CN102078816A - Selenium/carbon compound material, preparation of selenium/carbon compound material and application of selenium/carbon compound material in fuel-cell catalyst preparation - Google Patents
Selenium/carbon compound material, preparation of selenium/carbon compound material and application of selenium/carbon compound material in fuel-cell catalyst preparation Download PDFInfo
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- CN102078816A CN102078816A CN2010106014283A CN201010601428A CN102078816A CN 102078816 A CN102078816 A CN 102078816A CN 2010106014283 A CN2010106014283 A CN 2010106014283A CN 201010601428 A CN201010601428 A CN 201010601428A CN 102078816 A CN102078816 A CN 102078816A
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Abstract
The invention provides a novel catalyst carrier, namely, a selenium/carbon compound material, belonging to the technical field of compound materials. The selenium/carbon compound material has good dispersibility on metal nano particles, and selenium ion contained in the selenium/carbon compound material has a promotion effect on metal nano particles loaded on the selenium/carbon compound material, thus the selenium/carbon compound material as a catalyst carrier can be applied to preparation of fuel cell electrode catalysts. The fuel cell electrode catalyst prepared based on the selenium/carbon compound material as the carrier has good catalytic activity and stability in the reaction of a fuel cell as compared with the catalyst prepared based on the traditional carbon powder as the carrier, and the activity and utilization of active nano particle are greatly improved, thereby achieving the purpose of reducing the use amount of noble metal and catalyst cost and prolonging the service life of the catalyst.
Description
Technical field
The invention belongs to technical field of composite materials, relate to a kind of selenium/carbon composite and preparation method thereof; The present invention also relates to this composite simultaneously as the application of catalyst carrier in the preparation electrode catalyst of fuel cell.
Background technology
Fuel cell is a kind ofly without burning and directly by the electrochemical reaction mode chemical energy in the fuel to be converted into the TRT of electric energy, is a kind of green energy resource technology.As a kind of new and effective alternative energy source, fuel cell is not limited by Carnot cycle, has the high and low noise pollution of environmental friendliness, energy conversion efficiency, specific energy height, advantage such as simple to operate, easy to use.Because its excellent characteristic makes it be widely used in space flight, submarine, mobile phone, automobile, power generating equipment etc.
Electrode catalyst is the important part of fuel cell, directly influences fuel cell performance, efficient, stability and service life.At present, used eelctro-catalyst mainly is metallic catalysts such as Pt, Pd, Rh, Ag, Ru.Wherein the Pt metal has the d electron orbit that does not fill up, and the surface is the adsorption reaction thing very easily, and intensity is moderate, help forming highly active intermediate product, simultaneously, also having good characteristics such as high temperature resistant, anti-oxidant, corrosion-resistant, is one of present most widely used electrode catalyst.But metal Pt is a rare metal, costs an arm and a leg, and intermediate product such as the CO that is produced in the course of reaction very easily makes catalyst poisoning and loses catalytic activity.Thereby, seek to have high catalytic activity, resisting CO poison, and cheap new catalyst has crucial meaning.
In catalyst, material with carbon element has obtained to use widely as carrier, and the very big specific surface that they had helps improving the decentralization of catalyst activity component, and then obtains higher electro-chemical activity surface.Wherein Vulcan XC-72 is extensive use of the most that (the BET surface area is 254m with the most successful carbon support material
2/ g, electricity lead and are 0.25S/cm).But test finds that carbon carrier has a lot of deficiencies, for example: easily reunite, the porosity is low, add structure destructible in man-hour, thereby influence the performance etc. of catalyst.Therefore the research of development of new carbon carrier had got showing great attention to of people.
Summary of the invention
The objective of the invention is in order to overcome problems of the prior art, a kind of new fuel cell electrode catalyst agent carrier---selenium/carbon composite is provided.
Another object of the present invention provides a kind of preparation method of selenium/carbon composite.
A further object of the invention just provides the application of this selenium/carbon composite in the preparation electrode catalyst of fuel cell.
