CN1447468A - Method for preparing methanol oxidation electrode in direct methanol fuel cell - Google Patents
Method for preparing methanol oxidation electrode in direct methanol fuel cell Download PDFInfo
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- CN1447468A CN1447468A CN03117823A CN03117823A CN1447468A CN 1447468 A CN1447468 A CN 1447468A CN 03117823 A CN03117823 A CN 03117823A CN 03117823 A CN03117823 A CN 03117823A CN 1447468 A CN1447468 A CN 1447468A
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
Under aqueous solution containing platnum and ruthenium ions and in the electrode of carbon cloth or cloth or carbon paper with the substrate of using Nafion to glue the carbon carrier powder, platinum and ruthenium alloy is deposited on the carbon carrier powder, which contacts to the component of proton exchange membrane. With being water washed and electrochemistry activated, the methanol oxidation electrode is formed, carrying metal catalyst platnum and ruthenium. The invention possesses the advantages of simple technique, short production cycle, high catalysis activity and low cost. The direct methanol fuel cells made from the methanol oxidation electrode are widely applicable to electric automobile, portable electric device such as cameras, notebook computers and electric toys.
Description
One technical field
The present invention relates to the methanol oxidation electrode preparation method of direct methanol fuel cell.
Two background technologies
Direct methanol fuel cell (DMFC) is with methyl alcohol (CH
3OH) be the negative reaction material, air is an anode reactant matter.Methyl alcohol oxidation under the catalysis of battery cathode catalyst discharges electronics, carbon dioxide (CO
2) and proton (H
+).CO
2Be discharged in the middle of the atmosphere H
+Arrive anode through proton exchange membrane, electronics drives the load acting through external circuit, also flows to anode, airborne oxygen under the catalysis of anode catalyst, catch the electronics that arrives at through external circuit and with H from exchange membrane
+In conjunction with generating water (H
2O).When a battery produces current, get rid of CO
2And H
2O.With with H
2For the Proton Exchange Membrane Fuel Cells of fuel is compared, be the DMFC of fuel with methyl alcohol, because the fluid characteristics of methyl alcohol is convenient to storage, volumetric specific energy height, become the chemical power source that portable electric appts and electric automobile are praised highly the most.Yet, and H
2-O
2Fuel cell is compared, and the methyl alcohol anodic oxidation speed of DMFC is significantly less than H
2Anodic oxidation speed.Improving the speed of the anode-catalyzed oxidation of methyl alcohol, is the business-like key issue of DMFC.
The platinum ruthenium catalyst (PtRu/C) that with the carbon dust is carrier is the most common and the most effective methanol oxidation catalyst.Chinese patent CN1318873 A discloses a kind of " preparation method of nanometer electrical catalyst for protein exchange film fuel cell ", its preparation method comprises following each step: with the platinum ruthenium halogen compound aqueous solution is raw material, wherein platinum/ruthenium mol ratio is 1: 0.2-1, be dissolved in the beaker with deionized water, bullion content 0.5-10g/l, adding active carbon adsorbs, adjust its pH value 2.5-10.5 with alkaline solution, add redistilled water and be made into suspension, stir, be heated to 50-65 ℃, add the excessive 2.5-5 of relative noble metal molal quantity reducing agent doubly, keep temperature to continue to stir 1 hour with drip-injection method; With liquid filtering, washing was up to wherein there not being Cl when temperature dropped to room temperature
-The time till; 60-80 ℃ of following vacuumize, obtain the carried by active carbon noble metal catalyst PtRu/C of particle diameter 4 ± 0.5 nanometers.
