-like;The ammonia that ink-like product and weight portion are 2730 parts is put in hydrothermal reaction kettle, at 210 DEG C
At a temperature of react 5 hours, prepare nitrogen-doped graphene;
Additionally graphene oxide is prepared by hummer method.
The preparation method of a kind of nitrogen-doped graphene Pt-supported catalyst, comprises the following steps:
A) nitrogen-doped graphene joins supersound process in distilled water make it be uniformly dispersed to obtain nitrogen-doped graphene solution;
B) by PdCl2It is dissolved in enough distilled water and prepares PdCl2Solution, makes PdCl2The concentration of solution is 0.05mol/L,
By PdCl after supersound process2The pH value of solution is adjusted to 7.5;
C) potassium borohydride is joined in enough distilled water and make its positive good dissolving prepare solution of potassium borohydride;
D) PdCl that the nitrogen-doped graphene solution prepared by step a is prepared with step b2Solution mixes, and will mix molten
Liquid is heated to 50 DEG C;
E) mixed solution after processing through step d is slowly added to solution of potassium borohydride, makes potassium borohydride per minute
Addition is 30 weight portions;
F) mixed solution after adding potassium borohydride reacts 6 hours under 50 DEG C of nitrogen atmospheres;
G) by reacted for step f product through sucking filtration, washing, the dried nitrogen-doped graphene Pt-supported catalyst for preparing, dry
Dry carry out at a temperature of 70 DEG C.
The impact of performance characterizes:
1. detection method
A. prepared by catalysis electrode: claims 5mgPd/N-Graphene in plastic test tube, adds 15 μ L Nafion and 2 times
Dehydrated alcohol, in supersonic cleaning machine ultrasonic 20 minutes to ink-like (10 points are changed water once), pipette 27 μ L with liquid-transfering gun and be loaded in
The cleaned glass carbon surface of a diameter of 4mm (uses Al2O3Vitreous carbon after polishing), make load electrode;
B. the structural characterization of catalyst: after sample ultrasonic, carries out XRD test, Cu target, A=0.143124nm;
C. Catalysis experiments device and electrochemical property test:
Use three-electrode system, as it is shown in figure 1, include: catalysis electrode, reference electrode: saturated calomel electrode;Auxiliary electricity
Pole: platinum electrode, is used for conducting electric current.Use CV, LSV and IT Study of Catalyst electrocatalysis characteristic to formic acid oxidation.CV is permissible
Observe the current peak (between-0.2V~0.8V, sweep speed is 50mV/s to sweep limits) of the catalysis oxidation of catalyst;
LSV may determine that the initial oxidation current potential of catalyst;It can record formic acid electrocatalytic oxidation galvanic current and change over (constant potential
For 0.4V).Electrolyte is 1mol/L HCOOH+0.5mol/L H2SO4(being the most all referred to as electrolyte).It is passed through in the electrolytic solution
20min obtains nitrogen to remove the dissolved oxygen in electrolyte, can carry out electrochemical property test.
2. the performance test results:
A.XRD test result:
As in figure 2 it is shown, we can see that from figure the diffraction maximum of (002) crystal face at reduced graphene at 2 θ is
On the position of 26.5 °, Pd crystal (111), (200), (220), 2 θ of diffraction maximum of (311) crystal face are respectively 40.118 °,
46.658 °, 68.119 °, 82.098 °, illustrate that catalyst that different sintering temperature processes is by the Pd of cubic plane core structure and stone
Ink alkene composition.From figure, we have further appreciated that (002) crystal face of 600 DEG C of calcination process rear catalysts moves to right, according to formula:
2d sin θ=λ, it can be deduced that θ is the biggest, and d is the least, namely reduced graphene spacing between layers diminishes, and makes graphite
Alkene structure shortrange order, electric conductivity improves.
