CN103861583A - Platinum nanocrystal catalyst activity optimizing treatment method - Google Patents
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- CN103861583A CN103861583A CN201410076341.7A CN201410076341A CN103861583A CN 103861583 A CN103861583 A CN 103861583A CN 201410076341 A CN201410076341 A CN 201410076341A CN 103861583 A CN103861583 A CN 103861583A
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Abstract
The invention relates to a platinum nanocrystal catalyst activity optimizing treatment method. The method comprises the following steps: (1) synthesizing a Pt nanocrystal; (2) adding the Pt nanocrystal into a solvent and performing centrifugal separation purification; (3) adding the purified Pt nanocrystal into a carbon nano-tube and performing ultrasonic mixing, thereby obtaining a carbon nano-tube loaded Pt nanocrystal; and (4) heating the obtained sample in a tubular furnace to 100-800 DEG C, and performing heat treatment for 1 hour under an Ar atmosphere or an H2-Ar mixed atmosphere. The invention provides a new optimizing method for preparing an electrochemical oxygen-reduction catalyst by processing the Pt nanocrystal, i.e., on the basis of the existing crystal, the size of the Pt nanocrystal and the morphology of a crystal surface can be changed via a certain treatment approach, so that the excellent electrochemical catalyst is finally obtained and the activity of the catalyst is enhanced by 1-3 times than that of an untreated catalyst.
Description
Technical field
The present invention relates to the activity optimization processing method of Pt nanocrystal catalyst, thereby make its being widely used in electrochemical catalyst hydrogen reduction system field.
Background technology
At present, a lot of seminar have synthesized and have had difform Pt nanocrystal body by the method for colloidal state, for example cube, and truncated cube or cuboctahedron etc., this has separately warded off again a new road to the direction of catalyst.The size that the activity of catalyst not only depends on particle size also depends on the shape of nanocrystal.But, obtain effective catalytic property and must obtain the polymer of first removing nano grain surface, and a lot of catalytic reactions all occur at higher temperature.Therefore, application aspect in the future can need heatable catalyst, and for the activity of catalyst, the heat endurance that relates to the nanocrystal of change of shape is to be necessary very much research.
For the catalyst mixing, the interaction between metal and metallic carrier is particularly crucial aspect decision catalytic property.Especially the active metal heat endurance at higher temperature and change of shape on different carriers all needs by careful research, is all to occur at higher temperature just as a lot of practical catalytic reactions are applied in factory the inside.
Metallic particles at higher temperature, can be tending towards becoming spherical with reduce overall surface area and surface can become a general trend.Recently, Wang Zong woods seminar has reported the change of shape along with variations in temperature of Pt nanoparticle in amorphous carbon substrate, and they have shown that these nano particles can be melted or even be assembled the shape that forms similar ball by surface at higher temperature.
Now, fuel cell technology is very powerful and exceedingly arrogant in recent years as the skeleton of energy technology in the future.Fuel cell is the device that by electrochemical reaction, chemical energy is directly transformed into electric energy, although the transformation of hydrocarbon fuels is being to be worth paying much attention to aspect low-temperature fuel cell technological system energy density, but well-known, eelctro-catalyst can not provide considerable effective conversion efficiency and speed in actual applications.The kind of fuel cell has a lot, and alkaline fuel cell is to operate having in the hydrogen of pressure and oxygen, and they generally use potassium hydroxide aqueous solution as electrolyte, and efficiency is about 70%, and operating temperature is between 150 ℃ to 200 ℃; Carbonate fuel battery (MCFC) use of melting be the high temperature compound of carbonate as electrolyte, efficiency is 60% to 80%, operating temperature is 650 ℃; Phosphoric acid fuel cell (PAFC) use be phosphoric acid as electrolyte, efficiency is 40% to 80%, operating temperature is 150 ℃ to 200 ℃; Proton exchange membrane fuel cell (PEMFC) is a kind of thin permeable layer polymerization thing electrolyte of use, and efficiency is 40% to 50%, and operating temperature is 80 ℃; SOFC (SOFC) use be hard ceramic metal oxide (for example calcium, zinc) as electrolyte, efficiency is about 60%, operating temperature is about 1000 ℃.But, platinum based catalyst is considered to be in eelctro-catalyst best in proton exchange membrane fuel cell and phosphoric acid fuel cell, and carbon is the eelctro-catalyst of well-known hydroxide and hydrogen reduction as the platinum catalyst of carrier in phosphoric acid fuel cell and proton exchange membrane fuel cell.
