CN107008895B - A kind of rhotanium nanometer rods and preparation method thereof with excellent near-infrared absorption and PhotoelectrocatalytiPerformance Performance - Google Patents
A kind of rhotanium nanometer rods and preparation method thereof with excellent near-infrared absorption and PhotoelectrocatalytiPerformance Performance Download PDFInfo
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- CN107008895B CN107008895B CN201710237281.6A CN201710237281A CN107008895B CN 107008895 B CN107008895 B CN 107008895B CN 201710237281 A CN201710237281 A CN 201710237281A CN 107008895 B CN107008895 B CN 107008895B
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- 238000010521 absorption reaction Methods 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 75
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims abstract description 44
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000007864 aqueous solution Substances 0.000 claims abstract description 37
- 239000002105 nanoparticle Substances 0.000 claims abstract description 30
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 26
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000010931 gold Substances 0.000 claims abstract description 25
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims abstract description 25
- 229910052737 gold Inorganic materials 0.000 claims abstract description 24
- 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 abstract description 21
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 21
- 239000011734 sodium Substances 0.000 claims abstract description 21
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 19
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 14
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 14
- 238000013019 agitation Methods 0.000 claims abstract description 11
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 22
- 239000000047 product Substances 0.000 claims description 16
- 239000002244 precipitate Substances 0.000 claims description 15
- BBKFSSMUWOMYPI-UHFFFAOYSA-N gold palladium Chemical compound [Pd].[Au] BBKFSSMUWOMYPI-UHFFFAOYSA-N 0.000 claims description 11
- 239000002253 acid Substances 0.000 claims description 10
- 229910052763 palladium Inorganic materials 0.000 claims description 10
- KGYLMXMMQNTWEM-UHFFFAOYSA-J tetrachloropalladium Chemical compound Cl[Pd](Cl)(Cl)Cl KGYLMXMMQNTWEM-UHFFFAOYSA-J 0.000 claims description 9
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 claims description 8
- 239000004615 ingredient Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- AISMNBXOJRHCIA-UHFFFAOYSA-N trimethylazanium;bromide Chemical compound Br.CN(C)C AISMNBXOJRHCIA-UHFFFAOYSA-N 0.000 claims description 4
- 238000005352 clarification Methods 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 1
- 238000006555 catalytic reaction Methods 0.000 abstract description 7
- 230000009467 reduction Effects 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 230000005693 optoelectronics Effects 0.000 abstract description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 2
- 238000007146 photocatalysis Methods 0.000 abstract description 2
- 238000003860 storage Methods 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 15
- 238000000034 method Methods 0.000 description 14
- 239000003643 water by type Substances 0.000 description 14
- 230000003197 catalytic effect Effects 0.000 description 12
- 230000005540 biological transmission Effects 0.000 description 10
- 238000003756 stirring Methods 0.000 description 9
- 239000003054 catalyst Substances 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 239000002131 composite material Substances 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 6
- 239000003638 chemical reducing agent Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 241000209094 Oryza Species 0.000 description 4
- 235000007164 Oryza sativa Nutrition 0.000 description 4
- 238000002484 cyclic voltammetry Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 235000009566 rice Nutrition 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000000084 colloidal system Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000002073 nanorod Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- GDSOZVZXVXTJMI-SNAWJCMRSA-N (e)-1-methylbut-1-ene-1,2,4-tricarboxylic acid Chemical compound OC(=O)C(/C)=C(C(O)=O)\CCC(O)=O GDSOZVZXVXTJMI-SNAWJCMRSA-N 0.000 description 1
- RHAXKFFKGZJUOE-UHFFFAOYSA-N 7-acetyl-6-ethyl-3,5,8-trihydroxy-9,10-dioxoanthracene-1,2-dicarboxylic acid Chemical compound O=C1C2=CC(O)=C(C(O)=O)C(C(O)=O)=C2C(=O)C2=C1C(O)=C(CC)C(C(C)=O)=C2O RHAXKFFKGZJUOE-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 241000976924 Inca Species 0.000 description 1
- 235000000177 Indigofera tinctoria Nutrition 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000012696 Pd precursors Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 description 1
- HRHBQGBPZWNGHV-UHFFFAOYSA-N azane;bromomethane Chemical compound N.BrC HRHBQGBPZWNGHV-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- RFXSFVVPCLGHAU-UHFFFAOYSA-N benzene;phenol Chemical compound C1=CC=CC=C1.OC1=CC=CC=C1.OC1=CC=CC=C1 RFXSFVVPCLGHAU-UHFFFAOYSA-N 0.000 description 1
- 230000031709 bromination Effects 0.000 description 1
- 238000005893 bromination reaction Methods 0.000 description 1
- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000006735 epoxidation reaction Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000013007 heat curing Methods 0.000 description 1
- XQSBLCWFZRTIEO-UHFFFAOYSA-N hexadecan-1-amine;hydrobromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[NH3+] XQSBLCWFZRTIEO-UHFFFAOYSA-N 0.000 description 1
- 230000033444 hydroxylation Effects 0.000 description 1
- 238000005805 hydroxylation reaction Methods 0.000 description 1
