CN111957336A - Preparation method of ZIF-8-derived Fe-N-C oxygen reduction electrocatalyst - Google Patents
Preparation method of ZIF-8-derived Fe-N-C oxygen reduction electrocatalyst Download PDFInfo
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- CN111957336A CN111957336A CN202010783061.5A CN202010783061A CN111957336A CN 111957336 A CN111957336 A CN 111957336A CN 202010783061 A CN202010783061 A CN 202010783061A CN 111957336 A CN111957336 A CN 111957336A
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 21
- 239000001301 oxygen Substances 0.000 title claims abstract description 21
- 239000010411 electrocatalyst Substances 0.000 title claims abstract description 17
- 230000009467 reduction Effects 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000013154 zeolitic imidazolate framework-8 Substances 0.000 title claims abstract 6
- MFLKDEMTKSVIBK-UHFFFAOYSA-N zinc;2-methylimidazol-3-ide Chemical compound [Zn+2].CC1=NC=C[N-]1.CC1=NC=C[N-]1 MFLKDEMTKSVIBK-UHFFFAOYSA-N 0.000 title claims abstract 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000000243 solution Substances 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- 229940025294 hemin Drugs 0.000 claims abstract description 8
- BTIJJDXEELBZFS-QDUVMHSLSA-K hemin Chemical compound CC1=C(CCC(O)=O)C(C=C2C(CCC(O)=O)=C(C)\C(N2[Fe](Cl)N23)=C\4)=N\C1=C/C2=C(C)C(C=C)=C3\C=C/1C(C)=C(C=C)C/4=N\1 BTIJJDXEELBZFS-QDUVMHSLSA-K 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 7
- YSWBFLWKAIRHEI-UHFFFAOYSA-N 4,5-dimethyl-1h-imidazole Chemical compound CC=1N=CNC=1C YSWBFLWKAIRHEI-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 239000000446 fuel Substances 0.000 claims description 8
- 229910052573 porcelain Inorganic materials 0.000 claims description 7
- 239000008280 blood Substances 0.000 claims description 3
- 210000004369 blood Anatomy 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 abstract description 18
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- DSVGQVZAZSZEEX-UHFFFAOYSA-N [C].[Pt] Chemical compound [C].[Pt] DSVGQVZAZSZEEX-UHFFFAOYSA-N 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 230000010757 Reduction Activity Effects 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 34
- 238000006722 reduction reaction Methods 0.000 description 11
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 10
- 229910052799 carbon Inorganic materials 0.000 description 5
- 229910000510 noble metal Inorganic materials 0.000 description 5
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 239000003863 metallic catalyst Substances 0.000 description 4
- 208000021251 Methanol poisoning Diseases 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000011943 nanocatalyst Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000004611 spectroscopical analysis Methods 0.000 description 2
- 238000010183 spectrum analysis Methods 0.000 description 2
- 238000013112 stability test Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 description 1
- VSXQNMCMCVKLOI-UHFFFAOYSA-N CC1=NC=CN1.[Zn+2] Chemical compound CC1=NC=CN1.[Zn+2] VSXQNMCMCVKLOI-UHFFFAOYSA-N 0.000 description 1
- 208000005374 Poisoning Diseases 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/33—
-
- B01J35/60—
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9041—Metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
-
- 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
Abstract
The invention provides a preparation method of a ZIF-8 derived Fe-N-C oxygen reduction electrocatalyst, which is prepared by carrying out reaction on Zn (NO)3)2.6H2Adding O into methanol to obtain a mixed solution A; then adding dimethyl imidazole and hemin into methanol to obtain a mixed solution B; then rapidly adding the solution A into the solution B under vigorous stirring, and reacting at room temperature; drying the obtained product, heating at high temperature and preserving heat to obtain Fe x -N-C. The method has the advantages of low preparation cost, no pollution, high catalytic activity, excellent methanol resistance and high stability. Systematically researching the influence of the Fe doping amount on the oxygen reduction activity to obtain the optimal Fe55the-N-C catalyst has a half-slope potential of 0.892V vs RHE and a potential of 0.80V under basic conditionsThe current density was 17.5 mA cm‑2The catalytic performance is higher than commercial platinum carbon.
