CN102974380A - Iron and nitrogen doped carbon black catalyst and preparation method thereof - Google Patents
Iron and nitrogen doped carbon black catalyst and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an iron and nitrogen doped carbon black catalyst and a preparation method of the iron and nitrogen doped carbon black catalyst, and solves the technical problems that the preparation method of an oxygen reduction catalyst with carbon as the carrier is complex, and requirements for devices are high. The catalyst of the invention is prepared in the following processes: carbon blacks are mixed with melamine evenly through ball milling technique; and the mixed material is doped with iron atoms due to the use of ball milling technique, the iron atoms and nitrogen atoms are enabled to be doped into a stratified structure of the carbon blacks after a high-temperature treatment, and the iron and nitrogen doped carbon black catalyst is formed. The catalyst is very high in oxygen reduction activity, much higher than platinum base catalysts in oxygen reduction initial potential and half wave potential, and higher than the prior oxygen reduction catalyst with the carbon as the carrier in oxygen reduction activity. The preparation method of the iron and nitrogen doped carbon black catalyst is simple, practical, and low in cost. Therefore, the oxygen reduction catalyst is suitable for being used to prepare fuel cells.
Description
Technical field
The present invention relates to the fuel cell technology field, be specifically related to a kind of iron, nitrogen co-doped carbon black Catalysts and its preparation method.
Background technology
Fuel cell, such as Proton Exchange Membrane Fuel Cells and DMFC, because have environmental friendliness, start fast,, power density long without electrolyte loss, life-span and energy density advantages of higher, demonstrate wide application prospect at aspects such as electric powered motor power supply, portable power source, micro power and small-sized electric generating apparatus.For fuel cell, its Cathodic oxygen reduction is the rate controlling step of fuel cell electrocatalytic reaction.And the speed that improves Cathodic oxygen reduction will inevitably be used oxygen reduction catalyst.At present, carbon carries platinum and platinum alloy catalyst is most popular fuel cell oxygen reduction catalyst.But, because expensive, the resource scarcitys of noble metal such as platinum, ruthenium cause the cost of manufacture of fuel cell too high, seriously limited the commercialization process of fuel cell.Therefore, exploitation at a low price, non noble metal oxygen reduction catalyst has become the urgent task of fuel cell development efficiently.
In recent years, people mainly are devoted to the research of the oxygen reduction catalysts take carbon as carrier such as nitrogen-doped carbon material load transition metal, composite metal oxide.Above-mentioned two class catalyst have high activity and high selectivity to the Cathodic oxygen reduction of fuel cell, and preparation cost is low than the cost of platinum based catalyst.As the people such as Ma (The Journal of Physical Chemistry 2011 (115): 25148-25154) prepared the hollow carbon nanosphere that nitrogen mixes by vapour deposition process, its to the catalytic activity of hydrogen reduction close to platinum.Dai seminar is with cobaltosic oxide, and cobalt acid manganese is grown on the graphite oxide, graphite oxide is reduced again, carrying out nitrogen mixes, prepare cobaltosic oxide, the cobalt acid graphene composite catalyst that manganese/nitrogen mixes, this catalyst is higher than the catalyst performance of commercial 20% platinum content.Yet the preparation method of above-mentioned two class oxygen reduction catalysts is very complicated, and equipment is had very high requirement, and operation is wasted time and energy.For example, the hollow carbon nanosphere that nitrogen mixes is in preparation process, use 2,4, the 6-trinitrophenol need to be put into reactant high voltage bearing stainless steel cauldron as detonator during reaction, temperature is elevated to 320 ℃ rapidly, in reactor, formed like this 1000 ℃ of high temperature, reacted under the environment of 20-45 MPa high pressure.Its preparation method is complicated, needs to use equipment high temperature resistant, high pressure.