- 229940097275 indigo Drugs 0.000 description 1
- COHYTHOBJLSHDF-UHFFFAOYSA-N indigo powder Natural products N1C2=CC=CC=C2C(=O)C1=C1C(=O)C2=CC=CC=C2N1 COHYTHOBJLSHDF-UHFFFAOYSA-N 0.000 description 1
- 239000006193 liquid solution Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000001404 mediated effect Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000006053 organic reaction Methods 0.000 description 1
- 238000005120 petroleum cracking Methods 0.000 description 1
- 238000007626 photothermal therapy Methods 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
-
- 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
- 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
-
- 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
Abstract
The present invention relates to a kind of rhotanium nanometer rods and preparation method thereof, it is characterized in that the rhotanium nanometer rods obtained have excellent near-infrared absorption and PhotoelectrocatalytiPerformance Performance.Its preparation step are as follows: (1) gold nanoparticle seed is prepared in cetyl trimethylammonium bromide aqueous solution using sodium borohydride reduction；(2) under agitation, gold chloride, sodium tetrachloropallate, silver nitrate, hydroquinone aqueous solution are successively added in cetyl trimethylammonium bromide aqueous solution, acquisition prepares the growth solution of rhotanium nanometer rods；(3) a certain amount of gold nanoparticle seed colloidal solution is added in the growth solution of step (2) preparation, 40-70 degrees Celsius reaction 0.5-3 hour, acquisition green rhotanium nanometer rods colloidal solution.The rhotanium nanometer rods with excellent near-infrared absorption and PhotoelectrocatalytiPerformance Performance that the present invention obtains have important application value in terms of photocatalysis, electro-catalysis, opto-electronic device, information storage, near infrared light.
Description
Technical field
The present invention relates to a kind of rhotanium nanometer rods with excellent near-infrared absorption and PhotoelectrocatalytiPerformance Performance and its
Preparation method.
Background technique
Metal Palladium has very excellent catalytic performance, as important catalyst, in Industrial Catalysis, fuel cell, medicine
The fields such as object synthesis, purifying vehicle exhaust, petroleum cracking, water process have important application value.It is known that metal catalytic
Reaction typically occurs in the surface of particle, it is clear that its catalytic activity can effectively be enhanced by reducing catalyst particle size.However, right
For catalyst, other than catalytic efficiency, another important performance is then its stability.Pure Pd nano particle was using
The problems such as being prone to aggregation, dissolution, oxidation in journey, and then cause its catalytic performance to reduce and even inactivate.With Pd nano particle
It compares, gold nanoparticle is not only with good stability but also has unique surface plasmon absorption characteristic and life
Object compatibility.Studies have shown that Pd nano particle deposition is coated on the good Au nanoparticle sublist of chemical property torpescence, acid resistance
Face can effectively improve the catalytic activity and stabilization of palladium.Therefore, it constructs gold-palladium composite nanoparticle and causes people in recent years
Extensive concern.Currently, the synthetic strategy of gold-palladium composite nanoparticle mainly includes seed mediated growth method and co-reducing process.Based on kind
Sub- growth method, people's cetyl trimethylammonium bromide or hexadecyltrimethylammonium chloride make surfactant, and L- is anti-bad
Hematic acid makees reducing agent, makees seed with the gold nanoparticle of different-shape, synthesized in aqueous solution rodlike, octahedra, cubic block,
Golden@palladium nucleocapsid, the Heterogeneous Composite nanoparticle of a series of different-shapes such as flower-shaped.In addition, under the conditions of certain temperature, Ren Menxiang
Gold, two kinds of metal salts of palladium, surfactant coexist and add suitable sodium citrate, hydrazine, sodium borohydride, L-AA in solution
Make reducing agent, spherical, flower-shaped, dendritic, starlike rhotanium, core-shell nano are successfully prepared using co-reducing process.However,
The gold-palladium composite nanoparticle that the above method is constructed is although effectively increase the catalytic activity and stability of precious metal palladium, can
See, near-infrared region does not show good surface plasmon absorption characteristic.That is, using existing synthesis
Route, people are difficult to prepare the gold-palladium composite nanoparticle with superior optical characteristics.In recent years, total based on surface plasma
Photochemical catalyst of the noble metal/semiconductor plasma photochemical catalyst that vibration effect is constructed as a kind of novel photoresponse, has succeeded
For all more important organic reactions such as catalytic alcohol oxidation, alkene epoxidation, nitro reduction, the coupling of carbon carbon, benzene hydroxylations, in benefit
Huge application potential is shown with solar energy aspect.Obviously, pass through two kinds of organic collection alloy that acts synergistically between metal, palladium materials
The advantages of, the gold-palladium composite nanoparticle with catalysis and surface plasmon absorption multiple performance is constructed with important
Scientific meaning and practical application value.These characteristics will make it in surface plasma bulk optics, Industrial Catalysis, pharmaceutical synthesis, light
Being catalyzed organic synthesis, photo-thermal therapy etc. has very wide application prospect.
