CN110665497A - Graphene nanoribbon supported palladium monatomic catalyst and preparation method thereof - Google Patents
Graphene nanoribbon supported palladium monatomic catalyst and preparation method thereof Download PDFInfo
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- CN110665497A CN110665497A CN201910888760.3A CN201910888760A CN110665497A CN 110665497 A CN110665497 A CN 110665497A CN 201910888760 A CN201910888760 A CN 201910888760A CN 110665497 A CN110665497 A CN 110665497A
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- palladium
- graphene nanoribbon
- preparation
- supported
- monoatomic
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- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims abstract description 162
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 81
- 229910052763 palladium Inorganic materials 0.000 title claims abstract description 77
- 239000002074 nanoribbon Substances 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title claims abstract description 41
- 239000003054 catalyst Substances 0.000 title claims abstract description 36
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 20
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000001257 hydrogen Substances 0.000 claims abstract description 16
- 230000003197 catalytic effect Effects 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 230000001590 oxidative effect Effects 0.000 claims description 10
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000000137 annealing Methods 0.000 claims description 8
- 239000002048 multi walled nanotube Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 6
- 239000012696 Pd precursors Substances 0.000 claims description 6
- ZFOZVQLOBQUTQQ-UHFFFAOYSA-N Tributyl citrate Chemical compound CCCCOC(=O)CC(O)(C(=O)OCCCC)CC(=O)OCCCC ZFOZVQLOBQUTQQ-UHFFFAOYSA-N 0.000 claims description 6
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000003381 stabilizer Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 5
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 5
- -1 acrylic ester Chemical class 0.000 claims description 5
- 229910002094 inorganic tetrachloropalladate Inorganic materials 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 239000007800 oxidant agent Substances 0.000 claims description 5
- 239000012286 potassium permanganate Substances 0.000 claims description 5
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 4
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- 239000001110 calcium chloride Substances 0.000 claims description 3
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 3
- 235000011148 calcium chloride Nutrition 0.000 claims description 3
- 229960001484 edetic acid Drugs 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 3
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 3
- 229910052754 neon Inorganic materials 0.000 claims description 3
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 3
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 3
- YJVFFLUZDVXJQI-UHFFFAOYSA-L palladium(ii) acetate Chemical compound [Pd+2].CC([O-])=O.CC([O-])=O YJVFFLUZDVXJQI-UHFFFAOYSA-L 0.000 claims description 3
- INIOZDBICVTGEO-UHFFFAOYSA-L palladium(ii) bromide Chemical compound Br[Pd]Br INIOZDBICVTGEO-UHFFFAOYSA-L 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 claims description 3
- UKSZBOKPHAQOMP-SVLSSHOZSA-N (1e,4e)-1,5-diphenylpenta-1,4-dien-3-one;palladium Chemical compound [Pd].C=1C=CC=CC=1\C=C\C(=O)\C=C\C1=CC=CC=C1.C=1C=CC=CC=1\C=C\C(=O)\C=C\C1=CC=CC=C1 UKSZBOKPHAQOMP-SVLSSHOZSA-N 0.000 claims description 2
- WJFKNYWRSNBZNX-UHFFFAOYSA-N 10H-phenothiazine Chemical compound C1=CC=C2NC3=CC=CC=C3SC2=C1 WJFKNYWRSNBZNX-UHFFFAOYSA-N 0.000 claims description 2
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 claims description 2
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 2
- RBYGDVHOECIAFC-UHFFFAOYSA-L acetonitrile;palladium(2+);dichloride Chemical compound [Cl-].[Cl-].[Pd+2].CC#N.CC#N RBYGDVHOECIAFC-UHFFFAOYSA-L 0.000 claims description 2
- 235000010354 butylated hydroxytoluene Nutrition 0.000 claims description 2
- 235000010216 calcium carbonate Nutrition 0.000 claims description 2
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 2
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 2
- 239000001095 magnesium carbonate Substances 0.000 claims description 2
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 2
- 235000014380 magnesium carbonate Nutrition 0.000 claims description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 2
- 235000011147 magnesium chloride Nutrition 0.000 claims description 2
- NWVVVBRKAWDGAB-UHFFFAOYSA-N p-methoxyphenol Chemical compound COC1=CC=C(O)C=C1 NWVVVBRKAWDGAB-UHFFFAOYSA-N 0.000 claims description 2
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 claims description 2
- 229950000688 phenothiazine Drugs 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 229940068984 polyvinyl alcohol Drugs 0.000 claims description 2
