CN108380870A - A kind of nucleocapsid AuRh star decahedrons are nanocrystalline and its preparation method and application - Google Patents
A kind of nucleocapsid AuRh star decahedrons are nanocrystalline and its preparation method and application Download PDFInfo
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- CN108380870A CN108380870A CN201810151976.7A CN201810151976A CN108380870A CN 108380870 A CN108380870 A CN 108380870A CN 201810151976 A CN201810151976 A CN 201810151976A CN 108380870 A CN108380870 A CN 108380870A
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- nanocrystalline
- aurh
- nucleocapsid
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- decahedrons
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- 238000002360 preparation method Methods 0.000 title claims abstract description 45
- 238000005406 washing Methods 0.000 claims abstract description 22
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims abstract description 21
- 229910052703 rhodium Inorganic materials 0.000 claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 10
- -1 trifluoracetic acid rhodium dimer Chemical class 0.000 claims description 45
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical group CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 44
- 239000010948 rhodium Substances 0.000 claims description 44
- 239000010931 gold Substances 0.000 claims description 38
- 239000002244 precipitate Substances 0.000 claims description 18
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 18
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 15
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims description 13
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical group [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 5
- 230000003197 catalytic effect Effects 0.000 claims description 5
- RWRDJVNMSZYMDV-UHFFFAOYSA-L radium chloride Chemical compound [Cl-].[Cl-].[Ra+2] RWRDJVNMSZYMDV-UHFFFAOYSA-L 0.000 claims description 4
- 229910001630 radium chloride Inorganic materials 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- BKEOXUSOEGMVTL-UHFFFAOYSA-N trimethyl-$l^{3}-bromane Chemical class CBr(C)C BKEOXUSOEGMVTL-UHFFFAOYSA-N 0.000 claims 1
- 239000006185 dispersion Substances 0.000 abstract description 19
- 239000004615 ingredient Substances 0.000 abstract description 3
- 238000012986 modification Methods 0.000 abstract 1
- 230000004048 modification Effects 0.000 abstract 1
- 239000002243 precursor Substances 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 32
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 25
- 238000013019 agitation Methods 0.000 description 24
- 150000001875 compounds Chemical class 0.000 description 21
- 238000006243 chemical reaction Methods 0.000 description 18
- 229910052737 gold Inorganic materials 0.000 description 18
- 239000002245 particle Substances 0.000 description 18
- 239000007788 liquid Substances 0.000 description 17
- 235000019441 ethanol Nutrition 0.000 description 16
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 12
- 239000001257 hydrogen Substances 0.000 description 12
- 229910052739 hydrogen Inorganic materials 0.000 description 12
- 238000003756 stirring Methods 0.000 description 12
- SJUCACGNNJFHLB-UHFFFAOYSA-N O=C1N[ClH](=O)NC2=C1NC(=O)N2 Chemical compound O=C1N[ClH](=O)NC2=C1NC(=O)N2 SJUCACGNNJFHLB-UHFFFAOYSA-N 0.000 description 10
- XJWSAJYUBXQQDR-UHFFFAOYSA-M dodecyltrimethylammonium bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)C XJWSAJYUBXQQDR-UHFFFAOYSA-M 0.000 description 10
- 230000005540 biological transmission Effects 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- 239000013049 sediment Substances 0.000 description 8
- 239000006228 supernatant Substances 0.000 description 8
- 239000007795 chemical reaction product Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 description 6
- 238000006471 dimerization reaction Methods 0.000 description 6
- 239000006193 liquid solution Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 238000005868 electrolysis reaction Methods 0.000 description 5
- SONJTKJMTWTJCT-UHFFFAOYSA-K rhodium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Rh+3] SONJTKJMTWTJCT-UHFFFAOYSA-K 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 230000033228 biological regulation Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000002159 nanocrystal Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 241000258957 Asteroidea Species 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 125000005211 alkyl trimethyl ammonium group Chemical group 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000010944 silver (metal) Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
-
- 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
- B01J23/48—Silver or gold
- B01J23/52—Gold
-
- B01J35/23—
-
- B01J35/393—
-
- B01J35/397—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0553—Complex form nanoparticles, e.g. prism, pyramid, octahedron
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- 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
-
- 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
-
- 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
- C25B11/097—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 comprising two or more noble metals or noble metal alloys
-
- 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
It is nanocrystalline that the present invention discloses a kind of nucleocapsid AuRh star decahedrons, and wherein metal Au is kernel, and metal Rh is shell.The invention also discloses the nanocrystalline preparation methods of above-mentioned nucleocapsid AuRh star decahedrons, including：Au presomas are dissolved in oleyl amine, the solution of acquisition is added to and is preheated in 110~180 DEG C of oleyl amine, are reacted 3~4 hours at 110~180 DEG C, are centrifuged, washing is scattered in oleyl amine and is used as seed solution again；After seed solution is uniformly mixed with modification agent solution and is preheated to 180~190 DEG C, Rh precursor solutions are added, are stirred to react 3~4 hours at 180~190 DEG C, centrifuge, it is nanocrystalline to obtain nucleocapsid AuRh star decahedrons for washing.The nanocrystalline appearance and size homogeneity of nucleocapsid AuRh star decahedrons produced by the present invention is good, and good dispersion, ingredient is adjustable, and is easy to preserve.
