CN107008895A - A kind of rhotanium nanometer rods with excellent near-infrared absorption and PhotoelectrocatalytiPerformance Performance and preparation method thereof - Google Patents
A kind of rhotanium nanometer rods with excellent near-infrared absorption and PhotoelectrocatalytiPerformance Performance and preparation method thereof Download PDFInfo
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- CN107008895A CN107008895A CN201710237281.6A CN201710237281A CN107008895A CN 107008895 A CN107008895 A CN 107008895A CN 201710237281 A CN201710237281 A CN 201710237281A CN 107008895 A CN107008895 A CN 107008895A
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- 238000010521 absorption reaction Methods 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000243 solution Substances 0.000 claims abstract description 79
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000007864 aqueous solution Substances 0.000 claims abstract description 32
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 27
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims abstract description 25
- 239000002253 acid Substances 0.000 claims abstract description 23
- KGYLMXMMQNTWEM-UHFFFAOYSA-J tetrachloropalladium Chemical compound Cl[Pd](Cl)(Cl)Cl KGYLMXMMQNTWEM-UHFFFAOYSA-J 0.000 claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 22
- 150000005208 1,4-dihydroxybenzenes Chemical class 0.000 claims abstract description 21
- 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
- 239000011734 sodium Substances 0.000 claims abstract description 21
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 21
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 20
- 238000013019 agitation Methods 0.000 claims abstract description 14
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 14
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 14
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 20
- 239000000047 product Substances 0.000 claims description 17
- 239000002105 nanoparticle Substances 0.000 claims description 16
- 239000003643 water by type 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 14
- 238000000034 method Methods 0.000 claims description 14
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 13
- 239000010931 gold Substances 0.000 claims description 10
- 229910052737 gold Inorganic materials 0.000 claims description 9
- 229910052763 palladium Inorganic materials 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 239000000084 colloidal system Substances 0.000 claims description 4
- 238000009826 distribution Methods 0.000 claims description 4
- 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
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 claims 2
- 150000001875 compounds Chemical class 0.000 claims 1
- 239000006185 dispersion Substances 0.000 claims 1
- 238000006555 catalytic reaction Methods 0.000 abstract description 7
- 230000009467 reduction Effects 0.000 abstract description 5
- 238000013007 heat curing 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
- 230000003197 catalytic effect Effects 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 11
- 238000003756 stirring Methods 0.000 description 11
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- 230000005540 biological transmission Effects 0.000 description 9
- 239000003054 catalyst Substances 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 7
- 238000005119 centrifugation Methods 0.000 description 6
- 239000002131 composite material Substances 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000003638 chemical reducing agent Substances 0.000 description 5
- 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 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 238000002484 cyclic voltammetry Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000005516 engineering process 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
- 230000008569 process Effects 0.000 description 3
- 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 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 230000031709 bromination Effects 0.000 description 2
- 238000005893 bromination reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000006193 liquid solution Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000003287 optical effect Effects 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
- XKZQKPRCPNGNFR-UHFFFAOYSA-N 2-(3-hydroxyphenyl)phenol Chemical compound OC1=CC=CC(C=2C(=CC=CC=2)O)=C1 XKZQKPRCPNGNFR-UHFFFAOYSA-N 0.000 description 1
- UXAMZEYKWGPDBI-UHFFFAOYSA-N C(CCCCCCCCCCCCCCC)Br(C)(C)C Chemical compound C(CCCCCCCCCCCCCCC)Br(C)(C)C UXAMZEYKWGPDBI-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000976924 Inca Species 0.000 description 1
- 235000000177 Indigofera tinctoria Nutrition 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000012696 Pd precursors Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 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
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 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
- 239000003814 drug Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000005611 electricity Effects 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
- 230000003760 hair shine Effects 0.000 description 1
- 238000000703 high-speed centrifugation Methods 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
- 238000005259 measurement Methods 0.000 description 1
- 230000001404 mediated effect Effects 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
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000009738 saturating Methods 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
- 238000010189 synthetic method Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000001392 ultraviolet--visible--near infrared spectroscopy 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 process is：（1）Golden nanometer particle seed is prepared in the cetyl trimethylammonium bromide aqueous solution using sodium borohydride reduction；（2）Under agitation, gold chloride, tetrachloro-palladium acid sodium, silver nitrate, the hydroquinones aqueous solution are added in the cetyl trimethylammonium bromide aqueous solution successively, acquisition prepares the growth solution of rhotanium nanometer rods；（3）A certain amount of golden nanometer particle seed colloidal solution is added to step（2）In the growth solution of preparation, reacted 0.5 3 hours at 40 70 degrees Celsius, obtain green rhotanium nanometer rods colloidal solution.The rhotanium nanometer rods with excellent near-infrared absorption and PhotoelectrocatalytiPerformance Performance that the present invention is obtained have important application value in terms of photocatalysis, electro-catalysis, opto-electronic device, information storage, near infrared light heat cure.