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 2
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 2
- 235000011151 potassium sulphates Nutrition 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- BWYYYTVSBPRQCN-UHFFFAOYSA-M sodium;ethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=C BWYYYTVSBPRQCN-UHFFFAOYSA-M 0.000 claims description 2
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 claims description 2
- CYPYTURSJDMMMP-WVCUSYJESA-N (1e,4e)-1,5-diphenylpenta-1,4-dien-3-one;palladium Chemical compound [Pd].[Pd].C=1C=CC=CC=1\C=C\C(=O)\C=C\C1=CC=CC=C1.C=1C=CC=CC=1\C=C\C(=O)\C=C\C1=CC=CC=C1.C=1C=CC=CC=1\C=C\C(=O)\C=C\C1=CC=CC=C1 CYPYTURSJDMMMP-WVCUSYJESA-N 0.000 claims 1
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims 1
- NNXNKLLWTKSODZ-UHFFFAOYSA-N [acetyloxy-[2-(diacetyloxyamino)ethyl]amino] acetate;iron;sodium Chemical compound [Na].[Fe].CC(=O)ON(OC(C)=O)CCN(OC(C)=O)OC(C)=O NNXNKLLWTKSODZ-UHFFFAOYSA-N 0.000 claims 1
- WXNOJTUTEXAZLD-UHFFFAOYSA-L benzonitrile;dichloropalladium Chemical compound Cl[Pd]Cl.N#CC1=CC=CC=C1.N#CC1=CC=CC=C1 WXNOJTUTEXAZLD-UHFFFAOYSA-L 0.000 claims 1
- 150000002500 ions Chemical class 0.000 claims 1
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Substances C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 claims 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 229910052760 oxygen Inorganic materials 0.000 description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 9
- 239000001301 oxygen Substances 0.000 description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 9
- 229910052799 carbon Inorganic materials 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 238000004108 freeze drying Methods 0.000 description 4
- 239000002127 nanobelt Substances 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000010411 electrocatalyst Substances 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 238000004502 linear sweep voltammetry Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000004832 voltammetry Methods 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- XJECNSWAHCMYNZ-UHFFFAOYSA-N C=C.[Fe].[Na] Chemical group C=C.[Fe].[Na] XJECNSWAHCMYNZ-UHFFFAOYSA-N 0.000 description 1
- 229920000557 Nafion® Polymers 0.000 description 1
- 239000007983 Tris buffer Substances 0.000 description 1
- JFDZBHWFFUWGJE-UHFFFAOYSA-N benzonitrile Chemical compound N#CC1=CC=CC=C1 JFDZBHWFFUWGJE-UHFFFAOYSA-N 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 229940071106 ethylenediaminetetraacetate Drugs 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- JKDRQYIYVJVOPF-FDGPNNRMSA-L palladium(ii) acetylacetonate Chemical compound [Pd+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O JKDRQYIYVJVOPF-FDGPNNRMSA-L 0.000 description 1
- UQPUONNXJVWHRM-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 UQPUONNXJVWHRM-UHFFFAOYSA-N 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 229940083542 sodium Drugs 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- SRFKWQSWMOPVQK-UHFFFAOYSA-K sodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxymethyl)amino]acetate;iron(2+) Chemical compound [Na+].[Fe+2].OC(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O SRFKWQSWMOPVQK-UHFFFAOYSA-K 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
Images
Classifications
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/44—Palladium
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/12—Oxidising
-
- 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
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- 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
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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
- 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
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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
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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
- 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
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- Condensed Matter Physics & Semiconductors (AREA)
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Abstract
The invention relates to a graphene nanoribbon supported palladium monatomic catalyst and a preparation method thereof, which comprises the steps of preparing a graphene nanoribbon and preparing palladium monatomic, thus obtaining the graphene nanoribbon supported palladium monatomic catalyst and the preparation method thereof. Compared with the prior art, the preparation method takes the graphene nanoribbon as the ribbon-shaped carrier, the palladium monoatomic morphology features are uniform and regular, and the preparation method has good catalytic performance and stability in the field of hydrogen production, is simple in preparation process, is suitable for industrial production, and has high economic value.