Summary of the invention
The present invention is complicated for the preparation method who solves the oxygen reduction catalyst take carbon as carrier in the prior art, the technical problem high to equipment requirement, and provide a kind of preparation method simple, have the iron of higher oxygen reducing activity, nitrogen co-doped carbon black Catalysts and its preparation method.
In order to solve the problems of the technologies described above, technical scheme of the present invention is specific as follows:
A kind of iron, nitrogen co-doped carbon black catalyst, this catalyst is to be prepared by following method:
(1) takes by weighing black pearl 2000 and melamine for 1:20 ~ 1:5 in mass ratio, put into the ball mill ball milling 3 ~ 10 hours, obtain containing the mixed-powder of carbon, nitrogen and iron;
(2) mixed-powder that contains carbon, nitrogen and iron that obtains in the step (1) is put into tube furnace, 800 ~ 1000 ℃ of lower processing 0.5 ~ 5 hour, obtain iron, nitrogen co-doped carbon black catalyst.
The iron for preparing in the technique scheme, nitrogen co-doped carbon black catalyst, the ratio of its carbon, nitrogen and iron atom is 10:1 ~ 5:0.5 ~ 1.
The iron for preparing in the technique scheme, nitrogen co-doped carbon black catalyst, the ratio of its carbon, nitrogen and iron atom is 10:3:1.
The preparation method of a kind of iron, nitrogen co-doped carbon black catalyst, this preparation method's concrete steps and condition are as follows:
(1) takes by weighing black pearl 2000 and melamine for 1:20 ~ 1:5 in mass ratio, put into the ball mill ball milling 3 ~ 10 hours, obtain containing the mixed-powder of carbon, nitrogen and iron;
(2) mixed-powder that contains carbon, nitrogen and iron that obtains in the step (1) is put into tube furnace, 800 ~ 1000 ℃ of lower processing 0.5 ~ 5 hour, obtain described iron, nitrogen co-doped carbon black catalyst.
In technique scheme, the mass ratio of black pearl 2000 and melamine is 1:10 in the step (1).
In technique scheme, the tube furnace in the step (2) is single warm area slide rail stove.
In technique scheme, the Ball-milling Time in the step (1) is 4 hours.
In technique scheme, the treatment temperature in the step (2) is 900 ℃.
In technique scheme, the processing time in the step (2) is 1 hour.
The invention has the beneficial effects as follows:
1, iron provided by the invention, nitrogen co-doped carbon black catalyst are: use ball grinding technique that carbon black and melamine are mixed, owing to use ball grinding technique, introduced iron atom, high-temperature process again enters in the layer structure of carbon black iron, nitrogen atom doping and obtains.It is active that the catalyst for preparing has very high hydrogen reduction, and its hydrogen reduction take-off potential and half wave potential are that 20% platinum based catalyst is high a lot of than commercial platinum content, is that the hydrogen reduction of oxygen reduction catalyst of carrier is active high than existing carbon also.
2, when the ratio of carbon, nitrogen and iron atom in iron, the nitrogen co-doped carbon black catalyst is 10:1 ~ 5:0.5 ~ 1, with it in 0.1M KOH solution, the cyclic voltammogram of the saturated lower scanning of oxygen, test hydrogen reduction spike potential is-179 ~-89 mV; Utilize rotating disk electrode (r.d.e) to carry out linearity volt-ampere in the KOH solution of the 0.1mol/L that denitrogenates through oxygen and test, sweep speed is 5mV/s, records its hydrogen reduction take-off potential, and it is 20% Pt/C catalyst that half wave potential all is higher than commercial Pt content.
3, the preparation method of iron provided by the invention, nitrogen co-doped carbon black catalyst, simple, cost is low.Only need raw material black pearl 2000 and melamine are passed through ball milling, high-temperature process can prepare iron, nitrogen co-doped carbon black catalyst again, and iron atom is introduced by mechanical milling process, need not to add iron-bearing material.Therefore, such oxygen reduction catalyst is suitable for preparing fuel cell, and commercialization process that can the propellant battery has broad application prospects.