The preparation method of the methanol oxidation electrode of existing DMFC is, with mixture or independent film forming or the brushing of isopropyl alcohol, ptfe emulsion (Teflon), Nafion solution and catalyst Pt Ru/C or be printed on the impregnated afflux utmost point of Teflon (carbon cloth or carbon paper), then with the proton exchange membrane electrolyte, air electrode hot pressing forms " electrode/membrane " assembly together.The H that methyl alcohol generates in the oxidation of negative pole Catalytic Layer
+Must pass mutually via the proton exchange membrane Nafion that mixes in the Catalytic Layer.Therefore, effectively catalyst is that those uninterruptedly are connected to dielectric film along the dielectric film direction by Nafion (ionic conduction phase) in Catalytic Layer, uninterruptedly is connected to the catalyst granules PtRu/C of gas diffusion layers by carbon granules (electron conduction phase) along afflux extreme direction.
The weak point of existing DMFC methanol oxidation electrode preparation method is: in the bonding PtRu/C of Nafion, in film formed of PtRu/C and the Nafion proton, because the mutual agglomeration of PtRu/C powder, part PtRu/C always can not contact with the Nafion proton exchange membrane, thereby becomes spent catalyst.Therefore, the Catalytic Layer of the Proton Exchange Membrane Fuel Cells of the method preparation of the bonding PtRu/C of usefulness Nafion, the utilance of noble metal catalyst PtRu is not high.
Three summary of the invention
The object of the present invention is to provide a kind of direct methanol fuel cell methanol oxidation electrode preparation method.It is simple that the present invention has technology, with short production cycle, noble metal platinum ruthenium catalyst utilance height, characteristics such as with low cost.It is the new method of efficient, the low-cost DMFC methanol oxidation electrode of preparation.
The object of the present invention is achieved like this: a kind of direct methanol fuel cell methanol oxidation electrode preparation method, its principal character is that isopropyl alcohol, carbon carrier powder, Teflon emulsion and Nafion solution is mixed and made into carbon ink mark mixture, again it is brushed equably or be printed on impregnated carbon cloth of Teflon or the carbon paper, make the non-metal catalyst carbon electrode through heat treated; Then, in the aqueous solution of platiniferous (Pt) and ruthenium (Ru) ion, with the method for electrochemical deposition, with the PtRu alloy deposition with carbon carrier that the proton exchange membrane component contact on, the DMFC methanol oxidation electrode of formation metal supported catalyst PtRu.
The method step of DMFC methanol oxidation electrode preparation is as follows:
The first step: the preparation of base electrode
Place the Teflon emulsion to soak 10-30 minute carbon cloth or carbon paper, taking-up is dried, and under 300-350 ℃ temperature, sintering 1-20 minute, just makes base electrode again.
Second step: preparation carbon ink mark mixture
With carbon carrier powder and concentration is that 10-60% Teflon emulsion, concentration are that 0.1-5% Nafion solution is 100 in proportion: 0-50: 1-100 joins in the aqueous isopropanol; the amount of isopropyl alcohol is convenient to follow-up spreading with made carbon ink mark mixture and is advisable; carried out ultrasonic oscillation 5-60 minute, and formed carbon ink mark mixture.
The 3rd step: preparation non-metal catalyst carbon electrode
The carbon ink mark mixture for preparing is brushed equably or is printed on the carbon electrode for preparing, under 150-300 ℃ temperature, heat 2-30 minute after, naturally cool to room temperature, just make the non-metal catalyst carbon electrode.
The 4th step: preparation platinum ruthenium catalyst carbon electrode
With the non-metal catalyst carbon electrode for preparing, place the aqueous solution electrochemical dislodger that contains Pt and Ru ion, with inactive, conductive material (as platinized platinum or graphite etc.) is auxiliary electrode, at room temperature, carry out electrochemical deposition with pulse current (as square wave current etc.), Pt, Ru are deposited on the non-metal catalyst carbon electrode, form load platinum ruthenium catalyst carbon electrode.Clean platinum ruthenium catalyst carbon electrode repeatedly with deionized water again, then, at 0.01-5mol/l sulfuric acid (H
2SO
4) or perchloric acid (HClO
4) in the solution, in the 1.90V potential range, last at relative standard's hydrogen electrode-0.05 with electrochemical method (as linear potential scanning or step potential) activated electrode repeatedly, from sulfuric acid solution, take out electrode, clean repeatedly with deionized water again, dry.Just make platinum ruthenium catalyst carbon electrode.