Patent CN102641733A discloses a kind of method of preparing high catalytic activity Pt/CNTs material, the preparation of Pt/CNTs material comprises the steps: to adopt CNT as catalyst carrier, routine 1:1～4:1 weighs a certain amount of CNT and organic metal platinum compounds in mass ratio, then mix, heat again, heat time was 10～30 seconds, heating-up temperature is 250～400 ℃, make organic metal platinum compounds in carbon nano tube surface decomposes, formation has the Pt particle of catalytic activity, uniform load is in carbon nano tube surface, obtain Pt/CNTs catalyst material.
But, also do not occur using at present Pt nanocrystal body carried out to the method for a series of condition optimizing as good oxygen reduction catalyst.
Summary of the invention
The object of the invention is in order to overcome the deficiencies in the prior art, and a kind of activity optimization processing method of Pt nanocrystal catalyst is provided, the synthetic Pt nanocrystal body of the method utilization is as basis, to obtain the catalyst with good oxidation reducing activity.
For achieving the above object, the present invention adopts following technical proposals:
An activity optimization processing method for Pt nanocrystal catalyst, comprises that step is as follows:
(1) synthetic Pt is nanocrystalline;
(2) add centrifugation purifying in solvent by nanocrystalline Pt;
(3), by the Pt nanocrystal after purifying and mass ratio ultrasonic mix of CNT with 1:4-9, making platiniferous is the Pt nanocrystal body (Pt NCs-CNTs) on CNT that loads on of 10-20%;
(4) sample obtaining is put into tube furnace at H
2in-Ar mixed atmosphere or Ar atmosphere be warming up to 100-800 ℃, heat treated 1 hour in enclosing.
In said method, the nanocrystalline hydrothermal chemistry reducing process of preferably utilizing of Pt is synthetic, first in reactor, adds ethylene glycol, magneton, and temperature is adjusted to 190 ℃, after ebuillition of heated refluxes, then adds 2 × 10
-3the AgNO of M
3solution, immediately add molecular weight is the platinum acid chloride solution that 58000 polyvinylpyrrolidone and concentration are 62.5mM simultaneously, adds PVP and platinum acid chloride solution afterwards every 30s, until add, then boiling reflux 5-30min.In solution, presoma is H
2ptCl
66H
2o, coating agent is polyvinylpyrrolidone (PVP), in this method ethylene glycol be solvent be also reducing agent.PVP and H
2ptCl
66H
2o mass ratio is 12:1, AgNO
3solution, platinum acid chloride solution, ethylene glycol volume ratio are 1:3:5.
The described solvent of step (2) is one or more in acetone, ethanol or n-hexane.Centrifugal speed 3000-5000 rev/min.Preferably at 5000 revs/min of centrifugal 15min, supernatant is separated, gained sediment adds the acetone of three times, centrifugal 5min under 3000 revs/min again, collecting precipitation thing, in the ultrasonic ethanol that is dispersed in 3ml, then add n-hexane centrifugal 5min under 3000 revs/min of 9ml, last sediment is again at ethanol: in the mixed solvent in n-hexane=1:3, clean twice.
The described ultrasonic time of above-mentioned steps (3) is 10-30min.Step (4) tube furnace heating rate used is 10 ℃/min.
In step (4), be preferably warming up to 300 ℃.
In step (4), preferably in the time of 300 ℃, pass into H
2-Ar gaseous mixture, percent by volume 20%H
2, 80%Ar.Gas flow rate: 100ml/min.
Compared with prior art, the present invention proposes the nanocrystalline optimization method of preparing electrochemical oxygen reduction catalyst of a kind of new processing Pt, use on the basis of existing crystal, can change the nanocrystalline size of Pt, crystal face pattern and finally obtain good electrochemical catalyst, untreated front the raisings 1-3 of specific activity times by certain processing method.