4, the preparation method of iron provided by the invention, nitrogen co-doped carbon black catalyst, when taking by weighing black pearl 2000 and melamine ball milling 4 hours for 1:10 in mass ratio, mixed-powder with nitrogenous, carbon and iron is 900 ℃ in temperature again, processing time is that the ratio of 1 hour carbon for preparing, nitrogen and iron atom is the catalyst of 10:3:1, hydrogen reduction take-off potential and half wave potential that test obtains are the highest, its hydrogen reduction take-off potential can reach 50mV, and half wave potential is-87mV that the hydrogen reduction activity is the highest.
Description of drawings
Fig. 1 a be the iron of embodiment 1 preparation, nitrogen co-doped carbon black catalyst in 0.1M KOH solution, the cyclic voltammogram under oxygen is saturated.
Fig. 1 b be the iron of embodiment 2 preparation, nitrogen co-doped carbon black catalyst in 0.1M KOH solution, the cyclic voltammogram under oxygen is saturated.
Fig. 1 c be the iron of embodiment 3 preparation, nitrogen co-doped carbon black catalyst in 0.1M KOH solution, the cyclic voltammogram under oxygen is saturated.
Fig. 2 a be the iron of embodiment 1 preparation, nitrogen co-doped carbon black catalyst in 0.1M KOH solution, oxygen is saturated lower, the linear sweep voltammetry figure when sweeping speed for 5mv/s under the different rotation rates.
Fig. 2 b be the iron of embodiment 2 preparation, nitrogen co-doped carbon black catalyst in 0.1M KOH solution, oxygen is saturated lower, the linear sweep voltammetry figure when sweeping speed for 5mv/s under the different rotation rates.
Fig. 2 c be the iron of embodiment 3 preparation, nitrogen co-doped carbon black catalyst in 0.1M KOH solution, oxygen is saturated lower, the linear sweep voltammetry figure when sweeping speed for 5mv/s under the different rotation rates.
Among Fig. 3:
31 for Pt content is that 20% Pt/C catalyst is 1600 rpm at rotating speed, the linear sweep voltammetry figure when sweeping speed for 5mv/s;
32 iron, nitrogen co-doped carbon black catalyst for embodiment 1 preparation are 1600 rpm at rotating speed, the linear sweep voltammetry figure when sweeping speed for 5mv/s;
33 iron, nitrogen co-doped carbon black catalyst for embodiment 2 preparations are 1600 rpm at rotating speed, the linear sweep voltammetry figure when sweeping speed for 5mv/s;
34 iron, nitrogen co-doped carbon black catalyst for embodiment 3 preparations are 1600 rpm at rotating speed, the linear sweep voltammetry figure when sweeping speed for 5mv/s.
The specific embodiment
Invention thought of the present invention is:
Iron, nitrogen co-doped carbon black catalyst, to use ball grinding technique that carbon black and melamine are mixed, because what use is that ball grinding technique mixes raw material, and introduced iron atom, high-temperature process enters in the layer structure of carbon black iron, nitrogen atom doping again, forms iron, nitrogen co-doped carbon black catalyst, wherein, the ratio of carbon, nitrogen and iron atom is 10:1 ~ 5:0.5 ~ 1.The catalyst that this method prepares, wherein, the existence form of ferro element is: with the carbon atom around it, nitrogen-atoms forms complex, and nitrogen is then with pyrroles's nitrogen, and the form of pyridine nitrogen and graphitization nitrogen exists.The iron that forms, nitrogen activated centre can the catalytic oxidation-reduction reactions.
The preparation method of iron, nitrogen co-doped carbon black catalyst only needs by ball milling and high-temperature process, just can prepare oxygen reduction catalyst of the present invention, and this preparation method is simple, and cost is low; It is active that the catalyst for preparing has very high hydrogen reduction, and its hydrogen reduction take-off potential and half wave potential are that 20% platinum based catalyst is high a lot of than commercial platinum content, is that the hydrogen reduction of oxygen reduction catalyst of carrier is active high than existing carbon also.