In electrochemical deposition process, the deposition of platinum ruthenium (claiming load capacity again) can pass through to regulate platinum ruthenium ion concentration, pulse current size in the platinum ruthenium ion aqueous solution, and electrodeposition time is controlled.
In the process of preparation platinum ruthenium catalyst carbon electrode, on the matrix carbon electrode, brush equably or print in the mixture of forming by carbon carrier powder, Teflon emulsion, Nafion solution and isopropyl alcohol, to the carbon carrier powder of the carbon granule inside of Nafion polymer parcel, owing to can not contact with the aqueous solution of platiniferous ruthenium ion.Thereby, not with the direct contacted carbon carrier of Nafion on, the electrochemical deposition of platinum ruthenium ion will do not had, this has just guaranteed that all PtRu that are deposited always are deposited on the direct contacted carbon carrier with Nafion, thereby make the PtRu that is deposited be effective catalyst, the utilance height of noble metal catalyst PtRu, and then reduced the cost of electrode.
Nafion film 112 or 115 or 117 is placed with between the methanol oxidation platinum ruthenium carbon electrode of method for preparing and the traditional hydrogen reduction platinum carbon electrode, under 200-250 ℃ of temperature, after hot pressing 1-10 minute, take out and be cooled to room temperature, just make " electrode/membrane " assembly of DMFC.
After the present invention adopts technique scheme, the utilization ratio height of noble metal catalyst PtRu, prepared platinum ruthenium catalyst carbon electrode cost is low.Adopt the platinum ruthenium catalyst carbon electrode of the present invention's preparation to can be applicable to direct methanol fuel cell.Direct methanol fuel cell with the present invention makes is widely used in electric automobile, various spacecrafts, and portable electric appts, as video camera, notebook computer, electronic toy etc.
Four description of drawings
Fig. 1 is at 0.5mol/l H
2SO
4With 0.5mol/l CH
3In the OH solution, under the room temperature, electrode potential is constant in 0.6 volt of relative standard's hydrogen electrode current potential, and the load capacity of catalyst platinum ruthenium is 0.20mg/cm
2The time, methanol oxidation current density-time graph on the different electrodes.
Curve 1 is in the electrochemical deposition solution, and platinum/ruthenium mol ratio is 1: 0 o'clock, the methanol oxidation current density-time graph of the methanol oxidation electrode of preparation.
Curve 2 is in the electrochemical deposition solution, and platinum/ruthenium mol ratio is 1: 0.1 o'clock, the methanol oxidation current density-time graph of the methanol oxidation electrode of preparation.
Curve 3 is in the electrochemical deposition solution, and platinum/ruthenium mol ratio is 1: 0.4 o'clock, the methanol oxidation current density-time graph of the methanol oxidation electrode of preparation.
Curve 4 is in the electrochemical deposition solution, and platinum/ruthenium mol ratio is 1: 1 o'clock, the methanol oxidation current density-time graph of the methanol oxidation electrode of preparation.
Curve 5 is the methanol oxidation current density-time graph according to the methanol oxidation electrode of platinum ruthenium catalyst (its platinum/ruthenium mol ratio is 1: the 1) preparation of CN1318873 A patent preparation.
Five embodiments
Below in conjunction with embodiment, further specify the present invention.
Embodiment 1
The first step: the preparation of base electrode
Place 60% Teflon emulsion to soak 10 minutes carbon cloth or carbon paper, taking-up is dried, and under 300 ℃ temperature, sintering 10 minutes just makes base electrode again.