Description
Technical field
The present invention relates to field of nanometer material technology, and in particular to a kind of nucleocapsid AuRh star decahedrons are nanocrystalline and its make
Preparation Method and application.
Background technology
The burning of the fossil energies such as oil makes environmental problem getting worse, energy-saving and environmental protection become the theme of the world today,
The demand of exploitation clean energy resource is increasingly urgent to.In numerous energy technologys, Hydrogen Energy takes off as a kind of efficient, free of contamination energy
Grain husk and go out.The preparation method of hydrogen mainly has water electrolysis hydrogen production, water-gas hydrogen manufacturing, biomass hydrogen preparation, methanol decomposition hydrogen manufacturing etc..Electrolysis
Water hydrogen manufacturing is that under the action of catalyst, water decomposition generates hydrogen and oxygen, is the effective ways for continuing hydrogen making.Hydrogen economy
Realization, dependent on explore with high activity, high stability and low cost elctro-catalyst.
Noble metal nanocrystalline is primarily referred to as noble metal (such as Au, Ag, Rh, Pt, Pd) of the size between 1-100 nanometers
Grain, because it is concerned in the extensive use in the fields such as catalysis, optical sensing, biomedicine and microelectronics industry.Wherein Rh
It is nanocrystalline to be widely applied in terms of processing vehicle exhaust and electrocatalytic reaction as catalyst, as Oxidation of Carbon Monoxide is anti-
It answers, hydrogenation reaction, alkylation reaction etc..It is also applied in water electrolysis hydrogen production as catalyst in addition, Rh is nanocrystalline, however its
Catalytic activity and stability are still to be improved in catalysis is reacted, and therefore, improving Rh nanocrystalline catalytic activity and stability is
The key of high-efficient electrolytic water technological development.Domestic and international present Research is investigated it is found that having studied the shape for the Rh system nano-crystals delivered
Looks mainly have：Tetrahedron, starfish shape, hexahedron, tetrahexahedron (Angew.Chem.Int.Ed.2007,46,1152-1155；
Angew.Chem.Int.Ed.2010,49,5296-5300；Angew.Chem.Int.Ed.2012,51,10266-10270；
Angew.Chem.Int.Ed.2014,53,5097-5101)..
Invention content
Goal of the invention：The object of the present invention is to provide a kind of structure novels, and scale topography is uniform, and good dispersion, ingredient can
The nucleocapsid AuRh star decahedrons of control are nanocrystalline.
It is a further object of the present invention to provide the nanocrystalline preparation method of above-mentioned nucleocapsid AuRh star decahedrons and answer
With.
Technical solution：A kind of nucleocapsid AuRh star decahedrons of present invention offer are nanocrystalline, nucleocapsid AuRh stars
During shape decahedron is nanocrystalline, metal Au is kernel, and metal Rh is shell.
Performance is superior nanocrystalline in order to obtain, and the grain size for keeping above-mentioned nucleocapsid AuRh star decahedrons nanocrystalline is 10
The molar ratio of~12nm, Au element and Rh elements is 1: 1~1: 5.