With 0.1g black pearl 2000(hereinafter to be referred as BP 2000) and the 0.5g melamine put into the shimmy formula ball mill of high speed (Nanjing meaning sail, model GM-3B), high speed ball milling 4 hours.After the ball grinder temperature drops to room temperature, the mixed-powder that contains carbon, nitrogen and iron that obtains is placed single warm area slide rail stove, in 1.01 * 10
5Pa, 900 ℃ of lower high-temperature process 1 hour obtain iron, nitrogen co-doped carbon black catalyst.After temperature drops to room temperature, take out, for subsequent use.Record by ICP: the ratio of carbon, nitrogen and iron atom is 10:1:0.5.
Be iron, the nitrogen co-doped carbon black catalyst that adds the above-mentioned preparation of 5mg in 5% the Nafion solution to 100 μ L mass concentrations, ultrasonic dispersion 30min obtains solution; Get the described solution of 10 μ L and drip and be applied on the rotating disk electrode (r.d.e), after room temperature is dried, obtain membrane electrode; With the SCE electrode as reference electrode, Pt sheet as the three-electrode system to electrode, in the KOH solution of the 0.1mol/L that denitrogenates through oxygen, carry out cyclic voltammetry, sweep speed is 50mV/s, the result is referring to Fig. 1 a.By Fig. 1 a as can be known, the hydrogen reduction spike potential of the catalyst of embodiment 1 preparation is-164mV.
Utilize rotating disk electrode (r.d.e) to carry out the test of linearity volt-ampere in the KOH solution of the 0.1mol/L that denitrogenates through oxygen, sweep speed is 5mV/s, and the result is referring to Fig. 2 a.By Fig. 2 a as can be known, the hydrogen reduction take-off potential of the catalyst of embodiment 1 preparation is 46 mV, and its half wave potential is-108mV.
Among Fig. 3 32 is 1600 rpm for iron, the nitrogen co-doped carbon black catalyst that embodiment 1 prepares at rotating speed, the linear sweep voltammetry figure when sweeping speed for 5mv/s.As shown in Figure 32, the catalyst of embodiment 1 preparation is that the hydrogen reduction take-off potential of 20% Pt/C catalyst is high than Pt content.
0.1g BP 2000 and 1g melamine are put into the shimmy formula ball mill of high speed (Nanjing meaning sail, model GM-3B), high speed ball milling 4 hours.After the ball grinder temperature drops to room temperature, the mixed-powder that contains carbon, nitrogen and iron that obtains is placed single warm area slide rail stove, in 1.01 * 10
5Pa, 900 ℃ of lower high-temperature process 1 hour obtain iron, nitrogen co-doped carbon black catalyst.After temperature drops to room temperature, take out, for subsequent use.Record by ICP: the ratio of carbon, nitrogen and iron atom is 10:3:1.
Be iron, the nitrogen co-doped carbon black catalyst that adds the above-mentioned preparation of 5mg in 5% the Nafion solution to 100 μ L mass concentrations, ultrasonic dispersion 30min obtains solution; Get the described solution of 10 μ L and drip and be applied on the rotating disk electrode (r.d.e), after room temperature is dried, obtain membrane electrode; With the SCE electrode as reference electrode, Pt sheet as the three-electrode system to electrode, in the KOH solution of the 0.1mol/L that denitrogenates through oxygen, carry out cyclic voltammetry, sweep speed is 50mV/s, the result is referring to Fig. 1 b.By Fig. 1 b as can be known, the hydrogen reduction spike potential of the catalyst of embodiment 2 preparations is-179mV.