Description
Technical Field
The invention relates to a preparation method of a ZIF-8 derived Fe-N-C oxygen reduction electrocatalyst, belonging to the technical field of non-noble metal catalysts in electrocatalysis.
Background
The fuel cell is used as a novel energy conversion device, and the anode reaction of the fuel cell converts the chemical energy of the fuel into electric energy through an electrochemical catalytic process, so that the conversion of energy can be realized. In order to ensure the normal conversion of fuel cell energy and reduce the cost, the cathode process is often Oxygen Reduction Reaction (ORR). The oxygen content in air is relatively high (21%), so that air can be used directly as a source of oxygen for the cathode reaction. However, ORR is inefficient, limiting the efficient energy conversion of fuel cells. Commercial platinum carbon has high ORR activity under ideal conditions, but has the disadvantages of high price, poor stability and easy poisoning, so that the commercial platinum carbon is limited in practical application in many aspects.
In order to reduce the cost of the catalyst, on the premise of keeping high ORR catalytic activity, the method which is generally adopted at present is to reduce the use amount of Pt or replace Pt by other non-noble metals. In the research and development of fuel cells, the search for non-noble transition metal nanocatalysts to replace noble metal catalysts has become a hotspot of the research on ORR catalysts. Transition metal-nitrogen-carbon (M-N-C) electrocatalysts (M = Fe, Co, Ni, etc.) are considered to be the most promising commercial platinum-carbon candidate electrocatalysts due to high utilization of active sites, superior conductivity, coordination of metal sites with the matrix. Although there are many reports of the application of M-N-C nano-catalyst to oxygen reduction electrocatalysis, there are still many defects that the secondary microstructure is not well maintained by the catalyst (chem. Sci. 2013, 4, 2941-.
Disclosure of Invention
Aiming at the problems, the three-dimensional porous Fe-N-C oxygen reduction electrocatalyst with clear morphology is prepared by using blood crystal as a Fe source and using 2-methylimidazolium zinc salt MAF-4 (ZIF-8) as a precursor and a template, and the prepared catalyst has better methanol poisoning resistance and excellent stability and is expected to replace commercial platinum carbon.
The invention is realized by the following technical scheme:
a ZIF-8 derived Fe-N-C oxygen reduction electrocatalyst is prepared by subjecting Zn (NO)3)2.6H2Adding O into methanol to obtain a mixed solution A; then adding dimethyl imidazole and hemin into methanol to obtain a mixed solution B; then rapidly adding the solution A into the solution B under vigorous stirring, and reacting at room temperature; centrifuging and washing the obtained product for several times, and vacuum drying at 70 deg.C for one night to obtain Hemin product x @ZIF-8（x=20, 35, 55, 85); transferring the product to a porcelain boat, placing the porcelain boat in a tube furnace, heating and preserving heat to obtain a ZIF-8 derived Fe-N-C oxygen reduction electrocatalyst Fe x -N-C（x=20，35，55，85）。
Preferably, the mixed solution A is 1.07 g of Zn (NO)3)2.6H2O is added into 40 mL of methanol, and the mixed solution B is prepared by mixing 2.35 g of dimethyl imidazole andx mg（x=20, 35, 55, 85) hemin to 40 mL methanol.
Preferably, the solution A is added into the solution B and then reacts for 24 hours at room temperature; the heating and heat preservation conditions are as follows: heating to 900 ℃ at a heating rate of 5 ℃ per second in a nitrogen atmosphere and keeping the temperature for 3 h.
The invention also discloses a ZIF-8 derived Fe-N-C oxygen reduction electrocatalyst Fe prepared by the preparation method x -N-C（x=20, 35, 55, 85), preferably Fe55-N-C。
The invention also discloses a ZIF-8 derived Fe-N-C oxygen reduction electrocatalyst Fe x -N-C（x=20, 35, 55, 85) in fuel cells or metal-air cells.