Compared with patent CN102641733A, we obtain after support materials, material being carried out a series of heat treatment and having probed into the impact of different atmosphere on material activity, optimal conditions, and there is good stability.Can find out from the data obtained, in this series of processing procedure, load on Pt nanocrystal body on CNT along with the variation of pattern and size has occurred in the rising of temperature, therefore, affect its hydrogen reduction activity thereby this processing method is the situation of arranging that loads on the pt atom on CNT by regulation and control, specific activity simple thermal treatment improves 20%-80%.
The Pt nanocrystalline catalyst that the inventive method makes has good electro catalytic activity.Pt after optimization process is nanocrystalline has very large potential using value and huge market efficiency in fields such as fuel cells.The Pt nanocrystalline catalyst that this optimization method finally obtains, has larger active area, can obtain higher hydrogen reduction activity.
Accompanying drawing explanation
Figure 1A is the synthetic brilliant HRTEM of Pt and TEM figure.
Figure 1B is HRTEM and the TEM figure of synthetic Pt NCs-CNTs.
Fig. 1 C is 20%H
2in-80%Ar, process HRTEM and the TEM figure of the Pt NCs-CNTs after 1h for 100 ℃.
Fig. 1 D is 20%H
2in-80%Ar, process HRTEM and the TEM figure of the Pt NCs-CNTs after 1h for 200 ℃.
Fig. 1 E is 20%H
2in-80%Ar, process HRTEM and the TEM figure of the Pt NCs-CNTs after 1h for 300 ℃.
Fig. 1 F is 20%H
2in-80%Ar, process HRTEM and the TEM figure of the Pt NCs-CNTs after 1h for 400 ℃.
Fig. 1 G is 20%H
2in-80%Ar, process HRTEM and the TEM figure of the Pt NCs-CNTs after 1h for 600 ℃.
Fig. 1 H is 20%H
2in-80%Ar, process HRTEM and the TEM figure of the Pt NCs-CNTs after 1h for 800 ℃.
Fig. 1 I is that in pure Ar, 300 ℃ of HRTEM and TEM that process the Pt NCs-CNTs after 1h scheme.
The CV figure contrast of Fig. 2 to be that synthetic Pt is nanocrystalline load on CNT with it after.
Under Fig. 3 A different temperatures at 20%H
2the CV figure that processes the Pt NCs-CNTs after 1h in-80%Ar, a in illustration, without Overheating Treatment Pt NCs-CNTs b, 100 ℃ of c, 300 ℃ of d, 400 ℃.
Under Fig. 3 B different temperatures at 20%H
2the RRDE of Pt NCs-CNTs after treatment figure in-80%Ar.A in illustration, without Overheating Treatment Pt NCs-CNTs b, 100 ℃ of c, 300 ℃ of d, 400 ℃.
Fig. 4 A is Ar and 20%H at 300 ℃
2-80%Ar processes the CV comparison diagram a of the Pt NCs-CNTs after 1h, Ar b, 20%H
2-80%Ar.
Fig. 4 B is Ar and 20%H at 300 ℃
2the RRDE figure of the Pt NCs-CNTs that-80%Ar processes, a, Ar b, 20%H
2-80%Ar.
Fig. 5 A is the ADT figure of nonheat-treated Pt NCs-CNTs.
At Fig. 5 B100 ℃ at 20%H
2the ADT of Pt NCs-CNTs after treatment figure in-80%Ar.
Fig. 5 C is at 20%H at 200 ℃
2the ADT of Pt NCs-CNTs after treatment figure in-80%Ar.
Fig. 5 D is at 20%H at 300 ℃
2the ADT of Pt NCs-CNTs after treatment figure in-80%Ar.
Fig. 5 E is at 20%H at 400 ℃
2the ADT of Pt NCs-CNTs after treatment figure in-80%Ar.
Fig. 5 F is at 20%H at 600 ℃
2the ADT of Pt NCs-CNTs after treatment figure in-80%Ar.
