CN103816907B - The preparation method of the non-precious metal catalyst of nanometer doped zinc oxide - Google Patents
The preparation method of the non-precious metal catalyst of nanometer doped zinc oxide Download PDFInfo
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- CN103816907B CN103816907B CN201410081773.7A CN201410081773A CN103816907B CN 103816907 B CN103816907 B CN 103816907B CN 201410081773 A CN201410081773 A CN 201410081773A CN 103816907 B CN103816907 B CN 103816907B
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- 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
Abstract
The invention provides a kind of preparation method of non-precious metal catalyst of nanometer doped zinc oxide, after sucrose, lysine and nano zine oxide are fully mixed, in nitrogen protection, the condition of 800～1000 DEG C is carbonization treatment 1～3h next time, is then placed in the HCl solution that contains iron chloride and soaks 1～3h; Washing, dry after in zirconia ball grinding jar ball milling 1～3h, finally by gained powder in nitrogen protection, secondary carbonization treatment 1～3h and get final product under the condition of 800～1000 DEG C. Hydrogen reduction catalytic activity and the commercial catalysts Pt/C of the expensive metal catalyst of the non-gold of hydrogen reduction prepared by the present invention are quite approaching, and its cost is only 3% of commercial catalysts Pt/C, therefore, as the electrode catalyst of fuel cell, there is cost low, performance high, is of great significance for the tool of applying of fuel cell.
Description
Technical field
The invention belongs to new material technology field, relate to a kind of preparation of non-precious metal catalyst of nanometer doped zinc oxideMethod, is mainly used in the hydrogen reduction catalytic reaction of fuel cell.
Background technology
Fuel cell is a kind ofly will to be present in chemical energy in fuel and oxidant and to be converted into the TRT of electric energy.Fuel cell has the advantages such as generating efficiency is high, low in the pollution of the environment, and becomes a kind of more satisfactory generation technology. But restrictionThe key factor of fuel cell development and application is for Cathodic oxygen reduction catalyst. At present, urge as cathodic oxygen reductionThe raw material of agent is mainly noble metal platinum. But due to the platinum rare and expensive price of content on earth, make its one-tenthFor the biggest obstacle of fuel cell large-scale commercial production. Therefore, decades recently, people are being devoted to explore exploitation newlyOxygen reduction catalyst, can there is excellent activity and stability, go substitute business platinum C catalyst. In research, find, assorted formerNon-precious metal catalyst and the non-metallic catalyst of son doping, have good hydrogen reduction activity, anti methanol toxication ability and steadyQualitative. And nitrogen atom doping becomes people's research the most a kind of. Wu Gang seminar is used nitrogen atom doping to prepareThe oxygen reduction catalyst that performance can be takeed on platinum carbon ratio. This nitrogen-doping that contains lone pair electrons is oxygen reduction catalystResearch provides very important direction. But it is to be solved that this direction still has many problems to have, primary problem, is exactlyHow strengthening its catalytic activity by the specific area that increases catalyst, this also becomes people and will study from now on hydrogen reduction catalysisA significant challenge of agent.
Summary of the invention
The object of this invention is to provide a kind of preparation of non-precious metal catalyst of nanometer doped zinc oxide.
The preparation of the non-precious metal catalyst of nanometer doped zinc oxide of the present invention is by sucrose, lysine and nano oxidizedAfter zinc fully mixes, in nitrogen protection, the condition of 800～1000 DEG C is carbonization treatment 1～3h next time, is then placed into and containsIn the HCl solution of iron chloride, soak 1～2h; Washing, dry after in zirconia ball grinding jar ball milling 4～6h; Gained powder existsNitrogen protection, under the condition of 800～1000 DEG C, secondary carbonization treatment 1～3h, obtains non-precious metal catalyst.
The mol ratio of described sucrose, lysine, nano zine oxide is 1:0.5:0.5～1:1:2.
The concentration of described HCl solution is 1～3mol/L, the content of HCl Chlorine in Solution iron be 5% of sucrose quality～10%。
The structure of the non-precious metal catalyst of the nanometer doped zinc oxide of below being prepared by the present invention and hydrogen reduction performance are enteredRow analytic explanation.