Second step: preparation carbon ink mark mixture
With carbon carrier powder (Vulcan XC-72) and concentration is that 60% Teflon emulsion, concentration are that 0.1%Nafion solution joined in the aqueous isopropanol by weight 100: 1: 30; the amount of isopropyl alcohol is convenient to follow-up spreading with carbon ink mark mixture and is advisable; through ultrasonic oscillation 30 minutes, form carbon ink mark mixture.
The 3rd step: preparation non-metal catalyst carbon electrode
The carbon ink mark mixture for preparing is brushed equably on the carbon electrode for preparing, made the carbon carrier powder of electrode surface reach 0.8mg/cm
2, under 140 ℃ temperature, heat 5 minutes after, naturally cool to room temperature, just make the non-metal catalyst carbon electrode.
The 4th step: preparation platinum ruthenium catalyst carbon electrode
Non-metal catalyst carbon electrode with preparing places 1mol/l HCl, 1 * 10
-3Mol/lH
2PtCl
62H
2O and 0.1 * 10
-3Mol/l RuCl
3Solution is auxiliary electrode with the platinized platinum, with 14mA/cm
2Positive current and 140mA/cm
2The positive negative impulse current of negative current be applied between non-metal catalyst carbon electrode and the platinized platinum auxiliary electrode, positive current makes chloride ion-containing (Cl
-) Pt, Ru complex anion be enriched in the bonding carbon carrier surface of Nafion, negative current makes Pt in the complex anion that is enriched in the bonding carbon carrier surface of Nafion, Ru reduce deposition at carbon surface.According to number of times and the each time that keeps of reversal of determining that in the load capacity of electrode surface Pt, Ru reversal replaces.The number of times that the present embodiment reversal replaces is 20 times, and each 30 seconds time that keeps of reversal, the load capacity of PtRu is 0.20mg/cm
2Then, clean platinum ruthenium catalyst carbon electrode repeatedly, again at 0.1mol/l H with deionized water
2SO
4In the solution, in the 1.50V potential range, scan activated electrode repeatedly with linear potential at relative standard's hydrogen electrode-0.05, in the present embodiment, with the speed of 50mV/s, scan round 10 times.At last, from sulfuric acid solution, take out electrode, clean repeatedly with deionized water again.Just make platinum ruthenium catalyst carbon electrode.
The platinum ruthenium catalyst carbon electrode of above-mentioned preparation is placed 0.5mol/l H
2SO
4With 0.5mol/l CH
3In the OH solution, under the room temperature, be auxiliary electrode with the Pt sheet, electrode potential is constant when 0.6 volt of current potential of relative standard's hydrogen electrode, curve 2 among the methyl alcohol oxidation current density-time graph that records such as Fig. 1.
Embodiment 2
Respectively with 1mol/l HCl, 1 * 10
-3Mol/l H
2PtCl
62H
2O; 1mol/l HCl, 1 * 10
-3Mol/l H
2PtCl
62H
2O, 0.4 * 10
-3Mol/l RuCl
3With 1mol/l HCl, 1 * 10
-3Mol/lH
2PtCl
62H
2O, 1 * 10
-3Mol/l RuCl
3Replace electrochemical deposition solution (the 1mol/l HCl, 1 * 10 among the embodiment 1
-3Mol/l H
2PtCl
62H
2O and 0.1 * 10
-3Mol/l RuCl
3), each step of repetition embodiment 1 makes the load capacity of metallic catalyst on platinum or the platinum ruthenium catalyst carbon electrode be 0.20mg/cm
2Prepared platinum or platinum ruthenium catalyst carbon electrode are at 0.5mol/l H
2SO
4And 0.5mol/lCH
3In the OH solution, under the room temperature, be auxiliary electrode with the Pt sheet, electrode potential is constant when 0.6 volt of current potential of relative standard's hydrogen electrode, and the methyl alcohol oxidation current density-time graph that records is respectively as curve among Fig. 11, curve 3 and curve 4.
Contrast test
The first step: the preparation of base electrode
Place 60% ptfe emulsion (Teflon) to soak 10 minutes carbon cloth or carbon paper, taking-up is dried, and under 300 ℃ temperature, sintering 10 minutes just makes base electrode again.
