CN103920490B - A kind of platinum nano cubic block Catalysts and its preparation method of surfactant-free - Google Patents
A kind of platinum nano cubic block Catalysts and its preparation method of surfactant-free Download PDFInfo
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- CN103920490B CN103920490B CN201410133158.6A CN201410133158A CN103920490B CN 103920490 B CN103920490 B CN 103920490B CN 201410133158 A CN201410133158 A CN 201410133158A CN 103920490 B CN103920490 B CN 103920490B
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- cubic block
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 60
- 239000003054 catalyst Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000446 fuel Substances 0.000 claims abstract description 20
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000002245 particle Substances 0.000 claims abstract description 8
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 6
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 6
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 6
- 239000004094 surface-active agent Substances 0.000 claims abstract description 6
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 239000002243 precursor Substances 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 238000012546 transfer Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 150000003057 platinum Chemical class 0.000 claims 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 15
- 230000003197 catalytic effect Effects 0.000 abstract description 9
- 230000015572 biosynthetic process Effects 0.000 abstract description 8
- 238000003786 synthesis reaction Methods 0.000 abstract description 8
- 239000013078 crystal Substances 0.000 abstract description 6
- 230000003647 oxidation Effects 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- 238000002484 cyclic voltammetry Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 229910021645 metal ion Inorganic materials 0.000 abstract description 3
- 239000000654 additive Substances 0.000 abstract description 2
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 150000001298 alcohols Chemical class 0.000 description 2
- 239000011943 nanocatalyst Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- 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
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Abstract
The invention discloses the platinum nano cubic block Catalysts and its preparation method of a kind of surfactant-free of field of fuel cell technology.The method utilizes ascorbic acid in DMF solution, reduce platinum presoma, and high productivity prepares undersized platinum nano cubic block particle, and surface exposes is { 100} crystal face and abundant atomic steps.This method avoid the use of surfactant and other metal ion additives, make the platinum nano cubic block surface clean of synthesis, the specific area of catalyst and the activity of electro-catalysis can be improved in this surface totally.Using the anode catalyst of the platinum nano cubic block catalyst of the surfactant-free of preparation as alcohol fuel battery, in the catalytic oxidation process of alcohol, hydroxyl can be strengthened and adsorbs and promote catalytic activity, thus larger fuel cell output power can be brought.Cyclic voltammetry display in the KOH solution of methyl alcohol and ethanol, the peak oxidation current of this catalyst is respectively 2.2 and 1.6 times of commercial platinum/C catalyst.
Description
Technical field
The invention belongs to field of fuel cell technology, in particular, provide a kind of platinum nano cubic block Catalysts and its preparation method of surfactant-free.
Technical background
Fuel cell is a kind of chemical energy by fuel and oxygen reaction release is the cell apparatus of electric energy.Since 19th-century mid-term, after fuel cell is invented, the development of fuel cell technology seriously lags behind steam engine and the internal combustion engine of main flow.Until nearly decades, along with the growth of electricity needs, the exhaustion of petroleum resources, people to have restriked again enthusiasm to fuel cell.In pluralities of fuel battery, take alcohols as the direct alcohol fuel battery of fuel, obtain very large concern with its high-energy-density, high energy efficiency and lower operating temperature.
Alcohols (methyl alcohol, ethanol, ethylene glycol etc.) carries out under assistance normally at eelctro-catalyst of the oxidation of anode of fuel cell, is wherein main flow with platinum catalyst.The catalytic activity of but conventional platinum catalyst still can not meet business-like demand.Research shows, by changing particle size and the surface texture of platinum catalyst, can promote the activity of catalyst.Particularly platinum nano cubic block catalyst shows stronger catalytic activity and anti-poisoning capability relative to commercial platinum/C catalyst.But the multiple platinum nano cubic block reported, or size is comparatively large, or in building-up process, add surfactant or other metal ions as Morphological control agent.These factors all likely can cause the reduction of platinum catalyst performance.Particle is less than 5nm and the synthesis of the platinum nano cubic block of surfactant-free and do not see document and the patent report of association area as the application of alcohol fuel battery anode catalyst yet.
Summary of the invention
The object of the present invention is to provide a kind of platinum nano cubic block Catalysts and its preparation method of surfactant-free, to promote the electro catalytic activity of directly alcohol fuel battery anode at present, promote the power output of this fuel cell further.
Technical scheme of the present invention is: platinum presoma and ascorbic acid are reacted in DMF solution, and the metal platinum nanocatalyst surface of generation exists without extra surfactant.