Description
Technical Field
The invention belongs to the technical field of hydrogen production, and particularly relates to a graphene nanoribbon supported palladium monatomic catalyst and a preparation method thereof.
Background
With the continuous development of the current times, the hydrogen production by electrolyzing water becomes a suitable substitute for resource energy crisis power generation due to the advantages of high energy density, no pollution of products and the like. The hydrogen production reaction by water electrolysis occurs on the surface of the electrode, and comprises two basic half reactions of cathode hydrogen evolution reaction and anode oxygen evolution reaction. For the hydrogen production reaction by water electrolysis, how to effectively improve the catalytic activity of the catalytic material, reduce the opening overpotential and the tafel slope of the hydrogen evolution reaction, and improve the catalytic performance and the cycle stability of the electrode material is a hotspot and a key point of research in the field of electrocatalysis. Generally speaking, the catalyst is mainly based on platinum, and has excellent electrocatalytic hydrogen evolution activity due to the special surface electronic state and good d electronic center position of the catalyst, but the development process of the hydrogen evolution catalytic material is severely limited because platinum is expensive, low in reserves and easy to be poisoned by reaction intermediate CO. Therefore, the price of palladium is low and the poisoning resistance to CO is strong. Compared with the traditional carrier active carbon, the carbon spheres, the carbon nano tubes and the graphene, the graphene nanoribbons obtained by longitudinally cutting the carbon nano tubes are about 10nm wide, have energy gap bands with field effect and good catalytic performance, and therefore have huge application prospects on catalyst carriers.
In recent years, palladium is designed as a monatomic catalyst, and has good adsorption and desorption energy of hydrogen due to the monatomic size effect of the palladium, so that the catalyst is expected to have good electrocatalytic hydrogen evolution performance. So far, the application of non-noble metal-based monatomic catalyst in the field of hydrogen evolution by electrocatalysis hydrolysis still has more problems, one is that the load of the monatomic-based catalyst is usually too small because no metal bond is generated in the whole system; secondly, the transition metal chalcogenide is a semiconductor and has a slow electron transfer rate, so that the adoption of a substrate with good conductivity to load the catalyst is crucial to the electrocatalyst; and thirdly, the cycling stability of the prepared electrode is a problem, and the stability of the prepared electrocatalyst supported electrode is poor. In summary, how to design and prepare a high-loading monatomic electrolytic water hydrogen evolution catalytic material with high catalytic activity and good stability is a problem to be solved at present.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of graphene nanoribbon supported palladium monoatomic atoms, which has good catalytic performance and simple preparation process.
The purpose of the invention can be realized by the following technical scheme:
the preparation method of the graphene nanoribbon supported palladium monoatomic layer comprises the following steps:
(1) preparation of graphene nanoribbons
Adding a multi-walled carbon nanotube into potassium permanganate and concentrated sulfuric acid, oxidizing under a temperature condition, and centrifuging and cleaning for multiple times to obtain a graphene nanoribbon;
(2) preparation of graphene nanoribbon supported palladium monoatomic atom
Dissolving the graphene nanoribbon, the stabilizer and the palladium precursor in deionized water, continuously stirring at 10-200 ℃, centrifugally collecting and grinding the solution, and mixing and stirring the solution and solid powder to fully mix the solution. Then annealing at the gas protection temperature; and after the system is naturally cooled to room temperature, washing the system with absolute ethyl alcohol for multiple times, and drying the system in vacuum to obtain the graphene nanoribbon loaded palladium monoatomic atom.