Another aspect of the present invention provides a kind of preparation method that above-mentioned nucleocapsid AuRh star decahedrons are nanocrystalline, including
Following steps：
1) Au presomas are dissolved in oleyl amine, obtain the first solution；
2) the first solution that step 1) obtains is added to and is preheated in 110~180 DEG C of oleyl amine, it is anti-at 110~180 DEG C
It answers 3~4 hours, centrifuges, obtained black precipitate is scattered in oleyl amine by washing again, obtains seed solution；
3) the oleyl amine solution of dressing agent is added in the seed solution obtained to step 2), be uniformly mixed and it is preheated to 180~
After 190 DEG C (stirrings 8~10 minutes), the oleyl amine solution of Rh presomas is added, is stirred to react 3~4 hours at 180~190 DEG C, from
The heart, washing, it is nanocrystalline to obtain nucleocapsid AuRh star decahedrons.Above-mentioned dressing agent is cetyl trimethylammonium bromide, ten
The main function of six alkyl trimethyl ammonium chlorides or double dodecyl trimethyl ammonium bromide, dressing agent is that regulation and control gained is nanocrystalline
Appearance structure.
The present invention is that prepare nucleocapsid AuRh star decahedrons in oil phase nanocrystalline, therefore the selection of raw material is that oil is molten
Property, preferably, Au presomas are chlorauride or gold chloride in step 1)；In step 3) Rh presomas be acetylacetone,2,4-pentanedione rhodium,
Radium chloride or trifluoracetic acid rhodium dimer.
In step 1) and step 2), by the way that Au presomas are dissolved in a small amount of oleyl amine, be then added to and be preheated to 110~
In 180 DEG C of relatively great amount of oleyl amine, the nanocrystalline uniform particle diameter of final nucleocapsid AuRh star decahedrons obtained can be made.
Preferably, in step 1) Au presomas a concentration of 0.01~0.03mol/L；In step 2), the first solution and it is preheated to 110~
The volume ratio of 180 DEG C of oleyl amine is 3: 5~3: 9.
In step 3), the Au elements of addition and mole that the molar ratio of dressing agent is 1: 50~150, Au elements and Rh elements
Than being 1: 1~5.
It in above-mentioned preparation method, is found by comparative study, regulates and controls the concentration of Rh presomas to nanocrystalline appearance structure
Have a great impact, crossing the Rh presomas of low concentration causes the nanocrystalline of acquisition to be polyhedral structure, and before the Rh of excessive concentrations
Driving body can then cause the nanocrystalline of acquisition to be dendritic morphology.Preferably, step 3)
In the oleyl amine solution of middle Rh presomas, a concentration of 0.002~0.03mol/L of Rh presomas.
The main function of dressing agent is the nanocrystalline appearance structure of regulation and control gained in the present invention, according to Au used in solvent
The amount of presoma and Rh presomas determines the dosage of dressing agent.Preferably, in step 3), repaiied in the oleyl amine solution of dressing agent
Adorn a concentration of 0.12~0.54mol/L of agent；In the three kinds of dressing agents enumerated, hexadecyltrimethylammonium chloride for Au, Pt,
The transition-metal ions such as Rh have stronger coordination, have preferable stability to metal, are more advantageous to and obtain pattern ruler
It is very little uniform nanocrystalline, therefore preferably dressing agent is hexadecyltrimethylammonium chloride.
Another aspect of the present invention is to provide above-mentioned nanocrystalline the answering in catalytic field of nucleocapsid AuRh star decahedrons
With.
Advantageous effect：Compared with the prior art, the present invention has the advantage that：
1, the nanocrystalline appearance and size homogeneity of nucleocapsid AuRh star decahedrons produced by the present invention is good, good dispersion,
Ingredient is adjustable；Meanwhile of the invention nucleocapsid AuRh star decahedrons are nanocrystalline is easy to preserve, and are scattered in hexamethylene and preserve i.e.
It can.
2, existing Rh system nano-crystals of different shapes are compared to, nucleocapsid AuRh star decahedrons of the invention are received
Meter Jing has efficient electrolysis water performance.It is provided by the invention to prepare the nanocrystalline new method tool of nucleocapsid AuRh star decahedrons
There are critically important scientific research and economic implications.
Description of the drawings
Fig. 1 is Au particle transmission electron microscope pictures；
Fig. 2 is the nanocrystalline structural characterization figure of nucleocapsid AuRh star decahedrons, wherein figure A is nucleocapsid AuRh
The nanocrystalline transmission electron microscope picture of star decahedron, figure B is the nanocrystalline transmission energy spectrum diagram of nucleocapsid AuRh star decahedrons.