Summary of the invention
The problem to be solved in the present invention is to overcome the shortcoming of existing rhotanium nanoparticle technology of preparing, provides one
Kind is simple, efficiently prepares the synthetic method of rhotanium nanometer rods in aqueous solution.It is another object of the present invention to prepare
Different scale has the rodlike rhotanium nanoparticle of excellent near-infrared absorption and PhotoelectrocatalytiPerformance Performance, is photocatalysis, electricity
Catalysis, opto-electronic device, information storage, near infrared light heat cure etc. practical application provide material base.
Rodlike rhotanium nanometer with near-infrared absorption and PhotoelectrocatalytiPerformance Performance in the present invention is raw using seed
Regular way is heated under ambiance containing gold chloride, sodium tetrachloropallate, cetyl trimethylammonium bromide, hydroquinone, a small amount of nitre
What the aqueous solution of sour silver and gold nanoparticle seed obtained, comprising the following specific steps
(1) at room temperature, cetyl trimethylammonium bromide is added in aqueous solution, is obtained after mixing evenly dense
Degree is the achromaticity and clarification cetyl trimethylammonium bromide aqueous solution of 0.02-0.3 mol/L；
(2) prepared by gold nanoparticle seed: aqueous solution of chloraurate is added to 1-15 milliliters of cetyl trimethyl brominations
Aqueous ammonium, stirring rapidly join sodium borohydride aqueous solution after 2 minutes, the gold nanoparticle that scale is 2-3 nanometers is obtained, 35
Placed under degree Celsius make within 1-5 hours remain sodium borohydride decomposes completely, wherein gold chloride, sodium borohydride concentration be respectively
0.0001-0.001 mol/L, 0.0001-0.001 mol/L；
(3) rhotanium nanorod growth solution prepare: by gold chloride, sodium tetrachloropallate, a small amount of silver nitrate aqueous solution according to
It is secondary to be added in cetyl trimethylammonium bromide aqueous solution, brown solution is obtained after mixing evenly, is then added a certain amount of
Hydroquinone aqueous solution, solution colour are become colorless clear solution by yellowish-brown, and acquisition prepares the growth of rhotanium nanometer rods
Solution, wherein cetyl trimethylammonium bromide, gold chloride, sodium tetrachloropallate, silver nitrate, hydroquinone concentration be respectively
0.02-0.3 mol/L, 0.00005-0.005 mol/L, 0.00005-0.005 mol/L, 0.00001-0.0005 moles/
It rises, 0.005-0.05 mol/L；
(4) the gold nanoparticle seed colloidal solution that a certain amount of step (2) obtain is added to the growth of step (3) preparation
It in solution, is reacted 0.5-3 hours in 40-70 degrees Celsius of baking oven, obtains green rhotanium nanometer rods colloidal solution；
(5) rhotanium nanometer rods colloidal solution supercentrifuge under the conditions of 10000-14500 revs/min of revolving speed from
After heart 5-60 minutes, colourless solution in centrifuge tube is removed, obtains green precipitate product；
(6) the green precipitate product obtained with 18.2 megaohms of deionized water ultrasonic cleaning, is made the gold of different scale, ingredient
Palldium alloy nanometer rods.