Advantageous effects
The invention discloses a preparation method of a ZIF-8 derived Fe-N-C oxygen reduction electrocatalyst, which has the advantages of low preparation cost of raw materials, no pollution, high catalytic activity of products, excellent methanol resistance and high stability. Systematically researching the influence of the Fe doping amount on the oxygen reduction activity to obtain the optimal Fe55the-N-C catalyst has a half-slope potential of 0.892V vs RHE and a kinetic current density of 17.5 mA cm at 0.80V under alkaline conditions-2The catalytic performance is higher than commercial platinum carbon.
Drawings
FIG. 1 (A) Fe x -a schematic synthesis of an N-C catalyst; (B, F) each is Hemin55-N-C and Fe55-SEM images of N-C; (C, G) each is Hemin55-N-C and Fe55-TEM images of N-C; (D, E) Fe55-N-C high resolution TEM images; (H) fe55-N-C high angle annular dark field image-scanning transmission electron microscope image; (I) an element distribution image.
FIG. 2 (A) Fe55-XRD patterns of N-C and N-C; (B) fe55-XPS full spectrum analysis of N-C and N-C; (C) fe55-XPS spectroscopy of N1s in N-C catalyst; (D) fe55XPS spectrum analysis of Fe2p in the N-C catalyst.
FIG. 3 (A) various non-noble metal catalysts prepared in N2/O2CV curve in (1); (B) ORR polarization curves of various prepared non-metallic catalysts and commercial Pt/C in 0.1M KOH solution; (C) preparation of various non-metallic catalysts and commercial Pt/CE 1/2AndJ ka histogram.
FIG. 4 (A) Fe55Stability tests of N-C and commercial Pt/C; (B) fe55Anti-methanol poisoning experiments for N-C and commercial Pt/C.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
(1) Preparation and characterization of Fe-N-C electrocatalyst:
1.07 g of Zn (NO)3)2.6H2Adding O into 40 mL of methanol to obtain a mixed solution A; then 2.35 g of dimethylimidazole andxmg Xuezuosu (blood crystal)x=0, 20, 35, 55, 85) was added to 40 mL of methanol to obtain a mixed solution B; then rapidly adding the solution A into the solution B under vigorous stirring, and reacting for 24 hours at room temperature; finally, centrifugally washing the obtained product for several times, and carrying out vacuum drying at 70 ℃ for one night; according to the amount of added Hemin, we respectively mark the product as Hemin @ ZIF-8 and Hemin20@ZIF-8、Hemin35@ZIF-8、Hemin55@ ZIF-8 and Hemin85@ ZIF-8. Transferring the product to a porcelain boat, placing the porcelain boat in a tube furnace, heating the porcelain boat to 900 ℃ in a nitrogen atmosphere at a heating rate of 5 ℃ per second, and keeping the temperature for 3 h to obtain products respectively marked as N-C, Fe20-N-C、Fe35-N-C、Fe55-N-C and Fe85-N-C. From SEM and TEM images, Hemin55@ ZIF-8 is a rhombic dodecahedron with clear outline. After high temperature heat treatment, Hemin55@ ZIF-8 carbonization to Fe55N-C, the surface becomes rough, but the three-dimensional structure of the original ZIF-8 is substantially maintained and no iron particles are contained. Fe can be seen from the high-angle annular dark field image and the element distribution image55The elements of-N-C are uniformly distributed, and no obvious Fe-containing particles exist. XRD results also show Fe55-N-C is fully carbonized and free of iron-containing impurities. XPS technique for analyzing Fe55Chemical states of components N-C, it can be found by XPS spectrum analysis of N1s that N in the catalyst has three doping types, and the binding energies are 397.3 eV, 399.4 eV and 400.7 eV, which are respectively assigned to pyridine N, pyrrole N and graphite N. The XPS spectrum analysis of Fe2p shows that Fe element coexists in +2 and +3 valence states55-N-C catalyst.