Fig. 3 is the nanocrystalline polarization curve of nucleocapsid AuRh star decahedrons.
Specific implementation mode
Below by specific embodiment, the invention will be further described, but protection scope of the present invention be not limited to it is following
Embodiment.
Embodiment 1
A kind of nucleocapsid AuRh star decahedrons are nanocrystalline, and preparation method is：
(1) under room temperature, gold chloride is dissolved in 3 milliliters of oleyl amines, magnetic agitation is uniform, and compound concentration is
The chlorauric acid solution of 0.01mol/L；
(2) 7 milliliters of oleyl amines are added in 25 milliliters of three-necked flasks, which is put into 180 degrees Celsius of oil bath pans
In, magnetic agitation preheats 10 minutes, and the chlorauric acid solution of step (1) preparation is rapidly injected with pipettor, and the reaction was continued 3 hours,
After reaction product through hexamethylene and ethyl alcohol centrifuge washing three times, it is molten that the black precipitate of acquisition is scattered in 10 milliliters of oleyl amines again
In liquid, gold particle seed solution is obtained；
(3) under room temperature, hexadecyltrimethylammonium chloride is dissolved in 5 milliliters of oleyl amines, magnetic agitation is uniform, matches
Make the hexadecyltrimethylammonium chloride solution of a concentration of 0.18mol/L；Acetylacetone,2,4-pentanedione rhodium is dissolved in 3 milliliters of oleyl amines, magnetic
Power stirs evenly, and compound concentration is the acetylacetone,2,4-pentanedione rhodium solution of 0.002mol/L；
(4) it from being taken out in gold particle seed solution made from step (2) in 2 milliliters of addition to three-necked flasks, is burnt at three mouthfuls
Hexadecyltrimethylammonium chloride solution made from step (3) is continuously added in bottle, is put into 180 degrees Celsius of oil bath pans, magnetic force
Stirring preheating 10 minutes, is rapidly injected acetylacetone,2,4-pentanedione rhodium solution made from step (3), the reaction was continued 3 hours using pipettor；
(5) product for obtaining step (4) through hexamethylene and ethyl alcohol centrifuge washing three times, remove supernatant, taking precipitate；
(6) the sediment ultrasonic disperse for obtaining step (5) in hexamethylene to get nucleocapsid AuRh star decahedrons
Nanocrystalline dispersion liquid.The dispersion liquid room temperature preserves.
Fig. 1 is the Au particle transmission electron microscope pictures synthesized by the present embodiment step (2), and wherein A figures are that enlargement ratio is
200000 transmission electron microscope picture, B figures are the transmission electron microscope pictures that enlargement ratio is 150000.In Fig. 2, A figures are the present embodiment synthesis
The nanocrystalline transmission electron microscope picture of nucleocapsid AuRh star decahedrons, enlargement ratio 200000；B figures are the present embodiment synthesis
The nanocrystalline transmission energy spectrum diagram of nucleocapsid AuRh star decahedrons, wherein red indicate that Au elements, green indicate Rh elements,
B figure enlargement ratios are 250000.A figures are as it can be seen that the present embodiment obtains being that the more uniform star decahedron of size is received from Fig. 2
Meter Jing, and the transmission power spectrum of B figures shows that the final product that the present embodiment obtains be metal Au is kernel in Fig. 2, metal Rh is outer
Shell nucleocapsid.To the nanocrystalline carry out electrochemical property test of nucleocapsid AuRh star decahedrons of the present embodiment synthesis, Fig. 3
For corresponding polarization curve, it can be seen that the nucleocapsid AuRh star decahedrons that the present embodiment obtains are nanocrystalline excessively electric
Position is significantly less than the business Rh/C catalyst of same content of metal.Prove the nucleocapsid AuRh stars ten that the present embodiment obtains
Face body is nanocrystalline to have excellent catalytic activity for water electrolysis hydrogen production.