B.SEM test result analysis:
As shown in Figure 3, it is seen that in different embodiments, the dispersing morphology of Pd granule changes, and it is mainly at nitrating graphite
Alkene produces impact through the roasting of different temperatures, and sintering temperature changes the agglomeration of Pd, improves dispersibility.Compared to reality
Executing example 2 roasting at 400 DEG C, the embodiment 3 catalyst Pd granule under 600 DEG C of roastings more disperses, and improves catalyst
Performance;
As shown in fig. 4, it can be seen that C, N, O, Pd are the elements that mainly comprises of nitrogen-doped graphene Pt-supported catalyst, explanation
Graphene success nitrating.
C. catalyst electrocatalysis characteristic in formic acid oxidation is catalyzed:
Fig. 5 and Fig. 6 is respectively this catalysis electrode cyclic voltammogram under 20mV and 50mV in the electrolytic solution.Can from figure
A peak of prominence produced by formic acid oxidation is occurred in that at about 0.1V to find out;Under 20mV, its formic acid of the catalyst of not roasting
Oxidation peak current electric current density is 17.83mA cm-2, and embodiment 1,2,3 processes the formic acid oxidation peak point current of rear catalyst
Density improves the most in various degree, respectively 39.49mA cm-2, 42.99mA cm-2With 62.82mA cm-2.And during 50mV, rule
Restraining similar, its formic acid oxidation peak current electric current density of catalyst after embodiment 4 processes is 29.94mA cm-2, embodiment 1,2,
After 3 process, its formic acid oxidation peak current density all increases, and embodiment 1,2,3 processes the peak current density of rear catalyst
It is respectively 29.94mA cm-2, 57.25mA cm-2, 62.98mA cm-2, 95.70mA cm-2.We can see that embodiment
The electric current density of 3 process rear catalysts is the highest, and the catalytic performance of this catalyst is optimal;
Fig. 7, Fig. 8 are respectively the LSV figure that this catalyst electrode scanning speed in the electrolytic solution is 2mV/s and 10mV/s.From
In it can be seen that an obvious oxidation peak, play peak position at about-0.12V, it can be seen that embodiment 3 processes rear catalyst and rises
Peak position the most the earliest, so the better performances of this catalyst.
D. catalyst stability in Formic Acid Catalytic Oxidation:
The study on the stability of catalyst is mainly by chronoa mperometric plot and the sign of time-measuring electric potential curve;
As it is shown in figure 9, the catalyst after different embodiments are processed, in 3600s, all occur in that downward trend, embodiment
Electric current density after 3 process declines the slowest, and its electric current density is consistently higher than other catalyst.Electrode inactivation causes electricity
Current density declines, and can produce CO, and these poisonous substances CO can accumulate at catalyst surface, accounts for during being because formic acid indirect oxidation
According to partially catalyzed active center, thus Pd electrode inactivates, and peak point current declines.Electrochemistry after embodiment 3 process is described
Stability is more preferably;
Figure 10 is that different embodiment prepares the chronoa mperometric plot that catalyst is made under the constant current of 0.1mA, and Figure 11 is real
Execute the chronoa mperometric plot that the catalyst of example 3 preparation is made respectively under 0.1mA, 0.3mA, 0.6mA constant current;From Figure 10 we
Can be seen that take-off potential is-0.075mV, wherein embodiment 3 preparation catalyst parallel voltage-0.05mV~-
0.04mV, embodiment 3 preparation at-0.035mV~-0.025mV, embodiment 1 preparation at-0.025mV~0.03mV, implement
Example 4 preparation at 0mV~0.075mV;The take-off potential that we can see that catalyst from Figure 11 is 0.12mV, then exists
Plateau potential under 0.1mA is between 0.18mV~0.20mV, and the plateau potential of 0.3mA is under 0.19mV~0.21mV, 0.6mA
Plateau potential at 0.25mV~0.28mV;Because Pd/N-Graphene catalyst is as the negative pole in battery, so parallel
Voltage is the lowest more good;Figure 10 and Figure 11 all illustrates that catalyst stability prepared by embodiment 3 is better than other temperature calcination and processes
After catalyst.
