CN114411197B - Preparation method of noble metal doped hollow iron phosphide nano material - Google Patents
Preparation method of noble metal doped hollow iron phosphide nano material Download PDFInfo
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- CN114411197B CN114411197B CN202210094219.7A CN202210094219A CN114411197B CN 114411197 B CN114411197 B CN 114411197B CN 202210094219 A CN202210094219 A CN 202210094219A CN 114411197 B CN114411197 B CN 114411197B
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 23
- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 22
- VAKIVKMUBMZANL-UHFFFAOYSA-N iron phosphide Chemical compound P.[Fe].[Fe].[Fe] VAKIVKMUBMZANL-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 12
- 239000001257 hydrogen Substances 0.000 claims abstract description 12
- 239000002243 precursor Substances 0.000 claims abstract description 7
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims abstract description 3
- 239000008367 deionised water Substances 0.000 claims description 27
- 229910021641 deionized water Inorganic materials 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 18
- 239000000919 ceramic Substances 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 238000009210 therapy by ultrasound Methods 0.000 claims description 9
- 238000001291 vacuum drying Methods 0.000 claims description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 3
- 239000003792 electrolyte Substances 0.000 claims description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 239000012279 sodium borohydride Substances 0.000 claims description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 2
- 239000012692 Fe precursor Substances 0.000 description 14
- 229910021065 Pd—Fe Inorganic materials 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 101150003085 Pdcl gene Proteins 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- DPTATFGPDCLUTF-UHFFFAOYSA-N phosphanylidyneiron Chemical compound [Fe]#P DPTATFGPDCLUTF-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- 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
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention relates to a preparation method of a noble metal doped hollow iron phosphide nano material, which is characterized in that FeCl is adopted 3 ·6H 2 O, and noble metal M ξ+ (M ξ+ ＝Ru 3+ 、Pd 2+ 、Pt 4+ 、Ir 3+ ) As a precursor, through NaBH 4 Sodium hypophosphite NaH for rapid reduction 2 PO 2 ·H 2 O-phosphating and HCl washing to obtain the hollow noble metal doped iron phosphide nano material (H-M-FeP), the preparation method is simple, controllable and easy to implement, and the hollow iron phosphide nano material can be used for high-efficiency electrocatalytic hydrogen evolution reaction at room temperature.
Description
Technical Field
The invention relates to preparation of a noble metal doped hollow iron phosphide nano material, and belongs to the field of material preparation.
Background
The hollow nano material has larger specific surface area and more reactive sites, so that the hollow nano material attracts wide attention in the fields of medicine control release, biological sensing, energy storage, conversion and the like, particularly in the field of electrocatalytic hydrogen evolution, and researchers design and synthesize a large number of nano materials with different element compositions as hydrogen evolution electrocatalysts in order to obtain higher electrochemical hydrogen evolution performance. FeP is taken as Fe-based Transition Metal Phosphide (TMPs), has been paid attention to because of its abundant content in the crust, and has the advantages of good conductivity, mechanical strength, chemical corrosion resistance, etc., and has been intensively studied in terms of energy conversion and storage.
Research shows that the high concentration of P in TMPs weakens the delocalization capability of electrons in metal atoms, which results in serious reduction of the conductivity of TMPs, so that to optimize the catalytic hydrogen evolution activity of TMPs, the electronic characteristics of TMPs need to be regulated, and hetero-atom doping is the most effective electronic structure regulating method currently accepted, P can be stabilized by sharing electrons with atoms with high electronegativity, and finally the intrinsic activity of each active site is increased, particularly, noble metal doping into Fe-based frames can not only regulate the microscopic electronic structure of FeP to change the performance of FeP, but also obviously improve the conductivity of FeP nano materials and increase the number of reactive sites, thereby enhancing the electrocatalytic hydrogen evolution performance of the materials, and having important practical significance.
Disclosure of Invention
The invention aims to provide a preparation method of a noble metal doped hollow iron phosphide nano material (H-Ru-FeP) and application thereof in electrocatalytic hydrogen precipitation.