The strong oxidant in the step (1) is two or more of ammonium persulfate, sodium peroxide, potassium dichromate, potassium permanganate and concentrated sulfuric acid.
The temperature in step (1) is 40 ℃ to 500 ℃.
The mass ratio of the strong oxidant to the multi-walled carbon nano-tube in the step (1) is 0.1-10000%.
The stabilizer in the step (2) is sodium vinyl sulfonate, water-based vinyl acetate, 2, 6-di-tert-butyl-4-methylphenol, acrylate, ethylene diamine tetraacetic acid, tributyl citrate, disodium ethylene diamine tetraacetate, p-hydroxyanisole, tetrasodium ethylene diamine tetraacetate, polyvinyl alcohol, phenothiazine, sodium iron ethylene diamine tetraacetate and hydroquinone.
The palladium precursor in the step (2) is palladium nitrate, palladium chloride, potassium chloropalladite, palladium iodide, palladium dibromide, dichlorodiamondral palladium, palladium sulfate, sodium tetrachloropalladate, bis (dibenzylideneacetone) palladium, sodium chloropalladite, palladium acetate, ammonium chloropalladate, ammonium tetrachloropalladate, tris (dibenzylidecetone) dipalladium, dichlorotetraamminepalladium, bis (acetonitrile) palladium chloride, palladium triphenylphosphine acetate, bis (cyanobenzene) palladium dichloride, palladium tetranitrile tetrafluoroborate, bis (acetylacetonato) palladium.
The mass ratio of the palladium precursor to the stabilizer in the step (2) is 0.1-1000%.
The annealing temperature at the temperature in the step (2) is 50 ℃ to 2000 ℃.
The solid powder in the step (2) is calcium carbonate, sodium bicarbonate, magnesium carbonate, potassium sulfate, magnesium sulfate, calcium chloride and magnesium chloride.
And (3) the protective gas in the step (2) is one or more of nitrogen, argon, helium and neon.
The content of the metal palladium loaded by the palladium-loaded single atom on the prepared graphene nanoribbon is 0.001-99.99wt%, and the graphene nanoribbon has good catalytic performance and stability in the field of hydrogen production.
Compared with the prior art, the graphene nanoribbon is used as the ribbon-shaped carrier, the morphology features are uniform and regular, the palladium monoatomic morphology features are uniform and regular, and the graphene nanoribbon has good catalytic performance and stability in the field of hydrogen production, is simple in preparation process, is suitable for industrial scale, and has high economic value.
Drawings
Fig. 1 is a projection electron microscope (TEM) image of example 1 (a) a TEM image of graphene nanoribbons (b) a TEM image of a graphene nanoribbon supported palladium monatomic catalyst;
fig. 2 is an X-ray diffractometer (XRD) pattern of the graphene nanoribbons and the graphene nanoribbon supported palladium monatomic catalyst obtained in example 1;
FIG. 3 is a graph of a linear sweep voltammetry curve of a catalyst in 0.1mol/L KOH solution at a rotation speed of 1600rpm/s and a sweep rate of 5mV/s under oxygen saturation, 1 graphene nanoribbon supporting palladium monoatomic, 2 Pd/C with a commercial palladium content of 20%, and 3 graphene nanoribbon supporting palladium nanoparticles;
FIG. 4 is a linear sweep voltammetry curve of a catalyst in 0.5mol/L sulfuric acid solution at a rotation speed of 1600rpm/s and a sweep rate of 5mV/s under oxygen saturation, 1 graphene nanoribbon supporting palladium monoatomic, 2 commercial Pd/C with 20% palladium content, and 3 graphene nanoribbon supporting palladium nanoparticles.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
A graphene nanoribbon supported palladium single-atom catalyst and a preparation method thereof contain Pd, C, H and O elements.