1, Raman map analysis
Fig. 1 is the Raman comparison diagram of the base metal cathod catalyst prepared of the present invention. As seen from Figure 1, the present inventionThe non-precious metal catalyst of preparation is respectively at 1300cm-1And 1600cm-1There is characteristic peak D peak and the G peak of material with carbon element, saidBright this material exists with graphitization state. And compared with business XC-72 carbon dust, peak position is not offset, and shows to mixAfter assorted nano zine oxide, material with carbon element does not structurally change, the graphite structure of material with carbon element before still keeping. ButDue to the I of this catalystD/IGBe worth greatlyr than business carbon dust, so its carbon-coating blemish increases, there is better hydrogen reduction and liveProperty, this may be because there is the reason of nitrogen atom doping.
2, nitrogen adsorption desorption is analyzed
Fig. 2 is the nitrogen adsorption desorption figure of the non-metallic catalyst prepared of the present invention. Can visually see from Fig. 2, thisThe specific area of the non-metallic catalyst of bright preparation is at 703～705m2/ g(business XC-72 carbon dust specific area only has 237m2/G), business XC-72 carbon dust has larger specific area relatively. Because electrochemistry itself is exactly a surface reaction, haveBigger serface just illustrates that catalyst surface may have more avtive spot, and this oxygen that has just greatly improved catalyst alsoFormer activity.
3, hydrogen reduction performance test
Fig. 3 is nonmetal cathod catalyst and business XC-72 carbon dust prepared by the present invention, and business Pt/C is under alkali conditionHydrogen reduction linear sweep voltammetry curve map. From Fig. 3, can intuitively find out, compared with business XC-72 carbon dust, prepared by the present inventionOn nonmetal cathod catalyst electrode, hydrogen reduction take-off potential is compared respectively and has been shuffled than business carbon dust XC-72 with half wave potential234mV and 55mV, illustrate that this material shows better hydrogen reduction than conventional commercial XC-72 carbon dust under alkali conditionEnergy. Compared with business Pt/C catalyst, its polarization curves of oxygen reduction starting point position is identical with business Pt/C catalyst, half wave potentialOnly poor 75mV.
Hydrogen reduction catalytic activity and the commercial catalysts of the expensive metal catalyst of the non-gold of hydrogen reduction that in sum, prepared by the present inventionPt/C is quite approaching, and its cost is only 3% of commercial catalysts Pt/C, therefore, and as the electrode catalyst of fuel cell,Have cost low, performance high, is of great significance for the tool of applying of fuel cell.
Brief description of the drawings
Fig. 1 is the Raman comparison diagram of the expensive metal catalyst of non-gold prepared of the present invention.
Fig. 2 is the nitrogen adsorption desorption figure of the expensive metal catalyst of non-gold prepared of the present invention.
Fig. 3 is the expensive metal catalyst of non-gold and business XC-72 carbon dust prepared by the present invention, and business Pt/C is under alkali conditionHydrogen reduction linear sweep voltammetry curve map.
Detailed description of the invention
The preparation of the base metal cathod catalyst below by specific embodiment to nanometer doped zinc oxide of the present invention andIts performance is described further.
Embodiment 1
Take sucrose 1000mg, 1B 213.5mg, nano zine oxide 118.9mg, fully mixes and is placed on magneticIn boat, then magnetic boat is placed in tube furnace to nitrogen protection, graphitization processing 2h at 1000 DEG C; Be placed on and contain iron chlorideIn HCl solution, soak 2h(wherein the concentration of HCl solution be 1molL-1, the content of HCl Chlorine in Solution iron is 50mg. ), useWater washing, 60 DEG C of dry 6h in convection oven; Then ball milling 4h in zirconia ball grinding jar; Finally gained powder is placed inIn magnetic boat, and magnetic boat is placed in tube furnace, in nitrogen protection, under the condition of 800 DEG C, secondary carbonization 2h, obtains base metal and urgesAgent.
Test by nitrogen adsorption desorption, its specific area has reached 670m2/ g. Hydrogen reduction performance test is found, in alkalescenceUnder condition, hydrogen reduction take-off potential compares than business carbon dust XC-72 shuffled respectively 220mV and 46mV with half wave potential, saysBright this material shows better hydrogen reduction performance than conventional commercial XC-72 carbon dust under alkali condition. With business Pt/C catalysisAgent is compared, and its polarization curves of oxygen reduction starting point position is identical with business Pt/C catalyst, and half wave potential is poor 90mV only.
Embodiment 2
The temperature of a carbonization treatment is 900 DEG C, and other is identical with embodiment 1.