Embodiment 2
A kind of nucleocapsid AuRh star decahedrons are nanocrystalline, and preparation method is：
(1) under room temperature, gold chloride is dissolved in 3 milliliters of oleyl amines, magnetic agitation is uniform, and compound concentration is
The chlorauric acid solution of 0.01mol/L；
(2) 7 milliliters of oleyl amines are added in 25 milliliters of three-necked flasks, which is put into 110 degrees Celsius of oil bath pans
In, magnetic agitation preheat 10 minutes, with pipettor be rapidly injected step (1) made from chlorauric acid solution, the reaction was continued 4 hours,
After reaction product through hexamethylene and ethyl alcohol centrifuge washing three times, the black precipitate of acquisition is scattered in 10 milliliters of oleyl amines again
In solution, gold particle seed solution is obtained；
(3) under room temperature, hexadecyltrimethylammonium chloride is dissolved in 5 milliliters of oleyl amines, magnetic agitation is uniform, matches
Make the hexadecyltrimethylammonium chloride solution of a concentration of 0.18mol/L；Acetylacetone,2,4-pentanedione rhodium is dissolved in 3 milliliters of oleyl amines, magnetic
Power stirs evenly, and compound concentration is the acetylacetone,2,4-pentanedione rhodium solution of 0.004mol/L；
(4) from 2 milliliters of addition to three-necked flasks of taking-up in the gold particle seed solution of step (2), in three-necked flask
The hexadecyltrimethylammonium chloride solution for continuously adding step (3) preparation, is put into 190 degrees Celsius of oil bath pans, magnetic agitation
Preheating 8 minutes is rapidly injected the acetylacetone,2,4-pentanedione rhodium solution of step (3) preparation using pipettor, and the reaction was continued 3 hours；
(5) product for obtaining step (4) through hexamethylene and ethyl alcohol centrifuge washing three times, remove supernatant, taking precipitate；
(6) the sediment ultrasonic disperse for obtaining step (5) in hexamethylene to get nucleocapsid AuRh star decahedrons
Nanocrystalline dispersion liquid.The dispersion liquid room temperature preserves.
The result that the present embodiment obtains is similar to Example 1.
Embodiment 3
A kind of nucleocapsid AuRh star decahedrons are nanocrystalline, and preparation method is：
(1) under room temperature, chlorauride is dissolved in 3 milliliters of oleyl amines, magnetic agitation is uniform, and compound concentration is
The chlorogold solution of 0.02mol/L；
(2) 7 milliliters of oleyl amines are added in 25 milliliters of three-necked flasks, which is put into 180 degrees Celsius of oil bath pans
In, magnetic agitation preheats 10 minutes, and the chlorogold solution of step (1) preparation is rapidly injected with pipettor, and the reaction was continued 3 hours,
After reaction product through hexamethylene and ethyl alcohol centrifuge washing three times, the black precipitate of acquisition is scattered in 10 milliliters of oleyl amines again
In solution, gold particle seed solution is obtained；
(3) under room temperature, cetyl trimethylammonium bromide is dissolved in 6 milliliters of oleyl amines, magnetic agitation is uniform, matches
Make the cetyl trimethylammonium bromide solution of a concentration of 0.12mol/L；Radium chloride is dissolved in 3 milliliters of oleyl amines, magnetic force stirs
It mixes uniformly, compound concentration is the rhodium chloride solution of 0.004mol/L；
(4) from 1 milliliter of addition to three-necked flask of taking-up in the gold particle seed solution of step (2), in three-necked flask
The cetyl trimethylammonium bromide solution for continuously adding step (3) preparation, is put into 180 degrees Celsius of oil bath pans, magnetic agitation
Preheating 10 minutes is rapidly injected the rhodium chloride solution of step (3) preparation using pipettor, and the reaction was continued 3 hours；
(5) product for obtaining step (4) through hexamethylene and ethyl alcohol centrifuge washing three times, remove supernatant, taking precipitate；
(6) the sediment ultrasonic disperse for obtaining step (5) in hexamethylene to get nucleocapsid AuRh star decahedrons
Nanocrystalline dispersion liquid.The dispersion liquid room temperature preserves.
The result that the present embodiment obtains is similar to Example 1.