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 technology
Metal Palladium has very excellent catalytic performance, as important catalyst, in Industrial Catalysis, fuel cell, medicine
The fields such as thing 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 reduction catalyst particle size can effectively strengthen its catalytic activity.However, right
For catalyst, in addition to catalytic efficiency, another important performance is then its stability.Pure Pd nano particle was being used
The problems such as being prone to assemble in journey, dissolve, aoxidize, and then cause the reduction of its catalytic performance or even inactivate.With Pd nano particle
Compare, golden nanometer particle not only has good stability but also with unique surface plasmon absorption characteristic and life
Thing compatibility.Research shows, Pd nano particle deposition is coated on into the good Au nanoparticle sublists of chemical property torpescence, acid resistance
Face can effectively improve the catalytic activity of palladium with stably.Therefore, construct gold-palladium composite nanoparticle and cause people in recent years
Extensive concern.At present, the synthesis 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, and seed is made with the golden nanometer particle of different-shape, synthesized in aqueous bar-shaped, octahedra, cubic block,
Golden@palladiums nucleocapsid, the Heterogeneous Composite nano-particle 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 appropriate sodium citrate, hydrazine, sodium borohydride, L-AA are added in solution
Make reducing agent, spherical, flower-shaped, dendritic, starlike rhotanium, core-shell nano are successfully prepared using co-reducing process.However,
Although the gold-palladium composite nanoparticle that the above method is constructed effectively increases 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, it is common based on surface plasma
The noble metal that effect of shaking is constructed/semiconductor plasma photochemical catalyst has succeeded as the photochemical catalyst of the new photoresponse of a class
For all more important organic reactions such as catalytic alcohol oxidation, alkene epoxidation, nitro reduction, the coupling of carbon carbon, benzene hydroxylations, in profit
Huge application potential is shown with solar energy aspect.Obviously, organic collection alloy that acted synergistically between metal, two kinds of materials of palladium are passed through
Advantage, construct with catalysis and surface plasmon absorption multiple performance gold-palladium composite nanoparticle have it is important
Scientific meaning and actual application value.These characteristics will make it in surface plasma bulk optics, Industrial Catalysis, pharmaceutical synthesis, light
It is catalyzed in terms of organic synthesis, photo-thermal therapy with very wide application prospect.
The content of the invention
The problem to be solved in the present invention is to overcome the weak point of existing rhotanium nano-particle technology of preparing there is provided one
Plant simple, the efficient synthetic method for preparing rhotanium nanometer rods in aqueous.It is another object of the present invention to prepare
Different scale has the bar-shaped rhotanium nano-particle of excellent near-infrared absorption and PhotoelectrocatalytiPerformance Performance, is photocatalysis, electricity
Practical application provides material base in terms of catalysis, opto-electronic device, information storage, near infrared light heat cure.