Utilize rotating disk electrode (r.d.e) to carry out the test of linearity volt-ampere in the KOH solution of the 0.1mol/L that denitrogenates through oxygen, sweep speed is 5mV/s, and the result is referring to Fig. 2 b.By Fig. 2 b as can be known, the hydrogen reduction take-off potential of the catalyst of embodiment 2 preparations is 50mV, and its half wave potential is-87mV.
Among Fig. 3 33 is 1600 rpm for iron, the nitrogen co-doped carbon black catalyst that embodiment 2 prepares at rotating speed, the linear sweep voltammetry figure when sweeping speed for 5mv/s.As shown in Figure 33, the catalyst of embodiment 2 preparation is that the hydrogen reduction take-off potential of 20% Pt/C catalyst is higher than Pt content.
0.1g BP 2000 and 2g melamine are put into the shimmy formula ball mill of high speed (Nanjing meaning sail, model GM-3B), high speed ball milling 7 hours.After the ball grinder temperature drops to room temperature, the mixed-powder that contains carbon, nitrogen and iron that obtains is placed single warm area slide rail stove, in 1.01 * 10
5Pa, 900 ℃ of lower high-temperature process 5 hours obtain iron, nitrogen co-doped carbon black catalyst.After temperature drops to room temperature, take out, for subsequent use.Record by ICP: the ratio of carbon, nitrogen and iron atom is 10:5:1.
Be iron, the nitrogen co-doped carbon black catalyst that adds the above-mentioned preparation of 5mg in 5% the Nafion solution to 100 μ L mass concentrations, ultrasonic dispersion 30min obtains solution; Get the described solution of 10 μ L and drip and be applied on the glass-carbon electrode, after room temperature is dried, obtain membrane electrode; With the SCE electrode as reference electrode, Pt sheet as the three-electrode system to electrode, in the KOH solution of the 0.1mol/L that denitrogenates through oxygen, carry out cyclic voltammetry, sweep speed is 50mV/s, the result is referring to Fig. 1 c.By Fig. 1 c as can be known, the hydrogen reduction spike potential of the catalyst of embodiment 3 preparations is-168mV.
Utilize rotating disk electrode (r.d.e) to carry out the test of linearity volt-ampere in the KOH solution of the 0.1mol/L that denitrogenates through oxygen, sweep speed is 5mV/s, and the result is referring to Fig. 2 c.By Fig. 2 c as can be known, the hydrogen reduction take-off potential of the catalyst of embodiment 3 preparations is 46mV, and its half wave potential is-110mV.
Among Fig. 3 34 is 1600 rpm for iron, the nitrogen co-doped carbon black catalyst that embodiment 3 prepares at rotating speed, the linear sweep voltammetry figure when sweeping speed for 5mv/s.As shown in Figure 34, the catalyst of embodiment 3 preparation is that the hydrogen reduction take-off potential of 20% Pt/C catalyst is high than Pt content.
Embodiment 4
0.1g BP 2000 and 2g melamine are put into the shimmy formula ball mill of high speed (Nanjing meaning sail, model GM-3B), high speed ball milling 3 hours.After the ball grinder temperature drops to room temperature, the mixed-powder that contains carbon, nitrogen and iron that obtains is placed common tube furnace, in 1.01 * 10
5Pa, 1000 ℃ of lower high-temperature process 0.5 hour obtain iron, nitrogen co-doped carbon black catalyst.After temperature drops to room temperature, take out, for subsequent use.Record by ICP: the ratio of carbon, nitrogen and iron atom is 10:4:0.5.By test, the hydrogen reduction take-off potential of the catalyst of present embodiment preparation and half wave potential are 20% Pt/C catalyst height than commercial platinum content.
0.1g BP 2000 and 2g melamine are put into the shimmy formula ball mill of high speed (Nanjing meaning sail, model GM-3B), high speed ball milling 10 hours.After the ball grinder temperature drops to room temperature, the mixed-powder that contains carbon, nitrogen and iron that obtains is placed common tube furnace, in 1.01 * 10
5Pa, 800 ℃ of lower high-temperature process 3 hours obtain iron, nitrogen co-doped carbon black catalyst, after temperature drops to room temperature, take out, and are for subsequent use.Record by ICP: the ratio of carbon, nitrogen and iron atom is 10:2:0.8.By test, the hydrogen reduction take-off potential of the catalyst of present embodiment preparation and half wave potential are 20% Pt/C catalyst height than commercial platinum content.