Test by nitrogen adsorption desorption, its specific area has reached 690m2/ g. Hydrogen reduction performance test is found, in alkalescenceUnder condition, hydrogen reduction take-off potential compares than business carbon dust XC-72 shuffled respectively 230mV and 50mV with half wave potential; WithBusiness Pt/C catalyst is compared, and its polarization curves of oxygen reduction starting point position is identical with business Pt/C catalyst, and half wave potential is only poor85mV。
Embodiment 3
The temperature of a carbonization treatment is 800 DEG C, and other is identical with embodiment 1.
Test by nitrogen adsorption desorption, its specific area has reached 703.9m2/ g. Hydrogen reduction performance test is found, at alkaliUnder property condition, hydrogen reduction take-off potential compares than business carbon dust XC-72 shuffled respectively 234mV and 55mV with half wave potential.Compared with business Pt/C catalyst, its polarization curves of oxygen reduction starting point position is identical with business Pt/C catalyst, and half wave potential onlyPoor 75mV.
Embodiment 4
Take sucrose 1000mg, 1B 213.5mg, nano zine oxide 239.8mg, after fully mixing in tubular typeIn stove, nitrogen protection, graphitization processing 2h at 800 DEG C; Be placed in the HCl solution that contains iron chloride and soak 1h(whereinThe concentration of HCl solution is 1molL-1, the content of HCl Chlorine in Solution iron is 100mg), wash with water, in convection oven 60DEG C dry 6h; Then ball milling 4h in zirconia ball grinding jar; Finally gained powder is placed in to magnetic boat, then magnetic boat is placed onIn tube furnace, in nitrogen protection, under the condition of 1000 DEG C, secondary carbonization 2h, obtains non-precious metal catalyst.
Test by nitrogen adsorption desorption, the specific area of non-precious metal catalyst has reached 685m2/ g. Hydrogen reduction performanceTest discovery, under alkali condition, hydrogen reduction take-off potential is compared respectively and has been shuffled than business carbon dust XC-72 with half wave potential232mV and 53mV; Compared with business Pt/C catalyst, its polarization curves of oxygen reduction starting point position and business Pt/C catalyst phaseWith, half wave potential is poor 80mV only.
Embodiment 5
The temperature of secondary carbonization treatment is 900 DEG C, and other is identical with embodiment 4.
Test by nitrogen adsorption desorption, the specific area of non-metallic catalyst has reached 690m2/ g. Hydrogen reduction performance is surveyedExamination discovery, under alkali condition, hydrogen reduction take-off potential is compared and has been shuffled respectively 220 than business carbon dust XC-72 with half wave potentialMV and 47mV; Polarization curves of oxygen reduction starting point position is identical with business Pt/C catalyst, and half wave potential is poor 79mV only.
Embodiment 6
The temperature of a carbonization treatment is 800 DEG C, and other is identical with embodiment 4.
Test by nitrogen adsorption desorption, the specific area of non-metallic catalyst has reached 705m2/ g. Hydrogen reduction performance is surveyedExamination discovery, under alkali condition, hydrogen reduction take-off potential is compared and has been shuffled respectively 226 than business carbon dust XC-72 with half wave potentialMV and 52mV; Compared with business Pt/C catalyst, its polarization curves of oxygen reduction starting point position is identical with business Pt/C catalyst,Half wave potential is poor 74mV only.
Embodiment 7
Take sucrose 1000mg, 1B 213.5mg, nano zine oxide 118.9mg, fully mixes and is placed on magneticIn boat, then magnetic boat is placed in tube furnace to nitrogen protection, graphitization processing 2h at 800 DEG C; Be placed on and contain iron chlorideIn HCl solution, soak 1h(wherein the concentration of HCl solution be 1molL-1, the content of HCl solution chlorination iron is 100mg. ), useWater washing, 60 DEG C of dry 6h in convection oven; Then ball milling 6h in zirconia ball grinding jar, is finally placed in gained powderIn magnetic boat, then magnetic boat is placed in tube furnace, in nitrogen protection, under the condition of 800 DEG C, secondary carbonization 2h, obtains base metalCatalyst.
Test by nitrogen adsorption desorption, its specific area has reached 700m2/ g. Hydrogen reduction performance test is found, in alkalescenceUnder condition, hydrogen reduction take-off potential compares than business carbon dust XC-72 shuffled respectively 222mV and 48mV with half wave potential, saysBright this material shows better hydrogen reduction performance than conventional commercial XC-72 carbon dust under alkali condition. With business Pt/C catalysisAgent is compared, and its polarization curves of oxygen reduction starting point position is identical with business Pt/C catalyst, and half wave potential is poor 76mV only.