The preparation method of selenium/carbon composite of the present invention is that selenium and the triphenyl phosphorus mol ratio with 1:1 ~ 1:10 is joined in the organic solvent, stirs it is dissolved fully; The carbon dust that adds 5 ~ 50 times of selenium quality again, stirring is ultrasonic down fully to disperse it; Remove and desolvate, dry under the room temperature, get selenium/triphenyl phosphorus/carbon composite precursor; Then with selenium/triphenyl phosphorus/carbon composite precursor under inert gas shielding, in 200 ~ 1000 ℃ of following carbonization treatment 1 ~ 6 hour, obtain graphited selenium/carbon composite.
Described organic solvent is an oxolane.
Characterize the structure of composite and supported catalyst below by x-ray diffraction pattern (XRD).
Fig. 1 is CSe
x, XC-72, Se XRD figure, Fig. 2 is Pt/C and Pt/CSe
xThe XRD figure of catalyst.By Fig. 5 and Fig. 6 selenium/carbon composite of above-mentioned preparation as can be seen, be to be matrix with carbon, selenium is dispersed in the matrix of carbon.From Fig. 6, can be clearly seen that Pt/CSe
xWith four crystal faces (111) of Pt among the Pt/C, (200), (220) and (311).The doping of selenium has facilitation to loaded with nano metallic particles dispersiveness.And the selenium atom that wherein contains also has facilitation to the catalysis of the metal nanoparticle of load on it, thereby, as support applications in the preparation electrode catalyst of fuel cell.
For characterizing the performance of this catalyst excellence, be prepared as the catalyst (Pt/CSe that carries platinum 20 wt %
x), and compare with the catalyst (Pt/C) of conventional carriers carbon dust preparation.Concrete sign is as follows:
Fig. 3 is for being the catalyst Pt/CSe of preparing carriers with selenium/carbon composite of the present invention
xX-ray energy dispersion spectrum (EDX) figure.As can be seen from Figure 3, contain C, Pt and Se element in the composite, wherein do not contain the P P elements, the carrier that preparation is described is the composite that Se-C forms.
Fig. 4 is under the 200 kV conditions for being the catalyst use Tecnai G220 STWIN transmission electron microscope of preparing carriers with selenium/carbon composite of the present invention at accelerating potential, observes Pt/CSe
xThe pattern of catalyst.Wherein A figure is Pt/CSe
xScale is the transmission electron microscope picture of 50nm; B figure is scale Pt/CSe when being 5nm
xThe high power transmission electron microscope picture.From 4 figure as can be seen, the Pt catalyst granules is dispersed in selenium/carbon complex carrier surface uniformly, and the Pt catalyst granules is uniformly dispersed and particle is little.
Fig. 5 is Pt/C and Pt/CSe
xCatalyst is at 0.5M H
2SO
4Cyclic voltammetric resolution chart in the solution.As can be seen from Figure 5, in the cyclic voltammetric test, the Pt/CSe of identical carrying capacity metal
xCatalyst and Pt/C catalyst electrochemistry specific area are more or less the same.Selenium/carbon composite slightly is better than conventional carriers carbon dust Vulcan XC-72 as the catalyst of preparing carriers.
Fig. 6 is Pt/C and Pt/CSe
xAt 0.5M CH
3OH/H
2SO
4The cyclic voltammetric resolution chart of methanol oxidation in the solution.As can be seen from Figure 6, under identical noble metal carrying capacity, Pt/CSe of the present invention
xCatalyst reaches 2.14mA to the oxidization of methanol peak current, and the oxidation peak current of the Pt/C catalyst of conventional carriers preparation only has 1.70mA.Selenium/carbon carrier that the present invention preparation is described has cooperative effect to the nano-catalytic particle of load on it, can strengthen its catalytic effect.
In sum, the electrode catalyst of fuel cell that with advanced composite material (ACM) of the present invention is preparing carriers is the catalyst of preparing carriers with respect to traditional carbon dust, in the reaction of fuel cell, has better catalytic activity and stability, increase substantially the activity and the utilization rate of active nano particle, thereby realized reducing the use amount of noble metal and the purpose of catalyst cost, and had longer service life.