In the drawings: FIG. 1 (A) Fe x -a schematic synthesis of an N-C catalyst; (B, F) each is Hemin55-N-C and Fe55-SEM images of N-C; (C, G) are eachHemin55-N-C and Fe55-TEM images of N-C; (D, E) Fe55-N-C high resolution TEM images; (H) fe55-N-C high angle annular dark field image-scanning transmission electron microscope image; (I) an element distribution image.
FIG. 2 (A) Fe55-XRD patterns of N-C and N-C; (B) fe55-XPS full spectrum analysis of N-C and N-C; (C) fe55-XPS spectroscopy of N1s in N-C catalyst; (D) fe55XPS spectrum analysis of Fe2p in the N-C catalyst.
(2) Electrochemical oxygen reduction test:
all electrochemical tests were performed in a conventional three-electrode system at room temperature at the CHI 660 electrochemical station. A Rotating Disk Electrode (RDE), a Saturated Calomel Electrode (SCE) and a graphite rod were used as a working electrode, a reference electrode and a counter electrode, respectively. Both Cyclic Voltammetry (CV) and Linear Sweep (LSV) tests are at saturation N2Or O2In 0.1M KOH electrolyte. The scanning rates of CV and LSV were 50 mV s, respectively-1And 10 mV s-1。
FIG. 3 (A) various non-noble metal catalysts prepared in N2/O2CV curve in (1); (B) ORR polarization curves of various prepared non-metallic catalysts and commercial Pt/C in 0.1M KOH solution; (C) preparation of various non-metallic catalysts and commercial Pt/CE 1/2AndJ ka histogram.
FIG. 4 (A) Fe55Stability tests of N-C and commercial Pt/C; (B) fe55Anti-methanol poisoning experiments for N-C and commercial Pt/C.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (6)
1. A preparation method of a ZIF-8 derived Fe-N-C oxygen reduction electrocatalyst is characterized in thatZn(NO3)2.6H2Adding O into methanol to obtain a mixed solution A; then adding dimethyl imidazole and hemin into methanol to obtain a mixed solution B; then rapidly adding the solution A into the solution B under vigorous stirring, and reacting at room temperature; centrifuging and washing the obtained product for several times, and vacuum drying at 70 deg.C for one night to obtain Hemin product x @ZIF-8（x=20, 35, 55, 85); transferring the product to a porcelain boat, placing the porcelain boat in a tube furnace, heating and preserving heat to obtain a ZIF-8 derived Fe-N-C oxygen reduction electrocatalyst Fe x -N-C（x=20，35，55，85）。
2. The method according to claim 1, wherein the mixed solution A is 1.07 g of Zn (NO)3)2.6H2O is added into 40 mL of methanol, and the mixed solution B is prepared by mixing 2.35 g of dimethyl imidazole andxmg Xuezuosu (blood crystal)x=20, 35, 55, 85) was added to 40 mL of methanol.
3. The preparation method according to claim 1, wherein the solution A is added to the solution B and then reacted for 24 hours at room temperature; the heating and heat preservation conditions are as follows: heating to 900 ℃ at a heating rate of 5 ℃ per second in a nitrogen atmosphere and keeping the temperature for 3 h.
4. The method of claim 1, wherein the product is Fe55-N-C。
5. A ZIF-8 derived Fe-N-C oxygen reduction electrocatalyst Fe prepared by the preparation method of any one of claims 1 to 3 x -N-C（x=20，35，55，85）。
6. The ZIF-8 derived Fe-N-C oxygen reduction electrocatalyst Fe of claim 5 x -N-C（x=20, 35, 55, 85) in fuel cells or metal-air cells.
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| CN114614032A (en) * | 2022-03-18 | 2022-06-10 | 江苏索普化工股份有限公司 | Anode composite nano catalyst material of methanol fuel cell and preparation method and application thereof |
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| CN114188558A (en) * | 2021-11-29 | 2022-03-15 | 西安理工大学 | Preparation method of Fe-NC catalyst modified by oxygen vacancies |
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