Beneficial effects of the present invention:
(1) the present invention provides a kind of methods for preparing rhotanium nanometer rods, it is characterised in that rhotanium nanometer rods
It is that reducing agent is made with hydroquinone in cetyl trimethylammonium bromide aqueous solution, using chemical coreduction and Seed inducement
The method preparation combined is grown, it is easy to operation, experimental repeatability is good；
(2) the rhotanium nanometer rods yield of this method preparation is high, size is uniform, scale is adjustable；
(3) the rhotanium nanometer rods colloid color of this method preparation is green, is received different from reported other gold-palladiums
Rice corpuscles, spectral measurement and electrochemistry experiment show that rhotanium nanometer rods have excellent near-infrared absorption and photoelectrocatalysis
Energy；
(4) the rhotanium nanometer rods yield of this method preparation is high, and the scale of particle, draw ratio can pass through cetyl three
Methyl bromide ammonium concentration, hydroquinone concentration, the experiment parameters such as gold-palladium molar ratio, reaction time, seed additive amount in presoma
Effective Regulation is carried out, and then obtains the rhotanium nanometer rods of different draw ratios；
(5) this method can prepare rhotanium nanometer rods in the different precursor solution of gold-palladium molar concentration rate,
And rhotanium nanometer rods ingredient, performance can pass through gold-palladium precursor concentration Effective Regulation；
(6) gold can be prepared in the precursor solution that this method is under condition of different temperatures, gold-palladium molar concentration is different
Palldium alloy nanometer rods；
Detailed description of the invention
Fig. 1 is multiple optics shot after visually observing to rhotanium nanometer rods preparation process every 10 minutes with camera
Photo, the results show that solution colour was ultimately become by grey (10 minutes) by blue (20 minutes), Indigo (30 minutes)
Green (40-80 minutes)；
Fig. 2 is clapped after rhotanium nanometer rods obtained Japan Electronics JEOL-1400 transmission electron microscope observation
Multiple transmission electron microscope photos and particle size distribution taken the photograph, wherein Fig. 2 a is rhotanium nanometer rods low power transmission electron microscope photo,
Fig. 2 b is rhotanium nanometer rods high power transmission electron microscope photo, and Fig. 2 c is rhotanium nanorod diameter size distribution histogram,
Fig. 2 d is rhotanium nanorod length size distribution histogram.As can be seen that the average diameter of rhotanium nanometer rods is 7.5
Nm, average length are 26 nm, and draw ratio is about 3.5；
Fig. 3 is by the scanning transmission electron microscope photo of rhotanium nanometer rods obtained and with Inca. Oxford type
X-ray energy disperse spectroscopy carries out the X-ray energy spectrum diagram obtained after power spectrum test, the results show that the ingredient of the nanometer rods obtained includes
Gold and is uniformly distributed two kinds of elements of palladium in the grain, illustrate made from product be rhotanium nanometer rods；
Fig. 4 is with Japan Shimadzu UV-3101PC type ultraviolet-visible-near infrared spectrometer (UV-Vis-NIR)
Rhotanium nanometer rods obtained are carried out with the optical absorption map of test acquisition, wherein ordinate is absorption intensity, and abscissa is
Optical wavelength.It can be seen from the figure that rhotanium nanometer rods have lateral, longitudinal duplex surface plasma resonance absorption
Can, wherein lateral plasma resonance absorption peak is located at 510 nm, longitudinal plasma resonance absorption peak 710 nm and its absorb by force
For degree much larger than lateral plasma absorption, this shows that rhotanium nanometer rods have excellent near-infrared absorption performance；
Fig. 5 is the cyclic voltammetry curve of the Catalytic oxidation of ethanol measured by Shanghai Chen Hua 760D electrochemical workstation.Its
In, curve a is the Catalytic oxidation of ethanol for using the rhotanium nanometer rods that gold-palladium ratio obtained is 1:1 to measure as catalyst