Based on the above objects, the technical scheme of the invention is as follows:
1) X mol FeCl 3 ·6H 2 O, y mol noble metal M ξ+ (M ξ+ ＝Ru 3+ 、Pd 2+ 、Pt 4+ 、Ir 3+ ) (x+y=0.1 mol, and 0.08.ltoreq.x.ltoreq.0.1 mol, 0.ltoreq.y.ltoreq.0.02 mol) in 50mL deionized water; then 0.189g NaBH 4 Adding the solution, stirring for 5min, vacuum filtering after the reaction is finished, washing with deionized water and absolute ethyl alcohol for three times in sequence, and vacuum drying at 60 ℃ for 6h to obtain a precursor of noble metal-Fe. Will be placed 500mg NaH 2 PO 2 ·H 2 Placing the ceramic boat of O at the front end of a tube furnace, placing the ceramic boat containing 50mg of dried precursor sample of noble metal-Fe at the rear end of the tube furnace, heating to 350 ℃ in the tube furnace at a heating rate of 2 ℃/min, and preserving heat for 2 hours to obtain the noble metal M doped FeP nano material (M-FeP). Finally, adding 2mL of HCl solution with the concentration of 1mol/L into 40mg of M-FeP sample, carrying out ultrasonic treatment for 30min, standing for 3-24H, centrifuging, and washing with deionized water and absolute ethyl alcohol for three times respectively to obtain the hollow noble metal M-doped ferric phosphide nano material (H-M-FeP).
2) Use of noble metal doped hollow iron phosphide nanomaterials for acidity (0.5M H) 2 SO 4 ) The hydrogen evolution reaction was electrocatalytic under neutral (1M PBS), alkaline (1M KOH) electrolyte. The current density is 10mA cm -2 The potentials at this time were 42mV, 91mV and 110mV, respectively.
The invention has the following advantages:
1) By FeCl 3 ·6H 2 O, noble metal M ξ+ (M ξ+ ＝Ru 3+ 、Pd 2+ 、Pt 4+ 、Ir 3+ ) As a precursor, sodium borohydride (NaBH) 4 ) Sodium hypophosphite (NaH) with rapid reduction 2 PO 2 ·H 2 O) phosphating and hydrochloric acid (HCl) washing to obtain H-M-FeP, the method is simple, controllable and easy to implement, and can be used for high-efficiency electrocatalytic hydrogen evolution reaction
Drawings
FIG. 1 is a characterization result of a noble metal doped hollow iron phosphide nanomaterial, (a-b) electron microscope pictures, (c) XPS pictures and (d) XRD pictures, and (e) electrochemical hydrogen evolution linear scanning curves.
Detailed Description
The present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the following examples.
Example 1
0.09mol FeCl 3 ·6H 2 O、0.01mol RuCl 3 ·3H 2 O, dissolving in 50mL deionized water; then 0.189g NaBH 4 And adding the solution, stirring for 5min, vacuum filtering after the reaction is finished, washing with deionized water and absolute ethyl alcohol for three times in sequence, and vacuum drying at 60 ℃ for 6h to obtain the Ru-Fe precursor. Will be placed 500mg NaH 2 PO 2 ·H 2 Placing the ceramic boat of O at the front end of a tube furnace, placing the ceramic boat containing 50mg of dried Ru-Fe precursor sample at the rear end of the tube furnace, heating to 350 ℃ in the tube furnace at a heating rate of 2 ℃/min, and preserving heat for 2h to obtain Ru-FeP. Finally, adding 2mL of HCl solution with the concentration of 1mol/L into 40mg of Ru-FeP sample, carrying out ultrasonic treatment for 30min, standing for 12H, centrifuging, and washing with deionized water and absolute ethyl alcohol for three times respectively to obtain H-Ru-FeP.
Example 2
0.09mol FeCl 3 ·6H 2 O、0.01mol RuCl 3 ·3H 2 O, dissolving in 50mL deionized water; then 0.189g NaBH 4 And adding the solution, stirring for 5min, vacuum filtering after the reaction is finished, washing with deionized water and absolute ethyl alcohol for three times in sequence, and vacuum drying at 60 ℃ for 6h to obtain the Ru-Fe precursor. Will be placed 500mg NaH 2 PO 2 ·H 2 The porcelain boat of O is arrangedAnd (3) placing a porcelain boat containing 50mg of dried Ru-Fe precursor sample at the front end of the tube furnace at the rear end of the tube furnace, heating to 350 ℃ in the tube furnace at a heating rate of 2 ℃/min, and preserving heat for 2 hours to obtain Ru-FeP. Finally, adding 2mL of HCl solution with the concentration of 1mol/L into 40mg of Ru-FeP sample, carrying out ultrasonic treatment for 30min, standing for 24H, centrifuging, and washing with deionized water and absolute ethyl alcohol for three times respectively to obtain H-Ru-FeP. .