Fig. 6 is at 20%H
2aging front and back after treatment Data Comparison block diagram under-80%Ar different temperatures.
The specific embodiment
Below by specific embodiment, the present invention will be further elaborated, should be noted that following explanation is only in order to explain the present invention, does not limit its content.In embodiment, raw materials used and reagent is commercially available prod.
Embodiment 1:
Prepare Pt nanocrystal body, concrete preparation process is as follows:
2.5ml ethylene glycol backflow 5min, adds 0.5ml2 × 10
-3m AgNO
3solution, then, by 93.8 μ L0.375M polyvinylpyrrolidones (3mL altogether, polyvinylpyrrolidone/platinic acid=12:1) and 46.9 μ L0.0625M H
2ptCl
6.6H
2o (1.5mL altogether) solution (solvent is ethylene glycol) joins in the ethylene glycol of boiling every 30s in 16min, the final mixture 5min that refluxes again, product is centrifugal 15min under 5000 revs/min, supernatant is separated, gained sediment adds the acetone of three times, centrifugal 5min under 3000 revs/min again, collecting precipitation thing, in the ultrasonic ethanol that is dispersed in 3ml, then the n-hexane centrifugal 5min under 3000 revs/min that adds 9ml, last sediment is again at ethanol: in the mixed solvent in n-hexane=1:3, clean twice.Finally, sediment is dispersed in the water of 18ml, ultrasonic 20min.The Pt of synthesized is nanocrystalline to be characterized by high-resolution transmission electron microscope, as shown in Figure 1A.
The preparation of 20%Pt NCs-CNTs: above synthetic Pt nanocrystal solution mixes with CNT (mass ratio is 1:4), and ultrasonic 20min obtains 20%Pt NCs-CNTs, and it characterizes as shown in Figure 1B.
With the sample of the present embodiment gained, making containing Pt concentration is 1mg/ml sample, measuring 1ul drips and is applied to glass-carbon electrode surface, dry, drip the cation-exchange membrane of a nafion(polytetrafluoroethylene (PTFE) that is coated with 0.5ul0.5%) solution fixed sample, (glass-carbon electrode of made sample modification is working electrode, and Pt is to electrode, Hg/HgSO to adopt three-electrode system
4electrode is reference electrode), at H
2sO
4and H
2o
2in mixed liquor, process 20min, in sour environment, carry out cyclic voltammetry scan.
Experimental result is recorded in Figure of description 2 can be found out from figure cyclic voltammetry curve result, and after Pt nanocrystal is loaded on CNT, hydrogen reduction activity is increased to original 1.5 times.
Embodiment 2:
At different temperatures 20%H
2the 20%Pt NCs-CNTs that-80%Ar atmosphere Processing Example 1 makes: gained 20%PtNCs-CNTs is placed in quartz boat, quartz boat is put into quartz ampoule, then quartz ampoule is put into tube furnace, 20%H
2in heating up with the speed of 10 ℃/min in-80%Ar atmosphere from 100 ℃ to 800 ℃ different temperatures heat treated 1h.Gained sample characterization as Fig. 1 C, D, E, F, G, H, as shown in.
With 20%Pt NCs-CNTs sample after treatment in the present embodiment, making containing Pt concentration is 1mg/ml sample, measuring 1ul drips and is applied to glass-carbon electrode surface, dry, drip the nafion solution fixed sample that is coated with 0.5ul0.5%, (glass-carbon electrode of made sample modification is working electrode, and Pt is to electrode, Hg/HgSO to adopt three-electrode system
4electrode is reference electrode), at H
2sO
4and H
2o
2in mixed liquor, process 20min, in sour environment, carry out cyclic voltammetry scan.Experimental result is recorded in Figure of description 3A, cyclic voltammetry curve result can be found out, is 300 ℃ through the preferred temperature of a series of Temperature Treatment.