The graphene nanoribbon supported palladium monatomic catalyst and the preparation method thereof specifically comprise the following steps:
(1) preparation of graphene nanoribbons
Adding 0.5-100g of potassium permanganate and 10-100ml of concentrated sulfuric acid into 1-10g of multi-walled carbon nano-tubes, oxidizing at the temperature of 40-500 ℃, centrifuging and cleaning for many times, and freeze-drying to obtain the graphene nano-belt.
(2) Preparation of graphene nanoribbon supported palladium monoatomic atom
Dissolving 10-100mg of graphene nanoribbons, 1-100mg of ethylenediamine tetraacetic acid and 1-100mg of potassium chloropalladite in deionized water, continuously stirring at 10-200 ℃, then centrifugally collecting and grinding the solution, and mixing and stirring with calcium carbonate to fully mix the solution. Then annealing at 50-2000 deg.C under nitrogen protection. And after the system is naturally cooled to room temperature, washing the system with absolute ethyl alcohol for multiple times, and drying the system in vacuum for 10 hours to obtain the graphene nanoribbon loaded palladium monoatomic atom.
The obtained graphene nanoribbon supported palladium monatomic catalyst and the preparation method thereof were observed by a projection electron microscope (TEM), as shown in fig. 1. From the graph (a), it can be seen that the Graphene Nanoribbons (GNRs) as the carrier are of a uniform ribbon-shaped structure, the width is 10 nanometers, and from the graph (b), it can be seen that the palladium monoatomic atoms on the surface of the graphene nanoribbon supported palladium monatomic catalyst and the preparation method thereof are uniformly distributed, and the isolated single palladium monatomics are uniformly distributed on the graphene nanoribbons.
The graphene nanoribbon supported palladium monatomic catalyst and the preparation method thereof obtained as described above were scanned by an X-ray diffractometer, and the result is shown in fig. 2, from which it can be seen that the lowermost graphene nanoribbon corresponds to the plane having C (002), and from fig. 2, it is seen that the plane corresponds to Pd (100) at 2 θ equal to 40.2 °, the plane corresponds to Pd (200) at 2 θ equal to 46.8 °, the plane corresponds to Pd (220) at 2 θ equal to 68.1 °, and the plane corresponds to Pd (311) at 2 θ equal to 82.1 °, thereby proving that the obtained metal Pd is also metal Pd.
The obtained graphene nanoribbon supported palladium single-atom catalyst and the preparation method thereof are used for testing the electrochemical performance in a three-electrode system. Adding 5mg of the prepared catalyst into 50 mu L of Nafion with the mass concentration of 5% and 950 mu L of absolute ethanol solution, and performing ultrasonic dispersion for 30min to obtain a solution; then, the catalyst was subjected to 0.1mol/L KOH electrolyte and 0.5mol/L H2SO4And (3) testing in electrolyte:
dripping 10 mu L of the solution on a rotating disc electrode, and airing at room temperature to obtain a film electrode; a three-electrode system with an SCE electrode as a reference electrode and a Pt sheet as a counter electrode is used for carrying out linear voltammetry test by using a rotating disk electrode in a KOH solution of 0.1mol/L subjected to oxygen denitrogenation, and the scanning speed is 5 mV/s. As can be seen from FIG. 3, the graphene nanoribbon supported palladium monatomic catalyst prepared in example 1 and the preparation method thereof have an oxygen reduction initiation potential of 7mV and a half-wave potential of-140 mV. Comparative example Pd/C with a commercial palladium content of 20% (fig. 3 line 2) compared to the graphene nanoribbon supported palladium nanoparticle catalyst (fig. 3 line 3), the oxygen reduction onset potential and half-wave potential were more positive.