Platinum nano cubic block catalyst Average Particle Diameters of the present invention is 3.5 ~ 3.9nm, and it has nano cubic block pattern and rich surface contains atomic steps and { 100} crystallite face; In building-up process, do not add surfactant and other metal precursor, make it have clean surface texture.
The preparation method of the platinum nano cubic block catalyst of surfactant-free of the present invention is: preparation contains the DMF solution of 5 ~ 20mM platinum presoma and 50 ~ 100mM ascorbic acid; Then transfer in the sealing stainless steel cauldron of band polytetrafluoroethylliner liner, react 10 ~ 20 hours at 150 ~ 200 DEG C of temperature; Question response still cool to room temperature, centrifugation obtains black precipitate, namely obtains the platinum nano cubic block catalyst of surfactant-free with ethanol centrifuge washing.
Described platinum presoma is potassium chloroplatinate or acetylacetone,2,4-pentanedione platinum.
In above-mentioned reaction, the consumption of ascorbic acid is larger, and desired reaction temperature is lower; Reaction temperature is higher, and the required reaction time is shorter.
Using the application of the platinum nano cubic block catalyst of the surfactant-free of above-mentioned preparation as the anode catalyst of alcohol fuel battery.
By above-mentioned prepared material:
1. carry out the platinum nano catalyst that TEM and HRTEM characterize display preparation and have the shape of cubic block, its particle size is about 3.5nm, and the granular size of this and commercial platinum/C catalyst is suitable.The interplanar distance of this nano cubic block and outer crystal plane be parallel is 0.195nm, with metal platinum { 200} interplanar distance is consistent, shows that the exposure crystal face of synthesized Pt nanoparticle is { 100} crystal face.In addition this photocatalyst crystals surface is containing abundant atomic steps;
2. carry out XRD and characterize the characteristic peak showing platinum, and by this catalyst particle size of Scherrer formulae discovery;
3. carry out cyclic voltammetry curve (CV) test in KOH solution, show that the surface of this catalyst has abundant { 100} crystallite face and the larger step atom of coordination degree of unsaturation;
4. carry out the CV test in the KOH solution of methyl alcohol, ethanol, show that this catalyst is compared with the platinum/C catalyst of commercialization, has higher catalytic activity.
The invention has the advantages that: utilize ascorbic acid in DMF solution, reduce platinum presoma, high productivity prepares undersized platinum nano cubic block particle, and surface exposes is { 100} crystal face and abundant atomic steps.This method avoid the use of surfactant and other metal ion additives, make the platinum nano cubic block surface clean of synthesis, the specific area of catalyst and the activity of electro-catalysis can be improved in this surface totally.Using the anode catalyst of the platinum nano cubic block catalyst of the surfactant-free of preparation as alcohol fuel battery, in the catalytic oxidation process of alcohol, hydroxyl can be strengthened and adsorbs and promote catalytic activity, thus larger fuel cell output power can be brought.Cyclic voltammetry display in the KOH solution of methyl alcohol and ethanol, the peak oxidation current of this catalyst is respectively 2.2 and 1.6 times of commercial platinum/C catalyst, demonstrates the stronger catalytic activity to methyl alcohol and ethanol.
Accompanying drawing explanation
Fig. 1 is the TEM image of the platinum nano cubic block catalyst of the surfactant-free obtained under the embodiment of the present invention 1 synthesis condition; Built-in scale is 50nm; Built-in illustration is domain size distribution statistical chart.
Fig. 2 is the XRD spectra of the platinum nano cubic block catalyst of the surfactant-free obtained under the embodiment of the present invention 1 synthesis condition; Abscissa is 2Theta, unit: degree; Ordinate is intensity.
Fig. 3 is platinum nano cubic block catalyst and the cyclic voltammogram of commercial platinum/C catalyst in 0.5MKOH solution of the surfactant-free obtained under the embodiment of the present invention 1 synthesis condition; Sweep speed: 50mV/s; Abscissa is voltage, unit: V; Ordinate is current density, unit: mA/cm
2.Wherein: a is made platinum catalyst; B is commercial platinum/C catalyst.
Fig. 4 is that the platinum nano cubic block catalyst of the surfactant-free obtained under the embodiment of the present invention 1 synthesis condition and commercial platinum/C catalyst are at 0.5MKOH+1MCH
3cV figure in OH solution; Sweep speed: 50mV/s; Abscissa is voltage, unit: V; Ordinate is current density, unit: mA/cm
2.Wherein: a is made platinum catalyst; B is commercial platinum/C catalyst.