Cyclic voltammetry curve, curve b are cyclic voltammetry curve of the commercialized palladium/carbon catalyst to Catalytic oxidation of ethanol, and curve c is to use
The cyclic voltammetry curve for the Catalytic oxidation of ethanol that gold nanorods obtained are measured as catalyst, the results showed that, rhotanium is received
Rice stick shows excellent catalytic activity in the catalysis oxidation of ethyl alcohol；
Fig. 6 is made in various concentration cetyl trimethylammonium bromide solution under other experiment parameter permanence conditions
Rhotanium nanometer rods transmission electron microscope photo, wherein the concentration of cetyl trimethylammonium bromide is respectively as follows: 0.05 and rubs
You/liter (Fig. 6 a), 0.075 mol/L (Fig. 6 b), 0.125 mol/L (Fig. 6 c), 0.15 mol/L (Fig. 6 d), own in figure
Scale is 100 nanometers；
Fig. 7 is rhotanium nanometer rods obtained under gold chloride concentration different condition under other experiment parameter permanence conditions
Transmission electron microscope photo, wherein the concentration of gold chloride be respectively as follows: 0.0002 mol/L (Fig. 7 a), 0.0003 mol/L (figure
7b), 0.0004 mol/L (Fig. 7 c), 0.0005 mol/L (Fig. 7 d), all scales are 100 nanometers in figure；
Fig. 8 is under other experiment parameter permanence conditions, and rhotanium obtained is received under tetrachloro-palladium acid na concn different condition
The transmission electron microscope photo of rice stick, wherein the concentration of sodium tetrachloropallate is respectively as follows: 0.0001 mol/L (Fig. 8 a), 0.0002 rubs
You/liter (Fig. 8 b), 0.0003 mol/L (Fig. 8 c), 0.0004 mol/L (Fig. 8 d), all scales are 100 nanometers in figure；
Fig. 9 is to make rhotanium made from reducing agent with various concentration hydroquinone under other experiment parameter permanence conditions
The transmission electron microscope photo of nanometer rods, wherein the concentration of hydroquinone be respectively as follows: 0.004 mol/L (Fig. 9 a), 0.006 mole/
Rise (Fig. 9 b), 0.008 mol/L (Fig. 9 c), 0.01 mol/L (Fig. 9 d), 0.012 mol/L (Fig. 9 e), 0.014 mol/L
(Fig. 9 f), all scales are 100 nanometers in figure；
Figure 10 is the transmission electricity of rhotanium nanometer rods made from differential responses temperature under other experiment parameter permanence conditions
Mirror photo, wherein reaction temperature is respectively 40 degrees Celsius (Figure 10 a), 50 degrees Celsius (Figure 10 b), 60 degrees Celsius (Figure 10 c), 70
Degree Celsius (Figure 10 d), all scales are 100 nanometers in figure.
Specific embodiment
First from market purchase the present invention use gold chloride, sodium tetrachloropallate, cetyl trimethylammonium bromide, to benzene
Diphenol, silver nitrate, sodium borohydride；Then gold chloride, sodium tetrachloropallate, cetyl trimethyl are prepared with 18 megaohms of deionized waters
Ammonium bromide, hydroquinone, silver nitrate, sodium borohydride aqueous solution, wherein cetyl trimethylammonium bromide, gold chloride, tetrachloro palladium
Sour sodium, silver nitrate, sodium borohydride, hydroquinone concentration of aqueous solution be respectively 0.2 mol/L, 0.1 mol/L, 0.1 mole/
Liter, 0.1 mol/L, 0.1 mol/L, 1 mol/L.
Gold nanoparticle seed is prepared with sodium borohydride reduction: by 6 ml deionized waters, 0.06 milliliter of 0.1 mol/L
Aqueous solution of chloraurate is successively added to the cetyl ammonium bromide aqueous solution of 6 milliliter of 0.2 mol/L, stirring 2 under agitation
Sodium borohydride aqueous solution is rapidly joined under 1200 revs/min of revolving speeds after minute, solution colour becomes dark brown from yellow rapidly, obtains
The gold nanoparticle colloid solution that scale is 2-3 nanometers is obtained, placing under 35 degrees Celsius makes to remain sodium borohydride decomposes completely,
In, gold chloride, sodium borohydride concentration be 0.0005 mol/L, gold nanoparticle place 1-5 hour it is interior with effect most
It is good.
The contents of the present invention are described in further detail below with reference to specific implementation example, but the present invention is not limited to following
The specific examples enumerated.