E. catalyst electrocatalysis characteristic in sulphuric acid measures:
It is this catalyst electrode CV figure in sulfuric acid electrolyte as shown in figure 12;Cyclic voltammetry curve is by three part groups
Become: Part I is the adsorption desorption process of hydrogen, occurs in-0.20V~+0.10V scope;Part II is the discharge and recharge of electric double layer
Process, in+0.10V~+0.30V scope;Part III is oxidation and the reducing zone of oxygen, in+0.30V~+0.80V scope;Aobvious
So, the catalyst after four kinds for the treatment of of different temperature all occurs in that the desorption peaks of hydrogen, and the peak value of desorption peaks is different and becomes rule.From figure
In it may be seen that these four catalyst urge electrochemistry effective active specific surface area size order be embodiment 3 > embodiment 2
> embodiment 1 > embodiment 4, so the effective active specific surface area of the catalyst of embodiment 3 preparation is maximum.
Claims (3)
1. a nitrogen-doped graphene Pt-supported catalyst, it is characterised in that prepared by the raw material of following weight portion: nitrogen-doped graphene
60~90 parts, PdCl215~30 parts, potassium borohydride 300~320 parts.
A kind of nitrogen-doped graphene Pt-supported catalyst the most according to claim 1, it is characterised in that by following weight portion
Raw material prepares: nitrogen-doped graphene 80 parts, PdCl225 parts, potassium borohydride 317 parts.
A kind of nitrogen-doped graphene Pt-supported catalyst the most according to claim 1, it is characterised in that described nitrating graphite
Alkene has following methods to prepare:
The ammonia that weight portion is 2700~2800 parts, supersound process foot is added in the graphene oxide that weight portion is 30~35 parts
The enough long time so that it is in ink-like;The ammonia that ink-like product and weight portion are 2650~2750 parts is put into hydro-thermal reaction
In still, react 4~6 hours at a temperature of 200~240 DEG C, prepare nitrogen-doped graphene basic products;Nitrogen-doped graphene basic products is existed
React 6~7 hours at 300~600 DEG C, prepare nitrogen-doped graphene.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610576692.3A CN106207206A (en) | 2016-07-18 | 2016-07-18 | A kind of nitrogen-doped graphene Pt-supported catalyst |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610576692.3A CN106207206A (en) | 2016-07-18 | 2016-07-18 | A kind of nitrogen-doped graphene Pt-supported catalyst |
Publications (1)
Publication Number | Publication Date |
---|---|
CN106207206A true CN106207206A (en) | 2016-12-07 |
Family
ID=57491696
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201610576692.3A Pending CN106207206A (en) | 2016-07-18 | 2016-07-18 | A kind of nitrogen-doped graphene Pt-supported catalyst |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN106207206A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106848340A (en) * | 2017-02-28 | 2017-06-13 | 中国科学院大学 | A kind of preparation method of hypopolarization lithium air battery positive electrode catalysis material |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102145305A (en) * | 2011-04-08 | 2011-08-10 | 南京航空航天大学 | Method for preparing graphene-loaded nano alloy catalyst |
EP2687483A1 (en) * | 2012-07-16 | 2014-01-22 | Basf Se | Graphene containing nitrogen and optionally iron and/or cobalt |
CN104028293A (en) * | 2014-06-24 | 2014-09-10 | 常州大学 | Method for preparing low-temperature nitrogen-doped graphene supported nano Pd hydrogenation catalyst |
CN104307512A (en) * | 2014-10-14 | 2015-01-28 | 武汉大学苏州研究院 | Supported palladium catalyst and preparation method and application thereof |
-
2016
- 2016-07-18 CN CN201610576692.3A patent/CN106207206A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102145305A (en) * | 2011-04-08 | 2011-08-10 | 南京航空航天大学 | Method for preparing graphene-loaded nano alloy catalyst |
EP2687483A1 (en) * | 2012-07-16 | 2014-01-22 | Basf Se | Graphene containing nitrogen and optionally iron and/or cobalt |