The bar-shaped rhotanium nanometer in the present invention with near-infrared absorption and PhotoelectrocatalytiPerformance Performance is using seed life
Regular way is heated under ambiance containing gold chloride, tetrachloro-palladium acid sodium, cetyl trimethylammonium bromide, hydroquinones, a small amount of nitre
What the aqueous solution of sour silver and golden nanometer particle seed was obtained, including step in detail below：
（1）At ambient temperature, cetyl trimethylammonium bromide is added in the aqueous solution, concentration is obtained after stirring is
The achromaticity and clarification cetyl trimethylammonium bromide aqueous solution of 0.02-0.3 mol/Ls；
（2）It is prepared by golden nanometer particle seed：Aqueous solution of chloraurate is added to 1-15 milliliters of cetyl trimethylammonium bromide water
Solution, stirring rapidly joins sodium borohydride aqueous solution after 2 minutes, obtain the golden nanometer particle that yardstick is 2-3 nanometers, Celsius 35
Degree lower place makes residual sodium borohydride decompose completely for 1-5 hours, wherein, gold chloride, the concentration of sodium borohydride are respectively 0.0001-
0.001 mol/L, 0.0001-0.001 mol/Ls；
（3）Rhotanium nanorod growth solution is prepared：Gold chloride, tetrachloro-palladium acid sodium, a small amount of silver nitrate aqueous solution are added successively
It is added in the cetyl trimethylammonium bromide aqueous solution, brown solution is obtained after stirring, is subsequently added a certain amount of to benzene
The diphenol aqueous solution, solution colour is become colorless settled solution by yellowish-brown, and acquisition prepares the growth solution of rhotanium nanometer rods,
Wherein, cetyl trimethylammonium bromide, gold chloride, tetrachloro-palladium acid sodium, silver nitrate, the concentration of hydroquinones are respectively 0.02-
0.3 mol/L, 0.00005-0.005 mol/Ls, 0.00005-0.005 mol/Ls, 0.00001-0.0005 mol/Ls,
0.005-0.05 mol/Ls；
（4）By a certain amount of step（2）The golden nanometer particle seed colloidal solution of acquisition is added to step（3）The growth solution of preparation
In, reacted 0.5-3 hours in 40-70 degrees Celsius of baking oven, obtain green rhotanium nanometer rods colloidal solution；
（5）Rhotanium nanometer rods colloidal solution centrifuges 5- with supercentrifuge under the conditions of 10000-14500 revs/min of rotating speed
After 60 minutes, colourless solution in centrifuge tube is removed, green precipitate product is obtained；
（6）It is cleaned by ultrasonic the green precipitate product obtained with 18.2 megaohms of deionized waters, different scale is made, the gold-palladium of composition is closed
Gold nanorods.
Beneficial effects of the present invention：
（1）The invention provides a kind of method for preparing rhotanium nanometer rods, it is characterised in that rhotanium nanometer rods be
In the cetyl trimethylammonium bromide aqueous solution, reducing agent is made with hydroquinones, grown using chemical coreduction and Seed inducement
Prepared by the method being combined, its easy to operation, experimental repeatability is good；
（2）Rhotanium nanometer rods yield prepared by this method is high, size is homogeneous, yardstick is adjustable；
（3）Rhotanium nanometer rods colloid color prepared by this method is green, different from the other gold-palladium nanoparticles reported
Son, spectral measurement shows that rhotanium nanometer rods have excellent near-infrared absorption and PhotoelectrocatalytiPerformance Performance with electrochemistry experiment；
（4）Rhotanium nanometer rods yield prepared by this method is high, and the yardstick of particle, draw ratio can pass through cetyl trimethyl
The experiment parameter such as gold-palladium mol ratio, reaction time, seed addition is carried out in bromination ammonium concentration, hydroquinones concentration, presoma
Effective Regulation, and then obtain the rhotanium nanometer rods of different draw ratios；
（5）This method can prepare rhotanium nanometer rods, and gold in the different precursor solution of gold-palladium molar concentration rate
Palldium alloy nanometer rods composition, performance can pass through gold-palladium precursor concentration Effective Regulation；
（6）Gold-palladium conjunction can be prepared in the precursor solution that this method is under condition of different temperatures, gold-palladium molar concentration is different
Gold nanorods；
Brief description of the drawings
Fig. 1 is multiple optics shot after being visually observed to rhotanium nanometer rods preparation process every 10 minutes with camera
Photo, as a result shows, solution colour is by grey（10 minutes）By blueness（20 minutes）, Indigo（30 minutes）Ultimately become
Green（40-80 minutes）；
Fig. 2 is to obtained rhotanium nanometer rods with being shot after JEOL's JEOL-1400 transmission electron microscope observations