Embodiment 1
7.5 × 26 nanometers of rhotanium nanometer rods preparation
By 9.1 ml deionized waters, 0.1 milliliter of 0.1 mol/L gold chloride, 0.1 milliliter of 0.1 mol/L tetrachloro-palladium acid
Sodium, 0.02 milliliter of 0.1 mol/L silver nitrate aqueous solution are successively added to 10 milliliter of 0.2 mol/L hexadecane under agitation
In base trimethylammonium bromide solution, brown solution is obtained after mixing evenly, and 0.2 milliliter of 1 mol/L hydroquinone is then added
Aqueous solution, wherein cetyl trimethylammonium bromide, gold chloride, sodium tetrachloropallate, the concentration difference of silver nitrate, hydroquinone
For 0.1 mol/L, 0.0005 mol/L, 0.0005 mol/L, 0.0001 mol/L, 0.01 mol/L；In stirring condition
Under when solution colour becomes colorless clear solution by yellowish-brown, be added 0.4 milliliter of prefabricated gold nanoparticle seed colloid it is molten
Then liquid reacts it 1 hour in 50 degrees Celsius of baking ovens, obtain green rhotanium nanometer rods colloidal solution；With high speed from
Scheming is centrifuged after twenty minutes under the conditions of 14000 revs/min of revolving speed, removes colourless solution in centrifuge tube, obtains green precipitate production
Object；Green precipitate product is cleaned by ultrasonic 3-5 times with 18.2 megaohms of deionized waters, such as Fig. 2 a, Fig. 2 b, shown in Fig. 3 7.5 are made
× 26 nanometers of rhotanium nanometer rods；
Embodiment 2
Rhotanium nanometer rods are prepared in various concentration cetyl trimethylammonium bromide solution
4 parts of various concentration cetyl trimethylammonium bromide solutions are prepared, A, B, C, D are respectively labeled as, in stirring condition
It is lower 14.1,11.6,6.6,4.1 ml deionized waters are added separately to (A) 5, (B) 7.5, (C) 12.5, (D) rub for 15 milliliter 0.2
In that/liter cetyl trimethylammonium bromide solution, 0.1 milliliter of 0.1 mol/L gold chloride, 0.1 milliliter are then sequentially added
0.1 mol/L sodium tetrachloropallate, 0.02 milliliter of 0.1 mol/L silver nitrate aqueous solution, obtain brown solution after mixing evenly,
0.2 milliliter of 1 mol/L hydroquinone aqueous solution is then added, wherein the concentration of cetyl trimethylammonium bromide is respectively
(A) 0.05 mol/L, (B) 0.075 mol/L, (C) 0.125 mol/L, (D) 0.15 mol/L；Gold chloride, four in A-D
Chlorine palladium acid sodium, silver nitrate, hydroquinone concentration be 0.0005 mol/L, 0.0005 mol/L, 0.0001 mol/L,
0.01 mol/L；Under agitation when solution colour becomes colorless clear solution by yellowish-brown, 0.4 milliliter of addition is prefabricated
Gold nanoparticle seed colloidal solution, it is reacted 1 hour in 50 degrees Celsius of baking ovens then, obtains green rhotanium
Nanometer rods colloidal solution；It is centrifuged after twenty minutes, is removed in centrifuge tube under the conditions of 14000 revs/min of revolving speed with supercentrifuge
Colourless solution obtains green precipitate product；Green precipitate product is cleaned by ultrasonic 3-5 times with 18.2 megaohms of deionized waters, is made
The rhotanium nanometer rods of different scale as shown in Figure 6；
Embodiment 3
Rhotanium nanometer rods are prepared under gold chloride concentration different condition
By 36.4 ml deionized waters, 0.4 milliliter of 0.1 mol/L sodium tetrachloropallate, 0.08 milliliter of 0.1 mol/L nitric acid
Silver-colored aqueous solution is successively added under agitation in 40 milliliter of 0.2 mol/L cetyl trimethylammonium bromide solution, stirring
Brown solution is obtained after uniformly, wherein cetyl trimethylammonium bromide, sodium tetrachloropallate, the concentration of silver nitrate are respectively 0.1
Mol/L, 0.0005 mol/L, 0.0001 mol/L；The solution of above-mentioned preparation is divided into 4 parts, be respectively labeled as A, B,
C,D；It is then respectively adding not 0.1 mol/L aqueous solution of chloraurate of same amount, wherein 0.04 milliliter of (A), 0.06 milliliter of (B), (C)
0.08 milliliter, 0.1 milliliter of (D)；Then to being separately added into 0.2 milliliter of 1 mol/L hydroquinone aqueous solution in A-D；In stirring bar
Under part when solution colour becomes colorless clear solution by yellowish-brown, then 0.4 milliliter of prefabricated gold nano is added into A-D respectively
Then particle seed colloidal solution reacts it 1 hour in 50 degrees Celsius of baking ovens, obtain green rhotanium nanometer sticklac
Liquid solution；It is centrifuged after twenty minutes under the conditions of 14000 revs/min of revolving speed with supercentrifuge, removes colourless solution in centrifuge tube,
Obtain green precipitate product；Green precipitate product is cleaned by ultrasonic 3-5 times with 18.2 megaohms of deionized waters, is made as shown in Figure 7
Ingredient, rhotanium nanometer rods of different sizes；
Embodiment 4
Rhotanium nanometer rods are prepared under tetrachloro-palladium acid na concn different condition