Embodiment 4
A kind of nucleocapsid AuRh star decahedrons are nanocrystalline, and preparation method is：
(1) under room temperature, gold chloride is dissolved in 3 milliliters of oleyl amines, magnetic agitation is uniform, and compound concentration is
The chlorauric acid solution of 0.015mol/L；
(2) 7 milliliters of oleyl amines are added in 25 milliliters of three-necked flasks, which is put into 180 degrees Celsius of oil bath pans
In, magnetic agitation preheats 10 minutes, and the chlorauric acid solution of step (1) preparation is rapidly injected with pipettor, and the reaction was continued 3 hours,
After reaction product through hexamethylene and ethyl alcohol centrifuge washing three times, the black precipitate of acquisition is scattered in 10 milliliters of oleyl amines again
In solution, gold particle seed solution is obtained；
(3) under room temperature, double dodecyl trimethyl ammonium bromide are dissolved in 5 milliliters of oleyl amines, compound concentration is
Double dodecyl trimethyl ammonium bromide solution of 0.18mol/L；Radium chloride is dissolved in 3 milliliters of oleyl amines, magnetic agitation is uniform,
Compound concentration is the rhodium chloride solution of 0.009mol/L；
(4) 2 milliliters are taken out in the gold particle seed solution obtained from step (2) to be added into three-necked flask, burnt at three mouthfuls
Double dodecyl trimethyl ammonium bromide solution that step (3) preparation is continuously added in bottle, are put into 180 degrees Celsius of oil bath pans, magnetic
Power stirring preheating 10 minutes, the rhodium chloride solution of step (3) preparation is rapidly injected using pipettor, the reaction was continued 3 hours；
(5) product for obtaining step (4) through hexamethylene and ethyl alcohol centrifuge washing three times, remove supernatant, taking precipitate；
(6) the sediment ultrasonic disperse for obtaining step (5) in hexamethylene to get nucleocapsid AuRh star decahedrons
Nanocrystalline dispersion liquid.The dispersion liquid room temperature preserves.
The result that the present embodiment obtains is similar to Example 1.
Embodiment 5
A kind of nucleocapsid AuRh star decahedrons are nanocrystalline, and preparation method is：
(1) under room temperature, chlorauride is dissolved in 3 milliliters of oleyl amines, magnetic agitation is uniform, and compound concentration is
The chlorogold solution of 0.025mol/L；
(2) 7 milliliters of oleyl amines are added in 25 milliliters of three-necked flasks, which is put into 110 degrees Celsius of oil bath pans
In, magnetic agitation preheats 10 minutes, and the chlorogold solution of step (1) preparation is rapidly injected with pipettor, and the reaction was continued 4 hours,
After reaction product through hexamethylene and ethyl alcohol centrifuge washing three times, the black precipitate of acquisition is scattered in 10 milliliters of oleyl amines again
In solution, gold particle seed solution is obtained；
(3) under room temperature, hexadecyltrimethylammonium chloride is dissolved in 5 milliliters of oleyl amines, compound concentration is
The hexadecyltrimethylammonium chloride solution of 0.15mol/L；Acetylacetone,2,4-pentanedione rhodium is dissolved in 3 milliliters of oleyl amines, magnetic agitation is equal
Even, compound concentration is the acetylacetone,2,4-pentanedione rhodium solution of 0.02mol/L；
(4) from 2 milliliters of addition to three-necked flasks of taking-up in the gold particle seed solution of step (2), in three-necked flask
The hexadecyltrimethylammonium chloride solution for continuously adding step (3) preparation, is put into 190 degrees Celsius of oil bath pans, magnetic agitation
Preheating 8 minutes is rapidly injected the acetylacetone,2,4-pentanedione rhodium solution of step (3) preparation using pipettor, and the reaction was continued 3 hours；
(5) product for obtaining step (4) through hexamethylene and ethyl alcohol centrifuge washing three times, remove supernatant, taking precipitate；
(6) the sediment ultrasonic disperse for obtaining step (5) in hexamethylene to get nucleocapsid AuRh star decahedrons
Nanocrystalline dispersion liquid.The dispersion liquid room temperature preserves.Obtained result is similar to Example 1.