Dripping 10 mu L of the solution on a rotating disc electrode, and airing at room temperature to obtain a film electrode; a three-electrode system with an SCE electrode as a reference electrode and a Pt sheet as a counter electrode, and removing nitrogen in 0.5mol/L H by oxygen2SO4And performing linear voltammetry test in the electrolyte by using a rotating disk electrode, wherein the scanning speed is 5 mV/s. As can be seen from FIG. 4, the catalyst prepared in example 1 had an oxygen reduction initiation potential of 5570mV and a half-wave potential of 328 mV. Comparative example Pt/C with a commercial platinum content of 20% (fig. 4 line 2) and the graphene nanoribbon supported palladium nanoparticle catalyst (fig. 4 line 3) were more positive for oxygen reduction onset potential and half-wave potential.
Example 2
A graphene nanoribbon supported palladium single-atom catalyst and a preparation method thereof contain Pd, C, H and O elements.
The graphene nanoribbon supported palladium monatomic catalyst and the preparation method thereof specifically comprise the following steps:
(1) preparation of graphene nanoribbons
Adding 1-50g of potassium dichromate and 10-50ml of ammonium persulfate into 1-6g of multi-walled carbon nano-tube, oxidizing at the temperature of 40-500 ℃, centrifuging and cleaning for many times, and freeze-drying to obtain the graphene nano-belt.
(2) Preparation of graphene nanoribbon supported palladium monoatomic atom
Dissolving 10-50mg of graphene nanoribbons, 1-120mg of sodium iron ethylenediaminetetraacetate and 1-300mg of palladium dibromide in deionized water, continuously stirring at 10-150 ℃, then centrifugally collecting and grinding the solution, and mixing and stirring with calcium chloride to fully mix the solution. Then annealing at 50-800 deg.C under neon protection. And after the system is naturally cooled to room temperature, washing the system with absolute ethyl alcohol for multiple times, and drying the system in vacuum for 10 hours to obtain the graphene nanoribbon loaded palladium monoatomic atom.
Example 3
A graphene nanoribbon supported palladium single-atom catalyst and a preparation method thereof contain Pd, C, H and O elements.
The graphene nanoribbon supported palladium monatomic catalyst and the preparation method thereof specifically comprise the following steps:
(1) preparation of graphene nanoribbons
Adding 0.5-100g of potassium permanganate and 10-50ml of sodium peroxide into 1-10g of multi-walled carbon nano-tubes, oxidizing at the temperature of 30-400 ℃, centrifuging and cleaning for many times, and freeze-drying to obtain the graphene nano-belt.
(2) Preparation of graphene nanoribbon supported palladium monoatomic atom
Dissolving 10-50mg of graphene nanoribbons, 1-300mg of tributyl citrate and 1-40mg of ammonium tetrachloropalladate in deionized water, continuously stirring at 10-300 ℃, then centrifugally collecting and grinding the solution, and mixing and stirring with sodium bicarbonate to fully mix the solution. Then annealing at 70-1700 ℃ under the protection of helium. And after the system is naturally cooled to room temperature, washing the system with absolute ethyl alcohol for multiple times, and drying the system in vacuum for 9 hours to obtain the graphene nanoribbon loaded palladium monoatomic atom.
Example 4
A graphene nanoribbon supported palladium single-atom catalyst and a preparation method thereof contain Pd, C, H and O elements.
The graphene nanoribbon supported palladium monatomic catalyst and the preparation method thereof specifically comprise the following steps:
(1) preparation of graphene nanoribbons
Adding 0.5-110g of potassium dichromate and 10-300ml of concentrated sulfuric acid into 1-6g of multi-walled carbon nano-tube, oxidizing at the temperature of 40-200 ℃, centrifuging and cleaning for many times, and freeze-drying to obtain the graphene nano-belt.
(2) Preparation of graphene nanoribbon supported palladium monoatomic atom
Dissolving 10-80mg of graphene nanoribbons, 1-550mg of potassium dichromate and 1-60mg of palladium dichlorodiammine in deionized water, continuously stirring at 10-180 ℃, then centrifugally collecting and grinding the solution, and mixing and stirring with magnesium sulfate to fully mix the solution. Then annealing at 50 deg.C to 2000 deg.C under the protection of argon. And after the system is naturally cooled to room temperature, washing the system with absolute ethyl alcohol for multiple times, and drying the system in vacuum for 10 hours to obtain the graphene nanoribbon loaded palladium monoatomic atom.