With the 20%Pt NCs-CNTs sample of the present embodiment processing, making containing Pt concentration is 1mg/ml sample, measuring 1ul drips and is applied to glass-carbon electrode surface, dry, drip the nafion solution fixed sample that is coated with 0.5ul0.5%, (glass-carbon electrode of made sample modification is working electrode, and Pt is to electrode, Hg/HgSO to adopt three-electrode system
4electrode is reference electrode), at H
2sO
4and H
2o
2in mixed liquor, process 20min, in sour environment, be rotated ring-disc electrode test.Experimental result is recorded in Figure of description 3B curve result can be found out, through a series of Temperature Treatment 20%H
2-80%Ar processes, and hydrogen reduction take-off potential the most just, illustrates that oxygen reduction reaction speed is the fastest, the H that intermediate product obtains at 300 ℃
2o
2productive rate also minimum.
The 20%Pt NCs-CNTs sample of processing with embodiment 2, making containing Pt concentration is 1mg/ml sample, measuring 1ul drips and is applied to glass-carbon electrode surface, dry, drip the nafion solution fixed sample that is coated with 0.5ul0.5%, (glass-carbon electrode of made sample modification is working electrode, and Pt is to electrode, Hg/HgSO to adopt three-electrode system
4electrode is reference electrode), at H
2sO
4and H
2o
2in mixed liquor, process 20min, in sour environment, carry out cyclic voltammetric rapid scanning degradation data.Experimental result is recorded in Figure of description 5A, B, C, D, E, F can find out from figure cyclic voltammetry curve result, through a series of Temperature Treatment 20%H
2-80%Ar processes, 20%H at 300 ℃
2in-80%Ar through almost not losing under 10000 scan cycle.Its result can be very clear by Fig. 6.This enforcement has further been verified at 300 ℃ at 20%H
2the 20%PtNCs-CNTs sample of processing in-80%Ar has good stability.
The 20%Pt NCs-CNTs that Ar atmosphere Processing Example 1 makes at 300 ℃: gained 20%Pt NCs-CNTs is placed in quartz boat, quartz boat is put into quartz ampoule, again quartz ampoule is put into tube furnace, in Ar atmosphere, be warming up to 300 ℃ of heat treated 1h with the speed of 10 ℃/min, its sample characterization is as Fig. 1 I.
With the 20%PtNCs-CNTs sample of gained under same temperature in 20%Pt NCs-CNTs sample after treatment and embodiment 2 in the present embodiment, making containing Pt concentration is 1mg/ml sample, measuring 1ul drips and is applied to glass-carbon electrode surface, dry, drip the nafion solution fixed sample that is coated with 0.5ul0.5%, (glass-carbon electrode of made sample modification is working electrode, and Pt is to electrode, Hg/HgSO to adopt three-electrode system
4electrode is reference electrode), at H
2sO
4and H
2o
2in mixed liquor, process 20min, in sour environment, carry out cyclic voltammetry scan.Experimental result is recorded in Figure of description 4A cyclic voltammetry curve result can be found out, 20%H
2-80%Ar atmosphere is better than the effect of Ar atmosphere processing.
With the 20%PtNCs-CNTs sample of gained under same temperature in 20%Pt NCs-CNTs sample after treatment and embodiment 2 in the present embodiment, making containing Pt concentration is 1mg/ml sample, measuring 1ul drips and is applied to glass-carbon electrode surface, dry, drip the nafion solution fixed sample that is coated with 0.5ul0.5%, (glass-carbon electrode of made sample modification is working electrode, and Pt is to electrode, Hg/HgSO to adopt three-electrode system
4electrode is reference electrode), at H
2sO
4and H
2o
2in mixed liquor, process 20min, in sour environment, be rotated ring-disc electrode test.Experimental result is recorded in Figure of description 4B curve result can be found out, 20%H
2-80%Ar atmosphere sample oxygen reduction reaction after treatment speed is faster than the processing of Ar atmosphere, and the intermediate product H producing
2o
2also few.
20%H at 300 ℃
2-80%Ar atmosphere is processed 10%Pt NCs-CNTs:: Pt nanocrystal solution is placed in quartz boat, quartz boat is put into quartz ampoule, then quartz ampoule is put into tube furnace, 20%H with CNT (mass ratio is 1:9) gained 10%Pt NCs-CNTs
2in-80%Ar atmosphere, be warming up to 300 ℃ of heat treated 1h with the speed of 10 ℃/min.