Embodiment 6
A kind of nucleocapsid AuRh star decahedrons are nanocrystalline, and preparation method is：
(1) under room temperature, gold chloride is dissolved in 3 milliliters of oleyl amines, magnetic agitation is uniform, and compound concentration is
The chlorauric acid solution of 0.03mol/L；
(2) 7 milliliters of oleyl amines are added in 25 milliliters of three-necked flasks, which is put into 180 degrees Celsius of oil bath pans
In, magnetic agitation preheats 10 minutes, and the chlorauric acid solution of step (1) preparation is rapidly injected with pipettor, and the reaction was continued 3 hours,
After reaction product through hexamethylene and ethyl alcohol centrifuge washing three times, the black precipitate of acquisition is scattered in 10 milliliters of oleyl amines again
In solution, gold particle seed solution is obtained；
(3) under room temperature, hexadecyltrimethylammonium chloride is dissolved in 5 milliliters of oleyl amines, compound concentration is
The hexadecyltrimethylammonium chloride solution of 0.27mol/L；Trifluoracetic acid rhodium dimer is dissolved in 2 milliliters of oleyl amines, magnetic force
It stirs evenly, compound concentration is the trifluoracetic acid rhodium dimerization liquid solution of 0.027mol/L；
(4) 3 milliliters are taken out in the gold particle seed solution obtained from step (2) to be added into three-necked flask, burnt at three mouthfuls
The hexadecyltrimethylammonium chloride solution that step (3) preparation is continuously added in bottle, is put into 180 degrees Celsius of oil bath pans, magnetic force
Stirring preheating 10 minutes, the trifluoracetic acid rhodium dimerization liquid solution of step (3) preparation is rapidly injected using pipettor, the reaction was continued 3
Hour；
(5) product for obtaining step (4) through hexamethylene and ethyl alcohol centrifuge washing three times, remove supernatant, taking precipitate；
(6) the sediment ultrasonic disperse for obtaining step (5) in hexamethylene to get nucleocapsid AuRh star decahedrons
Nanocrystalline dispersion liquid.The dispersion liquid room temperature preserves.
The result that the present embodiment obtains is similar to Example 1.
Embodiment 7
A kind of nucleocapsid AuRh star decahedrons are nanocrystalline, and preparation method is：
(1) under room temperature, chlorauride is dissolved in 3 milliliters of oleyl amines, magnetic agitation is uniform, and compound concentration is
The chlorogold solution of 0.03mol/L；
(2) 7 milliliters of oleyl amines are added in 25 milliliters of three-necked flasks, which is put into 180 degrees Celsius of oil bath pans
In, magnetic agitation preheats 10 minutes, and the chlorogold solution of step (1) preparation is rapidly injected with pipettor, and the reaction was continued 3 hours,
After reaction product through hexamethylene and ethyl alcohol centrifuge washing three times, the black precipitate of acquisition is scattered in 10 milliliters of oleyl amines again
In solution, gold particle seed solution is obtained；
(3) under room temperature, double dodecyl trimethyl ammonium bromide are dissolved in 5 milliliters of oleyl amines, compound concentration is
Double dodecyl trimethyl ammonium bromide solution of 0.54mol/L；Trifluoracetic acid rhodium dimer is dissolved in 3 milliliters of oleyl amines, magnetic
Power stirs evenly, and compound concentration is the trifluoracetic acid rhodium dimerization liquid solution of 0.03mol/L；
(4) 2 milliliters are taken out in the gold particle seed solution prepared from step (2) to be added into three-necked flask, burnt at three mouthfuls
Double dodecyl trimethyl ammonium bromide solution that step (3) preparation is continuously added in bottle, are put into 180 degrees Celsius of oil bath pans, magnetic
Power stirring preheating 10 minutes, the trifluoracetic acid rhodium dimerization liquid solution of step (3) preparation is rapidly injected using pipettor, the reaction was continued
3 hours；
(5) product for obtaining step (4) through hexamethylene and ethyl alcohol centrifuge washing three times, remove supernatant, taking precipitate；
(6) the sediment ultrasonic disperse for obtaining step (5) in hexamethylene to get nucleocapsid AuRh star decahedrons
Nanocrystalline dispersion liquid.The dispersion liquid room temperature preserves.
The result that the present embodiment obtains is similar to Example 1.