Description of drawings
Fig. 1 is CSe
x, XC-72, Se the XRD resolution chart.
Fig. 2 is Pt/C and Pt/CSe
xThe XRD resolution chart of catalyst.
Fig. 3 is the corresponding Pt/CSe of selenium/carbon composite as preparing carriers
xCatalyst EDX figure.
Fig. 4 is the corresponding Pt/CSe of selenium/carbon composite as preparing carriers
xThe catalyst transmission electron microscope picture.
Fig. 5 is that selenium/carbon composite and carbon dust Vulcan XC-72R are respectively as the corresponding Pt/C and the Pt/CSe of preparing carriers
xCatalyst is at 0.5 M H
2SO
4Cyclic voltammetric resolution chart in the solution.
Fig. 6 is that selenium/carbon composite and carbon dust Vulcan XC-72R are respectively as the corresponding Pt/C and the Pt/CSe of preparing carriers
xCatalyst is at 0.5 M CH
3OH/H
2SO
4Cyclic voltammetric resolution chart in the solution.
The specific embodiment
Be described further below by the preparation of instantiation, and be example, composite that the present invention the prepares facilitation to the catalytic nanometer particle be described with load platinum catalyticing anode methanol oxidation reaction to composite of the present invention.
Embodiment 1
(1) selenium/carbon composite (CSe
x) preparation
In 100 ml round-bottomed flasks, the triphenyl phosphorus of 2g is joined in the oxolane of 50ml, stir, triphenyl phosphorus is dissolved fully; Add the 100mg selenium powder then, continue stirring, ultrasonic; Add the 1g carbon dust again, continue about stirring, ultrasonic 10min it to be uniformly dispersed, revolve steaming oxolane is removed, dry under room temperature, get selenium/triphenyl phosphorus/carbon precursor.
Selenium/triphenyl phosphorus/carbon precursor is placed tube furnace, under nitrogen protection,, get graphitization selenium/carbon carrier (CSe in 200 ℃ of heat treatments 6 hours
x).
(2) preparation of loaded Pt catalyst
Chloroplatinic acid 66 mg are joined in the 100 ml round-bottomed flasks, add 30 ml ethylene glycol, and add the magneton stirring, it was dissolved fully in ultrasonic 0.5 hour under stirring; PH value with 4 ~ 5%KOH/EG solution regulator solution is about 8 ~ 9, adds graphitization selenium/carbon carrier (CSe of above-mentioned preparation then
x) 100 mg, stirred 0.5 hour earlier, after ultrasonic again 0.5 hour, at 160 ℃ of back flow reaction 6 h.Gained solution suction filtration, with three water washings, 60 ℃ are dried to weight.
In the loaded Pt catalyst, Pt and CSe
xMass ratio be 1:4.
Pt/CSe
xThe current density that catalyst unit mass metal produces is 268 A/g, and commercial Pt/C catalyst improves 26%.
Embodiment 2
(1) selenium/carbon composite (CSe
x) preparation
In 200 ml round-bottomed flasks, the triphenyl phosphorus of 3.3g is joined in the oxolane of 100ml, stir, triphenyl phosphorus is dissolved fully; Add the 200mg selenium powder then, continue stirring, ultrasonic; Add the 1g carbon dust again, continue about stirring, ultrasonic 20min it to be uniformly dispersed, revolve to steam and remove oxolane, dry under room temperature, get selenium/triphenyl phosphorus/carbon precursor.
Selenium/triphenyl phosphorus/carbon precursor is placed tube furnace, under nitrogen protection,, get graphitization selenium/carbon carrier (CSe in 800 ℃ of heat treatments 5 hours
x).
(2) preparation of loaded Pt catalyst
Chloroplatinic acid 17 mg are joined in the 100 ml round-bottomed flasks, add 30 ml ethylene glycol, and add the magneton stirring, it was dissolved fully in ultrasonic 0.5 hour under stirring; PH value with 4 ~ 5%KOH/EG solution regulator solution is about 8 ~ 9, adds graphitization selenium/carbon carrier (CSe of above-mentioned preparation then
x) 100 mg, stirred 0.5 hour earlier, after ultrasonic again 0.5 hour, at 160 ℃ of back flow reaction 6 h.Gained solution suction filtration, with three water washings, 60 ℃ are dried to weight.