Claims (8)
1. an activity optimization processing method for Pt nanocrystal catalyst, is characterized in that, comprises that step is as follows:
(1) synthetic Pt is nanocrystalline;
(2) add centrifugation purifying in solvent by nanocrystalline Pt;
(3), by the Pt nanocrystal after purifying and mass ratio ultrasonic mix of CNT with 1:4-9, making platiniferous is the Pt nanocrystal body on CNT that loads on of 10-20%;
(4) sample obtaining is put into tube furnace at H
2in-Ar mixed atmosphere or Ar atmosphere be warming up to 100-800 ℃, heat treated 1 hour in enclosing.
2. the activity optimization processing method of a kind of Pt nanocrystal catalyst according to claim 1, is characterized in that, the nanocrystalline hydrothermal chemistry reducing process of utilizing of Pt is synthetic.
3. the activity optimization processing method of a kind of Pt nanocrystal catalyst according to claim 2, is characterized in that, described hydrothermal chemistry reducing process is for first adding ethylene glycol in reactor, and magneton, after ebuillition of heated refluxes, then adds 2 × 10
-3the AgNO of M
3solution, add subsequently molecular weight is the platinum acid chloride solution that 58000 polyvinylpyrrolidone and concentration are 62.5mM in batches simultaneously, until add, then boiling reflux 5-30min.
4. the activity optimization processing method of a kind of Pt nanocrystal catalyst according to claim 1, is characterized in that step
(2) described solvent is one or more in acetone, ethanol or n-hexane.
5. the activity optimization processing method of a kind of Pt nanocrystal catalyst according to claim 1, is characterized in that, the described ultrasonic time of step (3) is 10-30min.
6. the activity optimization processing method of a kind of Pt nanocrystal catalyst according to claim 1, is characterized in that, step (4) tube furnace heating rate used is 10 ℃/min.
7. the activity optimization processing method of a kind of Pt nanocrystal catalyst according to claim 1, is characterized in that, in step (4), is warming up to 300 ℃.
8. the activity optimization processing method of a kind of Pt nanocrystal catalyst according to claim 1, is characterized in that, is in the time of 300 ℃, to pass into H in step (4)
2-Ar gaseous mixture, percent by volume 20%H
2, 80%Ar.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040087441A1 (en) * | 2002-10-29 | 2004-05-06 | Christina Bock | Platinum based nano-size catalysts |
| CN1803292A (en) * | 2005-12-19 | 2006-07-19 | 华南理工大学 | Carbon-carried platinum-based catalyst for fuel cell and its preparation method |
| CN101890347A (en) * | 2009-05-19 | 2010-11-24 | 中国科学院理化技术研究所 | Method for preparing proton exchange membrane fuel cell supported catalyst |
| CN102773095A (en) * | 2012-08-03 | 2012-11-14 | 上海锦众信息科技有限公司 | Method for preparing platinum-based catalyst for fuel cell |
-
2014
- 2014-03-04 CN CN201410076341.7A patent/CN103861583B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040087441A1 (en) * | 2002-10-29 | 2004-05-06 | Christina Bock | Platinum based nano-size catalysts |
| CN1803292A (en) * | 2005-12-19 | 2006-07-19 | 华南理工大学 | Carbon-carried platinum-based catalyst for fuel cell and its preparation method |
| CN101890347A (en) * | 2009-05-19 | 2010-11-24 | 中国科学院理化技术研究所 | Method for preparing proton exchange membrane fuel cell supported catalyst |
| CN102773095A (en) * | 2012-08-03 | 2012-11-14 | 上海锦众信息科技有限公司 | Method for preparing platinum-based catalyst for fuel cell |
Non-Patent Citations (1)
| Title |
|---|
| HYUNJOON SONG，ET AL: "Pt Nanocrystals: Shape Control and Langmuir-Blodgett Monolayer Formation", 《J. PHYS. CHEM. B》, vol. 109, no. 1, 1 December 2004 (2004-12-01), pages 188 - 193 * |
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