Fig. 5 is that the platinum nano cubic block catalyst of the surfactant-free obtained under the embodiment of the present invention 1 synthesis condition and commercial platinum/C catalyst are at 0.5MKOH+1MCH
3cH
2cV figure in OH solution; Sweep speed: 50mV/s; Abscissa is voltage, unit: V; Ordinate is current density, unit: mA/cm
2.Wherein: a is made platinum catalyst; B is commercial platinum/C catalyst.
Detailed description of the invention
[embodiment 1]
Steps A: take 11.8mg acetylacetone,2,4-pentanedione platinum and 52.8mg ascorbic acid is dissolved in 6mlN, is configured to mixed solution in dinethylformamide (DMF) and stirs 10 minutes;
Step B: above-mentioned yellow solution is transferred in the sealing stainless steel cauldron of band polytetrafluoroethylliner liner, keep 16 hours at 150 DEG C of temperature;
Step C: after reaction terminates, question response still cool to room temperature, by the centrifugation 5 minutes under the rotating speed of 9000 revs/min of the solution of dark reddish brown wherein, obtain black product precipitation, the abundant centrifuge washing of product ethanol is separated 3 times.
Schemed from TEM, nano cubic block homogeneous sized by obtained Pt nanoparticle, its particle size is 3.50 ± 0.47nm, and the particle diameter of this and commercial platinum/carbon is suitable.In XRD figure, occurred three characteristic peaks of platinum, the nano cubic block size that larger peak width obtains is less.By Scherrer formulae discovery, its average crystal grain size is about 3.6nm.The CV image in 0.5MKOH solution by more made platinum nano cubic block and commercial platinum/carbon, can find that made platinum cubic block relates to hydrogen { peak of desorption is stronger on 100} crystal face, indicates a large amount of { existence in 100} crystallite face.By more made platinum nano cubic block and commercial platinum/carbon at 0.5MKOH+1MCH
3oH and 0.5MKOH+1MCH
3cH
2cV image in OH solution, can find that made platinum cubic block shows larger oxidative peak current.Its peak point current is respectively 2.2 and 1.6 times of commercial platinum/C catalyst.
[embodiment 2]
Steps A: take 11.8mg acetylacetone,2,4-pentanedione platinum and 52.8mg ascorbic acid and be dissolved in 6mlDMF and be configured to mixed solution and stir 10 minutes;
Step B: above-mentioned yellow solution is transferred in the sealing stainless steel cauldron of band polytetrafluoroethylliner liner, keep 10 hours at 180 DEG C of temperature;
Step C: after reaction terminates, question response still cool to room temperature, by the centrifugation 5 minutes under the rotating speed of 9000 revs/min of the solution of dark reddish brown wherein, obtain black product precipitation, the abundant centrifuge washing of product ethanol is separated 3 times.
Schemed from TEM, nano cubic block homogeneous sized by obtained Pt nanoparticle, its particle size is 3.42 ± 0.43nm, and the particle diameter of this and commercial platinum/carbon is suitable.In XRD figure, occurred three characteristic peaks of platinum, the nano cubic block size that larger peak width obtains is less.By Scherrer formulae discovery, its average crystal grain size is about 3.5nm.The CV image in 0.5MKOH solution by more made platinum nano cubic block and commercial platinum/carbon, can find that made platinum cubic block relates to hydrogen { peak of desorption is stronger on 100} crystal face, indicates a large amount of { existence in 100} crystallite face.By more made platinum nano cubic block and commercial platinum/carbon at 0.5MKOH+1MCH
3oH and 0.5MKOH+1MCH
3cH
2cV image in OH solution, can find that made platinum cubic block shows larger oxidative peak current.Its peak point current is respectively 2.1 and 1.7 times of commercial platinum/C catalyst.
[embodiment 3]
Steps A: take 14.5mg potassium chloroplatinate and 52.8mg ascorbic acid and be dissolved in 6mlDMF and be configured to mixed solution and stir 10 minutes;
Step B: above-mentioned yellow solution is transferred in the sealing stainless steel cauldron of band polytetrafluoroethylliner liner, keep 16 hours at 150 DEG C of temperature;
Step C: after reaction terminates, question response still cool to room temperature, by the centrifugation 5 minutes under the rotating speed of 9000 revs/min of the solution of dark reddish brown wherein, obtain black product precipitation, the abundant centrifuge washing of product ethanol is separated 3 times.