In the loaded Pt catalyst, Pt and CSe
xMass ratio be 1:6.
Pt/CSe
xCurrent density 235 A/g that catalyst unit mass metal produces, commercial Pt/C catalyst improves 10%.
Embodiment 3
(1) selenium/carbon composite (CSe
x) preparation
In 100 ml round-bottomed flasks, the triphenyl phosphorus of 2g is joined in the oxolane of 30ml, stir, triphenyl phosphorus is dissolved fully; Add the 300mg selenium powder then, continue stirring, ultrasonic; Add the 1g carbon dust again, continue about stirring, ultrasonic 60min it to be uniformly dispersed, revolve to steam and remove oxolane, dry under room temperature, get selenium/triphenyl phosphorus/carbon precursor.
Selenium/triphenyl phosphorus/carbon precursor is placed tube furnace, under nitrogen protection,, get graphitization selenium/carbon carrier (CSe in 900 ℃ of heat treatments 4 hours
x).
(2) preparation of loaded Pt catalyst
Chloroplatinic acid 10 mg are joined in the 100 ml round-bottomed flasks, add 30 ml ethylene glycol, and add the magneton stirring, it was dissolved fully in ultrasonic 0.5 hour under stirring; PH value with 4 ~ 5%KOH/EG solution regulator solution is about 8 ~ 9, adds graphitization selenium/carbon carrier (CSe of above-mentioned preparation then
x) 100 mg, stirred 0.5 hour earlier, after ultrasonic again 0.5 hour, at 160 ℃ of back flow reaction 6h.Gained solution suction filtration, with three water washings, 60 ℃ are dried to weight.
In the loaded Pt catalyst, Pt and CSe
xMass ratio be 1:10.
Pt/CSe
xThe current density that catalyst unit mass metal produces is 223 A/g, and commercial Pt/C catalyst improves 5%.
Claims (4)
1. the preparation method of selenium/carbon composite is that selenium and the triphenyl phosphorus mol ratio with 1:1 ~ 1:10 is joined in the organic solvent, stirs it is dissolved fully; The carbon dust that adds 5 ~ 50 times of selenium quality again, stirring is ultrasonic down fully to disperse it; Remove and desolvate, dry under the room temperature, get selenium/triphenyl phosphorus/carbon composite precursor; Then with selenium/triphenyl phosphorus/carbon composite precursor under inert gas shielding, in 200 ~ 1000 ℃ of following carbonization treatment 1 ~ 6 hour, obtain graphited selenium/carbon composite.
2. the preparation method of selenium/carbon composite according to claim 1, it is characterized in that: described organic solvent is an oxolane.
3. selenium/the carbon composite of method preparation according to claim 1, it is characterized in that: the mass ratio of selenium and carbon is 1:5 ~ 1:50.