Comparative Examples
Be that to add the commercial Pt content of 1mg in 5% the Nafion solution be 20% Pt/C catalyst to 100 μ L mass concentrations, ultrasonic dispersion 30min obtains solution; Get the described solution of 10 μ L and drip and be applied on the rotating disk electrode (r.d.e), after room temperature is dried, obtain membrane electrode; With the SCE electrode as reference electrode, Pt sheet as the three-electrode system to electrode.Utilize rotating disk electrode (r.d.e) to carry out the test of linearity volt-ampere in the KOH solution of the 0.1mol/L that denitrogenates through oxygen, sweep speed is 5mV/s.
Among Fig. 3 31 is that 20% Pt/C catalyst is 1600 rpm at rotating speed for Pt content, the linear sweep voltammetry figure when sweeping speed for 5mv/s.By 31 as can be known, Comparative Examples Pt content is that the hydrogen reduction take-off potential of 20% Pt/C catalyst is 0mV, is starkly lower than the hydrogen reduction take-off potential of the catalyst of the embodiment of the invention 1 ~ 3 preparation.
Obviously, above-described embodiment only is for technical scheme example of the present invention clearly is described, and is not the restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here need not also can't give all embodiments exhaustive.And the apparent variation of being extended out thus or change still are among the protection domain of the invention.
Claims (9)
1. an iron, nitrogen co-doped carbon black catalyst is characterized in that this catalyst is to be prepared by following method:
(1) takes by weighing black pearl 2000 and melamine for 1:20 ~ 1:5 in mass ratio, put into the ball mill ball milling 3 ~ 10 hours, obtain containing the mixed-powder of carbon, nitrogen and iron;
(2) mixed-powder that contains carbon, nitrogen and iron that obtains in the step (1) is put into tube furnace, 800 ~ 1000 ℃ of lower processing 0.5 ~ 5 hour, obtain iron, nitrogen co-doped carbon black catalyst.
2. iron according to claim 1, nitrogen co-doped carbon black catalyst is characterized in that, the ratio of the carbon of described catalyst, nitrogen and iron atom is 10:1 ~ 5:0.5 ~ 1.
3. iron according to claim 2, nitrogen co-doped carbon black catalyst is characterized in that, the ratio of the carbon of described catalyst, nitrogen and iron atom is 10:3:1.
4. the preparation method of iron according to claim 1, nitrogen co-doped carbon black catalyst is characterized in that, this preparation method's concrete steps and condition are as follows:
(1) takes by weighing black pearl 2000 and melamine for 1:20 ~ 1:5 in mass ratio, put into the ball mill ball milling 3 ~ 10 hours, obtain containing the mixed-powder of carbon, nitrogen and iron;
(2) mixed-powder that contains carbon, nitrogen and iron that obtains in the step (1) is put into tube furnace, 800 ~ 1000 ℃ of lower processing 0.5 ~ 5 hour, obtain described iron, nitrogen co-doped carbon black catalyst.
5. preparation method according to claim 4 is characterized in that, the mass ratio of black pearl 2000 and melamine is 1:10 in the step (1).
6. preparation method according to claim 4 is characterized in that, the tube furnace in the step (2) is single warm area slide rail stove.
7. according to claim 4,5 or 6 described preparation methods, it is characterized in that the Ball-milling Time in the step (1) is 4 hours.
8. preparation method according to claim 7 is characterized in that, the treatment temperature in the step (2) is 900 ℃.
9. preparation method according to claim 8 is characterized in that, the processing time in the step (2) is 1 hour.
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