Embodiment 8
In the HCl solution that contains iron chloride, soak time is 2h, and other is identical with embodiment 7.
Test by nitrogen adsorption desorption, the specific area of non-metallic catalyst has reached 704m2/ g. Hydrogen reduction performance is surveyedExamination discovery, under alkali condition, hydrogen reduction take-off potential is compared and has been shuffled respectively 228 than business carbon dust XC-72 with half wave potentialMV and 57mV; Compared with business Pt/C catalyst, its polarization curves of oxygen reduction starting point position is identical with business Pt/C catalyst,Half wave potential is poor 73mV only.
Embodiment 9
Take sucrose 1000mg, 1B 213.5mg, nano zine oxide 118.9mg, fully mixes and is placed on magneticIn boat, then magnetic boat is placed in tube furnace to nitrogen protection, graphitization processing 1h at 800 DEG C; Be placed on and contain iron chlorideIn HCl solution, soak 2h(wherein the concentration of HCl solution be 1molL-1, the content of HCl solution chlorination iron is 100mg. ), useWater washing, 60 DEG C of dry 6h in convection oven; Then ball milling 4h in zirconia ball grinding jar, is finally placed in gained powderIn magnetic boat, then magnetic boat is placed in tube furnace, in nitrogen protection, under the condition of 800 DEG C, secondary carbonization 2h, obtains base metalCatalyst.
Test by nitrogen adsorption desorption, its specific area has reached 699m2/ g. Hydrogen reduction performance test is found, in alkalescenceUnder condition, hydrogen reduction take-off potential compares than business carbon dust XC-72 shuffled respectively 227mV and 58mV with half wave potential, saysBright this material shows better hydrogen reduction performance than conventional commercial XC-72 carbon dust under alkali condition. With business Pt/C catalysisAgent is compared, and its polarization curves of oxygen reduction starting point position is identical with business Pt/C catalyst, and half wave potential is poor 80mV only.
Embodiment 10
A carbonization time is 2h, and other is identical with embodiment 9.
Test by nitrogen adsorption desorption, its specific area has reached 703m2/ g. Hydrogen reduction performance test is found, in alkalescenceUnder condition, hydrogen reduction take-off potential compares than business carbon dust XC-72 shuffled respectively 230mV and 62mV with half wave potential, saysBright this material shows better hydrogen reduction performance than conventional commercial XC-72 carbon dust under alkali condition. With business Pt/C catalysisAgent is compared, and its polarization curves of oxygen reduction starting point position is identical with business Pt/C catalyst, and half wave potential is poor 69mV only.
Embodiment 11
A carbonization time is 3h, and other is identical with embodiment 9.
Test by nitrogen adsorption desorption, its specific area has reached 700m2/ g. Hydrogen reduction performance test is found, in alkalescenceUnder condition, hydrogen reduction take-off potential compares than business carbon dust XC-72 shuffled respectively 224mV and 55mV with half wave potential, saysBright this material shows better hydrogen reduction performance than conventional commercial XC-72 carbon dust under alkali condition. With business Pt/C catalysisAgent is compared, and its polarization curves of oxygen reduction starting point position is identical with business Pt/C catalyst, and half wave potential is poor 73mV only.
Claims (3)
1. a preparation method for the non-precious metal catalyst of nanometer doped zinc oxide is by sucrose, lysine and nano oxidizedAfter zinc fully mixes, in nitrogen protection, the condition of 800～1000 DEG C is carbonization treatment 1～3h next time, is then placed into and containsIn the HCl solution of iron chloride, soak 1～2h; Washing, dry after in zirconia ball grinding jar ball milling 4～6h; Gained powder existsNitrogen protection, under the condition of 800～1000 DEG C, secondary carbonization treatment 1～3h, obtains non-precious metal catalyst; Described sucrose, bad ammoniaThe mol ratio of acid, nano zine oxide is 1:0.5:0.5～1:1:2.
2. the preparation method of the non-precious metal catalyst of nanometer doped zinc oxide as claimed in claim 1, is characterized in that: described inThe concentration of HCl solution is 1～3mol/L.
3. the preparation method of the non-precious metal catalyst of nanometer doped zinc oxide as claimed in claim 1, is characterized in that: described inThe content of iron chloride is 5%～10% of sucrose quality.
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Patent Citations (8)
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