By 36.4 ml deionized waters, 0.4 milliliter of 0.1 mol/L gold chloride, 0.08 milliliter of 0.1 mol/L silver nitrate water
Solution is successively added under agitation in 40 milliliter of 0.2 mol/L cetyl trimethylammonium bromide solution, stirs evenly
After obtain orange solution, wherein cetyl trimethylammonium bromide, gold chloride, silver nitrate concentration be respectively 0.1 mole/
Liter, 0.0005 mol/L, 0.0001 mol/L；The solution of above-mentioned preparation is divided into 4 parts, is respectively labeled as A, B, C, D；So
After be separately added into not 0.1 mol/L tetrachloro-palladium acid sodium water solution of same amount, wherein 0.02 milliliter of (A), 0.04 milliliter of (B), (C)
0.06 milliliter, 0.08 milliliter of (D)；Then to being separately added into 0.2 milliliter of 1 mol/L hydroquinone aqueous solution in A-D；It is stirring
Under the conditions of when solution colour becomes colorless clear solution by yellowish-brown, then respectively into A-D be added 0.4 milliliter of prefabricated Jenner
Then rice corpuscles seed colloidal solution reacts it 1 hour in 50 degrees Celsius of baking ovens, obtain green rhotanium nanometer rods
Colloidal solution；It is centrifuged after twenty minutes, is removed colourless molten in centrifuge tube under the conditions of 14000 revs/min of revolving speed with supercentrifuge
Liquid obtains green precipitate product；Green precipitate product is cleaned by ultrasonic 3-5 times with 18.2 megaohms of deionized waters, is made such as Fig. 8 institute
The ingredient that shows, rhotanium nanometer rods of different sizes；
Embodiment 5
Rhotanium nanometer rods are prepared as reducing agent with various concentration hydroquinone
By 36.4 ml deionized waters, 0.4 milliliter of 0.1 mol/L gold chloride, 0.4 milliliter of 0.1 mol/L tetrachloro-palladium acid
Sodium, 0.08 milliliter of 0.1 mol/L silver nitrate aqueous solution are successively added to 40 milliliter of 0.2 mol/L hexadecane under agitation
In base trimethylammonium bromide solution, brown solution is obtained, wherein cetyl trimethylammonium bromide, gold chloride, tetrachloro-palladium acid
Sodium, silver nitrate concentration be respectively 0.1 mol/L, 0.0005 mol/L, 0.0005 mol/L, 0.0001 mol/L；It will
The solution of above-mentioned preparation is divided into 6 parts, is respectively labeled as A, B, C, D, E, F；It is then added under agitation into A-F different
Measure 1 mol/L hydroquinone aqueous solution, wherein 0.08 milliliter of (A), 0.12 milliliter of (B), 0.16 milliliter of (C), 0.2 milliliter of (D),
(E) 0.24 milliliter, 0.28 milliliter of (F)；Add when solution colour becomes colorless clear solution by yellowish-brown, then respectively into A-F
Enter 0.4 milliliter of prefabricated gold nanoparticle seed colloidal solution, then react it 1 hour in 50 degrees Celsius of baking ovens, obtains
Green rhotanium nanometer rods colloidal solution；It is centrifuged after twenty minutes under the conditions of 14000 revs/min of revolving speed with supercentrifuge,
Colourless solution in centrifuge tube is removed, green precipitate product is obtained；It is clear to green precipitate product ultrasound with 18.2 megaohms of deionized waters
It washes 3-5 times, rhotanium nanometer rods of different sizes as shown in Figure 9 is made；
Embodiment 6
Rhotanium nanometer rods are prepared under different temperatures
By 36.4 ml deionized waters, 0.4 milliliter of 0.1 mol/L gold chloride, 0.4 milliliter of 0.1 mol/L tetrachloro-palladium acid
Sodium, 0.08 milliliter of 0.1 mol/L silver nitrate aqueous solution are successively added to 40 milliliter of 0.2 mol/L hexadecane under agitation
In base trimethylammonium bromide solution, brown solution is obtained after mixing evenly, and 0.8 milliliter of 1 mol/L hydroquinone is then added
Aqueous solution, wherein cetyl trimethylammonium bromide, gold chloride, sodium tetrachloropallate, the concentration difference of silver nitrate, hydroquinone
For 0.1 mol/L, 0.0005 mol/L, 0.0005 mol/L, 0.0001 mol/L, 0.01 mol/L；In stirring condition
Under when solution colour becomes colorless clear solution by yellowish-brown, the solution of above-mentioned preparation is divided into 4 parts, be respectively labeled as A,
B,C,D；0.4 milliliter of prefabricated gold nanoparticle seed colloidal solution is then added into A-D under agitation, then by A-
D, which is individually positioned in 40,50,60,70 degrees Celsius of baking ovens, to react 1 hour, obtains green rhotanium nanometer rods colloidal solution；
It is centrifuged after twenty minutes under the conditions of 14000 revs/min of revolving speed with supercentrifuge, removes colourless solution in centrifuge tube, obtain green
Color precipitated product；Green precipitate product is cleaned by ultrasonic 3-5 times with 18.2 megaohms of deionized waters, size as shown in Figure 10 is made
Different rhotanium nanometer rods.