Second step: preparation platinum ruthenium carbon ink mark mixture
Will be according to platinum ruthenium C catalyst (20% PtRu/C of CN1267922 A patent preparation; Pt: Ru is 1: 1) and concentration be that to be 0.1% Nafion solution joined in the aqueous isopropanol by weight 100: 1: 30 for 60% Teflon emulsion, concentration; the amount of isopropyl alcohol is convenient to follow-up spreading with made carbon ink mark mixture and is advisable; ultrasonic oscillation 30 minutes forms platinum ruthenium carbon ink mark mixture.
The 3rd step: preparation platinum ruthenium catalyst carbon electrode
The platinum ruthenium carbon ink mark mixture for preparing is brushed equably on the base electrode for preparing, made the load capacity of base electrode surface platinum ruthenium reach 0.2mg/cm
2, correspondingly, the area load amount of catalyst carrier carbon dust is 0.8mg/cm
2, under 140 ℃ temperature, heat 5 minutes after, naturally cool to room temperature, just make platinum ruthenium catalyst carbon electrode.
The platinum ruthenium catalyst carbon electrode of above-mentioned preparation is placed 0.5mol/l H
2SO
4With 0.5mol/l CH
3In the OH solution, under the room temperature, be auxiliary electrode with the Pt sheet, electrode potential is constant when 0.6 volt of current potential of relative standard's hydrogen electrode, curve 5 among the methyl alcohol oxidation current density-time graph that records such as Fig. 1.
As shown in Figure 1,, be increased to 1: 0.4 again, continue to be increased to 1: 1, constantly increase with the electric current of the methanol oxidation electrode catalyst oxidation methyl alcohol of the present invention preparation along with platinum ruthenium ion mol ratio in the electrochemical deposition solution was increased to 1: 0.1 from 1: 0.By the methyl alcohol oxidation current density-time graph of the embodiment of the invention and contrast test as can be known: under the room temperature, under 0.6 volt of current potential of relative standard's hydrogen electrode, the identical load amount and the methanol oxidation electrode of identical platinum ruthenium mol ratio, the present invention is than in advance the platinum ruthenium being deposited on the carbon carrier powder, methyl alcohol anodic oxidation catalysis platinum ruthenium electrode with the bonding method preparation of Nafion has bigger output current, the methanol oxidation current density (mA/cm that they are constantly different then
2) contrast as follows:
| Time (second) | 500 | ?1000 | ?1500 | ?2000 | ?2500 |
| The present invention's (curve 4) | 8.9 | ?7.8 | ?7.0 | ?6.4 | ?5.9 |
| CN1267922A patent (curve 5) | 4.0 | ?3.2 | ?2.9 | ?2.7 | ?2.5 |
Claims (4)
1, a kind of direct methanol fuel cell methanol oxidation electrode preparation method:
The first step: the preparation of base electrode
Place ptfe emulsion to soak 10-30 minute carbon cloth or carbon paper, taking-up is dried, again under 300-350 ℃ temperature, and sintering 1-20 minute;
It is characterized in that:
Second step: preparation carbon ink mark mixture
Mixture with carbon carrier powder, ptfe emulsion, Nafion solution and aqueous isopropanol carries out ultrasonic oscillation;
The 3rd step: preparation non-metal catalyst carbon electrode
The carbon ink mark mixture for preparing is brushed equably or is printed on the carbon electrode for preparing, after the heating, naturally cool to room temperature;
The 4th step: preparation platinum ruthenium catalyst carbon electrode
With the non-metal catalyst carbon electrode for preparing, placing the aqueous solution electrochemical dislodger of platiniferous, ruthenium ion, is auxiliary electrode with the inactive, conductive material, carries out electrochemical deposition, platinum-ruthenium alloys is deposited on the non-metal catalyst carbon electrode, clean platinum ruthenium catalyst carbon electrode repeatedly with deionized water again, then, in sulfuric acid or perchloric acid solution, with electrochemical method activated electrode repeatedly, at last, from sulfuric acid solution, take out electrode, clean repeatedly with deionized water again.