According to claim 1 selenium/the carbon composite of method preparation as the application of catalyst carrier in the preparation fuel-cell catalyst.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102614880A (en) * | 2012-01-12 | 2012-08-01 | 西北师范大学 | Preparation and application of carbon-supported amorphous metallic nickel |
| CN105070892A (en) * | 2015-09-22 | 2015-11-18 | 中国科学院化学研究所 | Preparation method and application of selenium-carbon compound |
| CN104716345B (en) * | 2013-12-15 | 2017-05-24 | 中国科学院大连化学物理研究所 | Preparation method for fuel cell cathode catalyst |
| CN107305943A (en) * | 2016-04-25 | 2017-10-31 | 中国科学院苏州纳米技术与纳米仿生研究所 | Lithium ion battery graphite cathode material, its preparation method and application |
| JP2019510716A (en) * | 2016-02-17 | 2019-04-18 | トゥー‐シックス・インコーポレイテッド | Immobilized selenium, method for producing the same, and use of immobilized selenium in secondary battery |
| US10734638B2 (en) | 2015-09-22 | 2020-08-04 | Ii-Vi Delaware, Inc. | Immobilized selenium, a method of making, and uses of immobilized selenium in a rechargeable battery |
| CN111969194A (en) * | 2020-08-27 | 2020-11-20 | 广东工业大学 | Battery positive electrode material and preparation method and application thereof |
| US11588149B2 (en) | 2015-09-22 | 2023-02-21 | Ii-Vi Delaware, Inc. | Immobilized selenium in a porous carbon with the presence of oxygen, a method of making, and uses of immobilized selenium in a rechargeable battery |
| US11784303B2 (en) | 2015-09-22 | 2023-10-10 | Ii-Vi Delaware, Inc. | Immobilized chalcogen and use thereof in a rechargeable battery |
| US11870059B2 (en) | 2017-02-16 | 2024-01-09 | Consejo Superior De Investigaciones Cientificas (Csic) | Immobilized selenium in a porous carbon with the presence of oxygen, a method of making, and uses of immobilized selenium in a rechargeable battery |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102614880A (en) * | 2012-01-12 | 2012-08-01 | 西北师范大学 | Preparation and application of carbon-supported amorphous metallic nickel |
| CN104716345B (en) * | 2013-12-15 | 2017-05-24 | 中国科学院大连化学物理研究所 | Preparation method for fuel cell cathode catalyst |
| US11515518B2 (en) | 2015-09-22 | 2022-11-29 | Institute Of Chemistry, Chinese Academy Of Sciences | Immobilized selenium, a method of making, and uses of immobilized selenium in a rechargeable battery |
| US10340507B2 (en) | 2015-09-22 | 2019-07-02 | Institute Of Chemistry, Chinese Academy Of Sciences | Method of preparing and application of carbon selenium composites |
| US10734638B2 (en) | 2015-09-22 | 2020-08-04 | Ii-Vi Delaware, Inc. | Immobilized selenium, a method of making, and uses of immobilized selenium in a rechargeable battery |
| US11482698B2 (en) | 2015-09-22 | 2022-10-25 | Ii-Vi Delaware, Inc. | Immobilized selenium, a method of making, and uses of immobilized selenium in a rechargeable battery |
| CN105070892A (en) * | 2015-09-22 | 2015-11-18 | 中国科学院化学研究所 | Preparation method and application of selenium-carbon compound |
| US11588149B2 (en) | 2015-09-22 | 2023-02-21 | Ii-Vi Delaware, Inc. | Immobilized selenium in a porous carbon with the presence of oxygen, a method of making, and uses of immobilized selenium in a rechargeable battery |
| US11784303B2 (en) | 2015-09-22 | 2023-10-10 | Ii-Vi Delaware, Inc. | Immobilized chalcogen and use thereof in a rechargeable battery |
| US11843109B2 (en) | 2015-09-22 | 2023-12-12 | Ii-Vi Delaware, Inc. | Method of preparing and application of carbon-selenium composites |
| US12002948B2 (en) | 2015-09-22 | 2024-06-04 | Consejo Superior De Investigaciones Cientificas (Csic) | Immobilized selenium in a porous carbon with the presence of oxygen, a method of making, and uses of immobilized selenium in a rechargeable battery |
| JP2019510716A (en) * | 2016-02-17 | 2019-04-18 | トゥー‐シックス・インコーポレイテッド | Immobilized selenium, method for producing the same, and use of immobilized selenium in secondary battery |
| CN107305943A (en) * | 2016-04-25 | 2017-10-31 | 中国科学院苏州纳米技术与纳米仿生研究所 | Lithium ion battery graphite cathode material, its preparation method and application |
| US11870059B2 (en) | 2017-02-16 | 2024-01-09 | Consejo Superior De Investigaciones Cientificas (Csic) | Immobilized selenium in a porous carbon with the presence of oxygen, a method of making, and uses of immobilized selenium in a rechargeable battery |
| CN111969194A (en) * | 2020-08-27 | 2020-11-20 | 广东工业大学 | Battery positive electrode material and preparation method and application thereof |
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Application publication date: 20110601 |