Obviously, those skilled in the art can have excellent near-infrared absorption and photoelectrocatalysis to of the present invention
Rhotanium nanometer rods of performance and preparation method thereof carry out various modification and variations without departing from the spirit and scope of the present invention.
In this way, if these modifications and changes of the present invention is within the scope of the claims of the present invention and its equivalent technology, then originally
Invention is also intended to include these modifications and variations.
Claims (2)
1. a kind of rhotanium nanometer rods with excellent near-infrared absorption and PhotoelectrocatalytiPerformance Performance, it is characterized in that it is a kind of by
Two kinds of gold, palladium elements are constructed jointly and gold, palladium equally distributed rod-like nano particle inside particle.
2. a kind of rhotanium nanometer rods described in claim 1 with excellent near-infrared absorption and PhotoelectrocatalytiPerformance Performance
Preparation method, comprising the following steps:
(1) compound concentration is the achromaticity and clarification cetyl trimethylammonium bromide aqueous solution of 0.02-0.3 mol/L；
(2) aqueous solution of chloraurate is added to cetyl trimethylammonium bromide aqueous solution, sodium borohydride aqueous solution is then added,
Obtain 2-3 nanometers of gold nanoparticle seed colloidal solution, wherein gold chloride, sodium borohydride concentration be respectively 0.0001-
0.001 mol/L, 0.0001-0.001 mol/L；
(3) under agitation, gold chloride, sodium tetrachloropallate, silver nitrate, hydroquinone aqueous solution are successively added to hexadecane
In base trimethylammonium bromide aqueous solution, acquisition prepares the growth solution of rhotanium nanometer rods, wherein gold chloride, tetrachloro-palladium acid
Sodium, silver nitrate, hydroquinone concentration be respectively 0.00005-0.005 mol/L, 0.00005-0.005 mol/L,
0.00001-0.0005 mol/L, 0.005-0.05 mol/L；
(4) the gold nanoparticle seed colloidal solution that a certain amount of step (2) obtain is added to the growth solution of step (3) preparation
In, it is reacted 0.5-3 hours in 40-70 degrees Celsius of baking oven, obtains green rhotanium nanometer rods colloidal solution；
(5) rhotanium nanometer rods colloidal solution is centrifuged under the conditions of 10000-14500 revs/min of revolving speed with supercentrifuge,
Colourless solution in centrifuge tube is removed after 5-60 minutes, obtains green precipitate product；
(6) the green precipitate product obtained with 18.2 megaohms of deionized water ultrasonic cleaning is made the different gold-palladium of scale, ingredient and closes
Gold nanorods.
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| CN107824782B (en) * | 2017-10-31 | 2019-07-09 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of gold nanorods of top supported palladium and products thereof and application |
| US10758983B1 (en) | 2018-04-17 | 2020-09-01 | Government Of The United States, As Represented By The Secretary Of The Air Force | Concentrated synthesis of monodispersed gold nanorods |
| CN108637269B (en) * | 2018-04-25 | 2021-06-25 | 中国科学院合肥物质科学研究院 | Gold nano double pyramid with quintuple twin crystal structure and preparation method thereof |
| CN108896638B (en) * | 2018-07-10 | 2020-01-21 | 山东理工大学 | Preparation method and application of immunosensor based on titanium dioxide doped graphene loaded sea cucumber-like gold-palladium core-shell nanoparticles |
| CN108993597B (en) * | 2018-08-01 | 2020-05-12 | 中国科学技术大学 | Catalyst for alkyne hydrogenation reaction and preparation method thereof |
| CN109464664B (en) * | 2018-11-13 | 2021-07-20 | 南昌大学 | Preparation method of intelligent eye patch for relieving xerophthalmia symptoms |
| CN110153410B (en) * | 2019-06-06 | 2021-07-30 | 安徽师范大学 | Method for growing ordered Pd array rod-like nanoparticles on surface of Au triangular plate and application of ordered Pd array rod-like nanoparticles |
| CN110581281B (en) * | 2019-09-11 | 2021-11-02 | 江南大学 | PdCu alloy nano catalyst applied to fuel cell field and preparation method thereof |
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| CN112958084B (en) * | 2021-03-02 | 2022-10-25 | 山东大学 | Plasma photocatalytic material, preparation method and application in aniline preparation |
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| CN113730600B (en) * | 2021-08-24 | 2023-04-25 | 上海大学 | Palladium-gold alloy diagnosis and treatment integrated nano composite system, preparation method and application thereof |
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