2, according to the described direct methanol fuel cell methanol oxidation of claim 1 electrode preparation method, it is characterized in that when preparation carbon ink mark mixture, carbon carrier powder and ptfe emulsion, the mixed proportion of Nafion solution are 100: 0-50: 1-100 joins in the aqueous isopropanol; The ultrasonic oscillation time is 5-60 minute; Heating-up temperature when preparation non-metal catalyst carbon electrode is 100-300 ℃, and be 2-30 minute heating time; When preparation platinum ruthenium catalyst carbon electrode, the operating current of electrochemical deposition is a pulse current; The potential range that electrode is activated repeatedly with electrochemical method is that relative standard's hydrogen electrode-0.05 is to 1.90 volts; The medium that electrode is activated repeatedly is sulfuric acid or perchloric acid, and its concentration range is 0.01-5mol/l.
3, according to claim 1,2 described direct methanol fuel cell methanol oxidation electrode preparation methods, it is characterized in that when preparation platinum ruthenium catalyst carbon electrode, by platinum, ruthenium ion concentration, the pulse current size in the adjusting platinum and the ruthenium ion aqueous solution, and the deposition of the length of electrochemical deposition time control platinum ruthenium.
4,, it is characterized in that the concentration range of used ptfe emulsion is 10-60% when preparation carbon ink mark mixture according to claim 1,2 described direct methanol fuel cell methanol oxidation electrode preparation methods; The concentration range of Nafion solution is 0.1-5%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031178235A CN1221050C (en) | 2003-04-29 | 2003-04-29 | Method for preparing methanol oxidation electrode in direct methanol fuel cell |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031178235A CN1221050C (en) | 2003-04-29 | 2003-04-29 | Method for preparing methanol oxidation electrode in direct methanol fuel cell |
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| Publication Number | Publication Date |
|---|---|
| CN1447468A true CN1447468A (en) | 2003-10-08 |
| CN1221050C CN1221050C (en) | 2005-09-28 |
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100384001C (en) * | 2006-04-28 | 2008-04-23 | 华南理工大学 | Direct spraying method for preparing fuel cell membrane electrode |
| CN100427945C (en) * | 2005-12-14 | 2008-10-22 | 中国科学院大连化学物理研究所 | Alcohol concentration sensor for alcohol fuel battery system |
| CN101808735B (en) * | 2007-07-25 | 2014-07-23 | 约翰逊马西燃料电池有限公司 | Catalyst |
| CN116103693A (en) * | 2022-11-25 | 2023-05-12 | 东莞理工学院 | Hydrogen evolution electrode, preparation method thereof and application thereof in hydrogen production by water electrolysis |
-
2003
- 2003-04-29 CN CNB031178235A patent/CN1221050C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100427945C (en) * | 2005-12-14 | 2008-10-22 | 中国科学院大连化学物理研究所 | Alcohol concentration sensor for alcohol fuel battery system |
| CN100384001C (en) * | 2006-04-28 | 2008-04-23 | 华南理工大学 | Direct spraying method for preparing fuel cell membrane electrode |
| CN101808735B (en) * | 2007-07-25 | 2014-07-23 | 约翰逊马西燃料电池有限公司 | Catalyst |
| CN116103693A (en) * | 2022-11-25 | 2023-05-12 | 东莞理工学院 | Hydrogen evolution electrode, preparation method thereof and application thereof in hydrogen production by water electrolysis |
| CN116103693B (en) * | 2022-11-25 | 2023-09-12 | 东莞理工学院 | Hydrogen evolution electrode, preparation method thereof and application thereof in hydrogen production by water electrolysis |
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| Publication number | Publication date |
|---|---|
| CN1221050C (en) | 2005-09-28 |
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