Example 3
0.085mol FeCl 3 ·6H 2 O、0.015mol RuCl 3 ·3H 2 O, dissolving in 50mL deionized water; then 0.189g NaBH 4 And adding the solution, stirring for 5min, vacuum filtering after the reaction is finished, washing with deionized water and absolute ethyl alcohol for three times in sequence, and vacuum drying at 60 ℃ for 6h to obtain the Ru-Fe precursor. Will be placed 500mg NaH 2 PO 2 ·H 2 Placing the ceramic boat of O at the front end of a tube furnace, placing the ceramic boat containing 50mg of dried Ru-Fe precursor sample at the rear end of the tube furnace, heating to 350 ℃ in the tube furnace at a heating rate of 2 ℃/min, and preserving heat for 2h to obtain Ru-FeP. Finally, adding 2mL of HCl solution with the concentration of 1mol/L into 40mg of Ru-FeP sample, carrying out ultrasonic treatment for 30min, standing for 12H, centrifuging, and washing with deionized water and absolute ethyl alcohol for three times respectively to obtain H-Ru-FeP.
Example 4
0.085mol FeCl 3 ·6H 2 O、0.015mol RuCl 3 ·3H 2 O, dissolving in 50mL deionized water; then 0.189g NaBH 4 And adding the solution, stirring for 5min, vacuum filtering after the reaction is finished, washing with deionized water and absolute ethyl alcohol for three times in sequence, and vacuum drying at 60 ℃ for 6h to obtain the Ru-Fe precursor. Will be placed 500mg NaH 2 PO 2 ·H 2 Placing the ceramic boat of O at the front end of a tube furnace, placing the ceramic boat containing 50mg of dried Ru-Fe precursor sample at the rear end of the tube furnace, heating to 350 ℃ in the tube furnace at a heating rate of 2 ℃/min, and preserving heat for 2h to obtain Ru-FeP. Finally, adding 2mL of HCl solution with the concentration of 1mol/L into 40mg of Ru-FeP sample, carrying out ultrasonic treatment for 30min, standing for 18H, centrifuging, and washing with deionized water and absolute ethyl alcohol for three times respectively to obtain H-Ru-FeP.
Example 5
0.09mol FeCl 3 ·6H 2 O、0.01mol H 14 Cl 6 O 6 Pt dissolved in 50mL deionized water; then 0.189g NaBH 4 Adding the solution, stirring for 5min, vacuum filtering after the reaction is finished, washing with deionized water and absolute ethyl alcohol for three times in sequence, and vacuum drying at 60 ℃ for 6h to obtain the Pt-Fe precursor. Will be placed 500mg NaH 2 PO 2 ·H 2 Placing the ceramic boat of O at the front end of a tube furnace, placing the ceramic boat with 50mg of dried Pt-Fe precursor sample at the rear end of the tube furnace, then heating to 350 ℃ in the tube furnace at a heating rate of 2 ℃/min, and preserving heat for 2 hours to obtain Pt-FeP. Finally, adding 2mL of HCl solution with the concentration of 1mol/L into 40mg of Pt-FeP sample, carrying out ultrasonic treatment for 30min, standing for 12H, centrifuging, and washing with deionized water and absolute ethyl alcohol for three times respectively to obtain H-Pt-FeP.
Example 6
0.09mol FeCl 3 ·6H 2 O、0.01mol PdCl 2 Dissolving in 50mL deionized water; then 0.189g NaBH 4 Adding the solution, stirring for 5min, vacuum filtering after the reaction is finished, washing with deionized water and absolute ethyl alcohol for three times in sequence, and vacuum drying at 60 ℃ for 6h to obtain the Pd-Fe precursor. Will be placed 500mg NaH 2 PO 2 ·H 2 Placing the ceramic boat of O at the front end of a tube furnace, placing the ceramic boat with 50mg of dried Pd-Fe precursor sample at the rear end of the tube furnace, then heating to 350 ℃ in the tube furnace at a heating rate of 2 ℃/min, and preserving heat for 2 hours to obtain Pd-FeP. Finally, adding 2mL of 1mol/L HCl solution into 40mg of Pd-FeP sample, carrying out ultrasonic treatment for 30min, standing for 12H, centrifuging, and washing with deionized water and absolute ethyl alcohol for three times to obtain H-Pd-FeP
Example 7
0.09mol FeCl 3 ·6H 2 O、0.01mol IrCl 3 Dissolving in 50mL deionized water; then 0.189g NaBH 4 Adding the solution, stirring for 5min, vacuum filtering after the reaction is finished, washing with deionized water and absolute ethyl alcohol for three times in sequence, and vacuum drying at 60 ℃ for 6h to obtain the Ir-Fe precursor. Will be placed 500mg NaH 2 PO 2 ·H 2 Placing the ceramic boat of O at the front end of a tube furnace, placing the ceramic boat containing 50mg of dried Ir-Fe precursor sample at the rear end of the tube furnace, heating to 350 ℃ in the tube furnace at a heating rate of 2 ℃/min, and preserving heat for 2 hours to obtain Ir-FeP. Finally, adding 2mL of HCl solution with the concentration of 1mol/L into 40mg of Ir-FeP sample, carrying out ultrasonic treatment for 30min, standing for 12H, centrifuging, and washing with deionized water and absolute ethyl alcohol for three times respectively to obtain H-Ir-FeP.