Embodiment 8
A kind of nucleocapsid AuRh star decahedrons are nanocrystalline, and preparation method is：
(1) under room temperature, gold chloride is dissolved in 3 milliliters of oleyl amines, magnetic agitation is uniform, and compound concentration is
The chlorauric acid solution of 0.01mol/L；
(2) 7 milliliters of oleyl amines are added in 25 milliliters of three-necked flasks, are put into 110 degrees Celsius of oil bath pans, magnetic agitation is pre-
Heat 10 minutes is rapidly injected the chlorauric acid solution of step (1) preparation with pipettor, and the reaction was continued 4 hours, product after reaction
Three times through hexamethylene and ethyl alcohol centrifuge washing, the black precipitate of acquisition is scattered in again in 10 milliliters of oleyl amine solution, obtains gold
Grain seed solution；
(3) under room temperature, double dodecyl trimethyl ammonium bromide are dissolved in 5 milliliters of oleyl amines, compound concentration is
Double dodecyl trimethyl ammonium bromide solution of 0.18mol/L；Trifluoracetic acid rhodium dimer is dissolved in 3 milliliters of oleyl amines, magnetic
Power stirs evenly, and compound concentration is the trifluoracetic acid rhodium dimerization liquid solution of 0.002mol/L；
(4) 2 milliliters are taken out in the gold particle seed solution obtained from step (2) to be added into three-necked flask, burnt at three mouthfuls
Double dodecyl trimethyl ammonium bromide solution that step (3) preparation is continuously added in bottle, are put into 190 degrees Celsius of oil bath pans, magnetic
Power stirring preheating 8 minutes, the trifluoracetic acid rhodium dimerization liquid solution of step (3) preparation is rapidly injected using pipettor, the reaction was continued 3
Hour；
(5) product for obtaining step (4) through hexamethylene and ethyl alcohol centrifuge washing three times, remove supernatant, taking precipitate；
(6) the sediment ultrasonic disperse for obtaining step (5) in hexamethylene to get nucleocapsid AuRh star decahedrons
Nanocrystalline dispersion liquid.The dispersion liquid room temperature preserves.
The result that the present embodiment obtains is similar to Example 1.
Claims (10)
1. a kind of nucleocapsid AuRh star decahedrons are nanocrystalline, which is characterized in that the nucleocapsid AuRh star decahedrons
In nanocrystalline, metal Au is kernel, and metal Rh is shell.
2. nucleocapsid AuRh star decahedrons according to claim 1 are nanocrystalline, which is characterized in that the nucleocapsid
The nanocrystalline grain size of AuRh star decahedrons is 10-12nm.
3. nucleocapsid AuRh star decahedrons according to claim 1 are nanocrystalline, which is characterized in that the nucleocapsid
During AuRh star decahedrons are nanocrystalline, the molar ratio of Au elements and Rh elements is 1: 1~1: 5.
4. the nanocrystalline preparation method of nucleocapsid AuRh star decahedrons described in a kind of any one of claims 1 to 3,
It is characterized in that, the preparation method includes the following steps：
1) Au presomas are dissolved in oleyl amine, obtain the first solution；
2) first solution that step 1) obtains is added to and is preheated in 110~180 DEG C of oleyl amine, it is anti-at 110~180 DEG C
It answers 3~4 hours, centrifuges, obtained black precipitate is scattered in oleyl amine by washing again, obtains seed solution；
3) the oleyl amine solution of dressing agent is added in the seed solution obtained to step 2), be uniformly mixed and it is preheated to 180~
After 190 DEG C, the oleyl amine solution of Rh presomas is added, is stirred to react 3~4 hours at 180~190 DEG C, centrifuges, washing obtains institute
It is nanocrystalline to state nucleocapsid AuRh star decahedrons；
The dressing agent is cetyl trimethylammonium bromide, hexadecyltrimethylammonium chloride or double trimethyl bromines
Change ammonium.
5. preparation method according to claim 4, which is characterized in that the Au presomas are chlorauride or gold chloride；Institute
It is acetylacetone,2,4-pentanedione rhodium, radium chloride or trifluoracetic acid rhodium dimer to state Rh presomas.
6. preparation method according to claim 4, which is characterized in that in step 1), in first solution, before the Au
Drive a concentration of 0.01~0.03mol/L of body.
7. preparation method according to claim 4, which is characterized in that in step 2), first solution and the preheating
Volume ratio to 110~180 DEG C of oleyl amines is 3: 5~3: 9.
8. preparation method according to claim 4, which is characterized in that in step 3), the Au elements of addition and dressing agent
Molar ratio is 1: 50~150, Au elements and the molar ratio of Rh elements is 1: 1~5.
9. preparation method according to claim 4, which is characterized in that in step 3), in the oleyl amine solution of the dressing agent,
A concentration of 0.12~0.54mol/L of dressing agent；In the oleyl amine solution of the Rh presomas, a concentration of the 0.002 of Rh presomas
~0.03mol/L.
10. nanocrystalline the answering in catalytic field of nucleocapsid AuRh star decahedrons described in any one of claims 1 to 3
With.
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