The foregoing is merely an example of the embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A graphene nanoribbon supported palladium monatomic catalyst and a preparation method thereof are disclosed, and the method comprises the following steps:
(1) preparation of graphene nanoribbons
Adding a multi-walled carbon nanotube into a strong oxidant, oxidizing under a temperature condition, and centrifugally cleaning for multiple times to obtain a graphene nanoribbon;
(2) preparation of graphene nanoribbon supported palladium monoatomic atom
Dissolving the graphene nanoribbon, the stabilizer and the palladium precursor in deionized water, continuously stirring at 10-200 ℃, centrifugally collecting and grinding the solution, mixing with the solid powder, stirring fully, and annealing at a protective temperature; and after the system is naturally cooled to room temperature, washing the system with absolute ethyl alcohol for multiple times, and drying the system in vacuum to obtain the graphene nanoribbon loaded palladium monoatomic atom.
2. The method for preparing graphene nanoribbon supported palladium monatomic according to claim 1, wherein the strong oxidizing agent in step (1) is a combination of two or more of ammonium persulfate, sodium peroxide, potassium dichromate, potassium permanganate, and concentrated sulfuric acid.
3. The method for preparing graphene nanoribbon-supported palladium monoatomic according to claim 1, wherein the temperature in the step (1) is 50 to 500 ℃.
4. The method for preparing graphene nanoribbons supporting palladium monoatomic atoms according to claim 1, wherein the mass ratio of the strong oxidant to the multi-walled carbon nanotubes in the step (1) is 0.1% to 10000%.
5. The method for preparing graphene nanoribbon supported palladium monoatomic ions according to claim 1, wherein the stabilizer in the step (2) is sodium vinyl sulfonate, aqueous vinyl acetate, 2, 6-di-tert-butyl-4-methylphenol, acrylic ester, ethylene diamine tetraacetic acid, tributyl citrate, disodium ethylene diamine tetraacetate, p-hydroxyanisole, tetrasodium ethylene diamine tetraacetate, polyvinyl alcohol, phenothiazine, sodium iron ethylenediamine tetraacetate, and hydroquinone.
6. The method according to claim 1, wherein the palladium precursor in step (2) is palladium nitrate, palladium chloride, potassium chloropalladite, palladium iodide, palladium dibromide, dichlorodiamondral, palladium sulfate, sodium tetrachloropalladate, bis (dibenzylideneacetone) palladium, sodium chloropalladite, palladium acetate, ammonium chloropalladite, ammonium tetrachloropalladate, tris (dibenzylideneacetone) dipalladium, dichlorotetraamminepalladium, bis (acetonitrile) palladium chloride, palladium acetate triphenylphosphine, bis (cyanophenyl) palladium dichloride, palladium tetrafluoroborate tetraacetonitrile, palladium bis (acetylacetonate).
7. The preparation method of the graphene nanoribbon supported palladium monatomic according to claim 1, wherein the mass ratio of the palladium precursor to the stabilizer in the step (2) is 0.1% -1000%; the annealing temperature is 50 ℃ to 2000 ℃.
8. The method for preparing graphene nanoribbon supported palladium monoatomic according to claim 1, wherein the solid powder in the step (2) is calcium carbonate, sodium bicarbonate, magnesium carbonate, potassium sulfate, magnesium sulfate, calcium chloride, or magnesium chloride.
9. The method for preparing graphene nanoribbon supported palladium monoatomic atoms according to claim 1, wherein the protective gas in the step (2) is one or more of nitrogen, argon, helium and neon.
10. The preparation method of the graphene nanoribbon supported palladium monatomic according to claim 1, characterized in that the content of the metal palladium supported by the graphene nanoribbon supported palladium monatomic obtained by the preparation is 0.0001-99.99wt% and has good catalytic performance and stability in the field of hydrogen production.
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