Schemed from TEM, nano cubic block homogeneous sized by obtained Pt nanoparticle, its particle size is 3.80 ± 0.68nm, and the particle diameter of this and commercial platinum/carbon is suitable.In XRD figure, occurred three characteristic peaks of platinum, the nano cubic block size that larger peak width obtains is less.By Scherrer formulae discovery, its average crystal grain size is about 3.9nm.The CV image in 0.5MKOH solution by more made platinum nano cubic block and commercial platinum/carbon, can find that made platinum cubic block relates to hydrogen { peak of desorption is stronger on 100} crystal face, indicates a large amount of { existence in 100} crystallite face.By more made platinum nano cubic block and commercial platinum/carbon at 0.5MKOH+1MCH
3oH and 0.5MKOH+1MCH
3cH
2cV image in OH solution, can find that made platinum cubic block shows larger oxidative peak current.Its peak point current is respectively 1.9 and 1.5 times of commercial platinum/C catalyst.
Claims (4)
1. a platinum nano cubic block catalyst, is characterized in that, this platinum nano cubic block catalyst Average Particle Diameters is 3.5 ~ 3.9nm, and it has nano cubic block pattern and rich surface contains atomic steps and { 100} crystallite face; In building-up process, do not add surfactant and other metal precursor, make it have clean surface texture.
2. a preparation method for the platinum nano cubic block catalyst of surfactant-free, it is characterized in that, its specific operation process is: preparation contains the DMF solution of 5 ~ 20mM platinum presoma and 50 ~ 100mM ascorbic acid; Then transfer in the sealing stainless steel cauldron of band polytetrafluoroethylliner liner, react 10 ~ 20 hours at 150 ~ 200 DEG C of temperature; Question response still cool to room temperature, centrifugation obtains black precipitate, namely obtains the platinum nano cubic block catalyst of surfactant-free with ethanol centrifuge washing.
3. the preparation method of the platinum nano cubic block catalyst of surfactant-free according to claim 2, is characterized in that, described platinum presoma is potassium chloroplatinate or acetylacetone,2,4-pentanedione platinum.
4. the platinum nano cubic block catalyst of the surfactant-free prepared according to the method in claim 2 or 3 is as the application of the anode catalyst of alcohol fuel battery.
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| CN105478794A (en) * | 2015-12-11 | 2016-04-13 | 中国科学院深圳先进技术研究院 | Platinum-copper alloy nano particle and preparation method thereof |
| CN106450350B (en) * | 2016-10-20 | 2019-04-30 | 绍兴文理学院 | A kind of synthetic method of platinum nano cubic block |
| CN107552044B (en) * | 2017-09-28 | 2020-04-28 | 中国科学院青岛生物能源与过程研究所 | Preparation method for effectively liquefying noble metal and improving electrocatalysis performance of noble metal |
| CN109848434B (en) * | 2019-01-21 | 2020-07-28 | 西安交通大学 | Preparation method of superfine platinum nanowire rich in twin crystal defects |
| US11331725B2 (en) * | 2019-07-19 | 2022-05-17 | Honda Motor Co., Ltd. | Synthetic method for preparing small palladium nanocubes |
| CN116072898A (en) * | 2021-10-29 | 2023-05-05 | 中国石油化工股份有限公司 | Platinum-carbon catalyst, preparation method and application thereof, and hydrogen fuel cell |
| CN114976077B (en) * | 2022-06-16 | 2024-03-01 | 南京师范大学 | Sub-2 nm ultra-small Pt nano cube array and preparation method and application thereof |
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| CN101100002A (en) * | 2006-07-06 | 2008-01-09 | 三星电机株式会社 | Method for producing metal nano granule |
| KR20100135423A (en) * | 2009-06-17 | 2010-12-27 | 연세대학교 산학협력단 | Shaped-controlled pt nanoparticles catalyst for fuel cell, and the method for the preparing the same |
| CN102078826A (en) * | 2010-12-24 | 2011-06-01 | 苏州方昇光电装备技术有限公司 | Preparation method and application of ionic liquid modified carbon sphere loaded platinum nanoparticle catalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101100002A (en) * | 2006-07-06 | 2008-01-09 | 三星电机株式会社 | Method for producing metal nano granule |
| KR20100135423A (en) * | 2009-06-17 | 2010-12-27 | 연세대학교 산학협력단 | Shaped-controlled pt nanoparticles catalyst for fuel cell, and the method for the preparing the same |
| CN102078826A (en) * | 2010-12-24 | 2011-06-01 | 苏州方昇光电装备技术有限公司 | Preparation method and application of ionic liquid modified carbon sphere loaded platinum nanoparticle catalyst |
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