CN104028293A (en) * | 2014-06-24 | 2014-09-10 | 常州大学 | Method for preparing low-temperature nitrogen-doped graphene supported nano Pd hydrogenation catalyst |
CN104307512A (en) * | 2014-10-14 | 2015-01-28 | 武汉大学苏州研究院 | Supported palladium catalyst and preparation method and application thereof |
Non-Patent Citations (2)
Title |
---|
BO ZHENG,JIONG WANG等: "Low-loading cobalt coupled with nitrogen-doped porous graphene as excellent electrocatalyst for oxygen reduction reaction", 《JOURNAL OF MATERIALS CHENISTRY A》 * |
胡佳杰,胡翔,金燕仙等: "PdCo/RGO催化剂对甲酸的氧化电催化性能", 《化学研究》 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106848340A (en) * | 2017-02-28 | 2017-06-13 | 中国科学院大学 | A kind of preparation method of hypopolarization lithium air battery positive electrode catalysis material |
CN106848340B (en) * | 2017-02-28 | 2019-07-30 | 中国科学院大学 | A kind of preparation method of hypopolarization lithium-air battery anode catalytic material |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN106694007B (en) | A kind of single dispersion metal atom/graphene composite catalyst and its preparation method and application | |
CN106654300B (en) | A kind of electrochemistry swelling graphite prepares single dispersion metal atom/graphene composite material method | |
EP2613389B1 (en) | Lithium air battery | |
CN104681823B (en) | A kind of nitrogen-doped graphene and Co3O4 hollow nano-sphere composites and its preparation method and application | |
CN109718822B (en) | Method for preparing metal-carbon composite catalytic material and application thereof | |
CN106669739A (en) | Transition metal sulfide/carbon nanotube composite material as well as preparation method and application thereof | |
CN107829107A (en) | A kind of graphene/carbon nano-tube load single dispersion metal atomic composite catalyst and its preparation method and application | |
CN105289687A (en) | Nitrogen-doped graphene-supported iron-based nanoparticle composite catalyst and preparation method thereof | |
CN107335451A (en) | The preparation method of platinum/molybdenum disulfide nano sheet/graphene three-dimensional combination electrode catalyst | |
CN103022521A (en) | Palladium-cobalt/graphene nano electro-catalyst and preparation method thereof | |
CN108336374A (en) | Nitrogenous carbon material of a kind of high-performance ternary Fe-Co-Ni codopes and its preparation method and application | |
CN106268901A (en) | A kind of nitrogen-doped graphene load P d/Ni catalyst and preparation method thereof | |
CN109935840A (en) | A kind of preparation method of fuel cell Pt base catalyst | |
CN106410214A (en) | Preparation method of NiS2 catalyst with high specific surface area | |
CN110400939A (en) | A kind of preparation method of biomass nitrating porous carbon oxygen reduction catalyst | |
CN106268899A (en) | A kind of preparation method of nitrogen-doped graphene Pt-supported catalyst | |
CN106207205A (en) | A kind of fuel cell PtPd eelctro-catalyst and preparation method thereof | |
CN110629248A (en) | Fe-doped Ni (OH)2Preparation method of/Ni-BDC electrocatalyst | |
CN102593475A (en) | Modified Pt-based fuel-cell catalyst and preparation methods thereof | |
CN110592616A (en) | Method for preparing platinum/titanium dioxide nanotube composite electrode by electroplating method | |
CN104600332B (en) | Without membrane cell catalyst pulp and prepare catalyst pulp and electrode method | |
CN101562250B (en) | Method for preparing cathode catalyst of proton exchange membrane fuel cell | |
CN113201759A (en) | Three-dimensional porous carbon supported bismuth sulfide/bismuth oxide composite catalyst and preparation method and application thereof | |
CN109201054B (en) | Self-supporting bimetallic catalyst and preparation method and application thereof | |
CN101176844A (en) | Direct methanol fuel cell anode catalyzer as well as preparation method and application thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20161207 |
|
RJ01 | Rejection of invention patent application after publication |