Claims (2)
1. Preparation method of noble metal doped hollow iron phosphide nano material, wherein FeCl is adopted as nano material 3 ·6H 2 O and noble metal M ξ+ ＝Ru 3+ 、Pd 2+ 、Pt 4+ Or Ir 3+ As a precursor, sodium borohydride (NaBH) 4 ) Sodium hypophosphite (NaH) with rapid reduction 2 PO 2 ·H 2 O) phosphating and hydrochloric acid (HCl) washing to obtain hollow noble metal doped iron phosphide nano material (H-M-FeP), wherein the hollow iron phosphide nano material can be used for high-efficiency electrocatalytic hydrogen evolution reaction at room temperature; the preparation of the noble metal doped hollow iron phosphide nano material comprises the following steps:
(1) 0.08 to 0.1mol FeCl 3 ·6H 2 O and 0.01-0.02 mol of noble metal are dissolved in 50mL of deionized water, and stirred until dissolved; then 0.189g NaBH 4 Adding the solution, stirring for 5min, vacuum filtering after the reaction is finished, washing with deionized water and absolute ethyl alcohol for three times in sequence, and vacuum drying for 6h at 60 ℃ to obtain a precursor of noble metal-Fe;
(2) will be placed 500mg NaH 2 PO 2 ·H 2 Placing the ceramic boat of O at the front end of a tube furnace, placing the ceramic boat containing 50mg of dried precursor of noble metal-Fe at the rear end of the tube furnace, heating to 350deg.C in the tube furnace at a heating rate of 2deg.C for 2 min -1 Preserving heat for 2h to obtain a noble metal M doped FeP nano material (M-FeP);
(3) finally, adding 2mL of HCl solution with the concentration of 1mol/L into 40mg of M-FeP sample, carrying out ultrasonic treatment for 30min, standing for 3-24H, centrifuging, and washing with deionized water and absolute ethyl alcohol for three times respectively to obtain H-M-FeP.
2. The use of a noble metal doped hollow iron phosphide nanomaterial prepared according to the method of claim 1, characterized by:
use of noble metal doped hollow iron phosphide nanomaterial for acidity 0.5M H 2 SO 4 Electrocatalytic hydrogen evolution reaction with neutral 1M PBS and alkaline 1M KOH electrolyte, current density of 10mA cm -2 The potentials at this time were 42mV, 91mV and 110mV, respectively.
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| US9259724B2 (en) * | 2011-07-21 | 2016-02-16 | Nanjing University | Supported bimetallic nanocomposite catalyst and the preparation method thereof |
| CN109967099A (en) * | 2019-03-11 | 2019-07-05 | 浙江大学 | A kind of Co with hollow nanostructures2P@C composite and its preparation method and application |
| CN109989070A (en) * | 2019-05-07 | 2019-07-09 | 江西师范大学 | Three-dimensional classification FeP nanometer sheet Electrocatalytic Activity for Hydrogen Evolution Reaction material and its preparation method and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US9259724B2 (en) * | 2011-07-21 | 2016-02-16 | Nanjing University | Supported bimetallic nanocomposite catalyst and the preparation method thereof |
| CN109967099A (en) * | 2019-03-11 | 2019-07-05 | 浙江大学 | A kind of Co with hollow nanostructures2P@C composite and its preparation method and application |
| CN109989070A (en) * | 2019-05-07 | 2019-07-09 | 江西师范大学 | Three-dimensional classification FeP nanometer sheet Electrocatalytic Activity for Hydrogen Evolution Reaction material and its preparation method and application |
Non-Patent Citations (1)
| Title |
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| Zixuan Wang et.al..Microwave-assisted to decorate Ru onto Hollow-structured Fe-P spheres as efficient Electrocatalyst for hydrogen generation in wide pH range.《Applied Surface Science》.2023,157026. * |
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