Multiple transmission electron microscope photos and particle size distribution, wherein, Fig. 2 a are rhotanium nanometer rods low power transmission electron microscope photo, Fig. 2 b
For rhotanium nanometer rods high power transmission electron microscope photo, Fig. 2 c are rhotanium nanorod diameter Size Distribution block diagram, Fig. 2 d
For rhotanium nanorod length Size Distribution block diagram.As can be seen that the average diameter of rhotanium nanometer rods is 7.5 nm
, average length is 26 nm, and draw ratio is about 3.5；
Fig. 3 is penetrated by the scanning transmission electron microscope photo of obtained rhotanium nanometer rods and with Inca. Oxford types X-
Line energy disperse spectroscopy carries out the X-ray energy spectrum diagram obtained after power spectrum test, as a result shows, the composition of the nanometer rods of acquisition includes gold, palladium
Two kinds of elements and it is uniformly distributed in particle, illustrates that obtained product is rhotanium nanometer rods；
Fig. 4 is to use Japan Shimadzu UV-3101PC types ultraviolet-visible-near infrared spectrometer（UV-Vis-NIR）To system
The rhotanium nanometer rods obtained carry out the optical absorption map of test acquisition, wherein, ordinate is absorption intensity, and abscissa is light wave
Wavelength.It can be seen that rhotanium nanometer rods have horizontal, longitudinal duplex surface plasma resonance absorption performance, its
In, horizontal plasma resonance absorption peak is located at 510 nm, and longitudinal plasma resonance absorption peak is in 710 nm and its absorption intensity is remote
More than horizontal plasma absorption, this shows that rhotanium nanometer rods have excellent near-infrared absorption performance；
Fig. 5 is the cyclic voltammetry curve with the Catalytic oxidation of ethanol measured by Shanghai Chen Hua 760D electrochemical workstations.Wherein, it is bent
Line a is that the gold-palladium ratio made from is 1:The circulation for the Catalytic oxidation of ethanol that 1 rhotanium nanometer rods are measured as catalyst
Volt-ampere curve, curve b is cyclic voltammetry curve of the commercialized palladium/carbon catalyst to Catalytic oxidation of ethanol, and curve c is with obtained
The cyclic voltammetry curve of Catalytic oxidation of ethanol that is measured as catalyst of gold nanorods, illustration is experimental result enlarged drawing, knot
Fruit shows that rhotanium nanometer rods show excellent catalytic activity in the catalysis oxidation of ethanol；
Under Fig. 6 is other experiment parameter permanence conditions, the obtained gold in various concentrations cetyl trimethylammonium bromide solution
The transmission electron microscope photo of palldium alloy nanometer rods, wherein, the concentration of cetyl trimethylammonium bromide is respectively：0.05 mol/L
（Fig. 6 a）, 0.075 mol/L（Fig. 6 b）, 0.125 mol/L（Fig. 6 c）, 0.15 mol/L（Fig. 6 d）, all scales are equal in figure
For 100 nanometers；
Under Fig. 7 is other experiment parameter permanence conditions, obtained rhotanium nanometer rods is saturating under gold chloride concentration different condition
Electromicroscopic photograph is penetrated, wherein, the concentration of gold chloride is respectively：0.0002 mol/L（Fig. 7 a）, 0.0003 mol/L（Fig. 7 b）、
0.0004 mol/L（Fig. 7 c）, 0.0005 mol/L（Fig. 7 d）, all scales are 100 nanometers in figure；
Under Fig. 8 is other experiment parameter permanence conditions, obtained rhotanium nanometer rods under tetrachloro-palladium acid na concn different condition
Transmission electron microscope photo, wherein, the concentration of tetrachloro-palladium acid sodium is respectively：0.0001 mol/L（Fig. 8 a）, 0.0002 mol/L
（Fig. 8 b）, 0.0003 mol/L（Fig. 8 c）, 0.0004 mol/L（Fig. 8 d）, all scales are 100 nanometers in figure；
Under Fig. 9 is other experiment parameter permanence conditions, rhotanium nanometer made from reducing agent is made with various concentrations hydroquinones
The transmission electron microscope photo of rod, wherein, the concentration of hydroquinones is respectively：0.004 mol/L（Fig. 9 a）, 0.006 mol/L（Figure
9b）, 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（Figure
9f）, all scales are 100 nanometers in figure；
Under Figure 10 is other experiment parameter permanence conditions, the transmission electron microscope of rhotanium nanometer rods made from differential responses temperature shines
Piece, wherein, reaction temperature is respectively 40 degrees Celsius（Figure 10 a）, 50 degrees Celsius（Figure 10 b）, 60 degrees Celsius（Figure 10 c）, it is 70 Celsius
Degree（Figure 10 d）, all scales are 100 nanometers in figure.
Embodiment
First from market buy the present invention use gold chloride, tetrachloro-palladium acid sodium, cetyl trimethylammonium bromide, to benzene two
Phenol, silver nitrate, sodium borohydride；Then gold chloride, tetrachloro-palladium acid sodium, cetyl trimethyl bromine are prepared with 18 megaohms of deionized waters
Change ammonium, hydroquinones, silver nitrate, wherein sodium borohydride aqueous solution, cetyl trimethylammonium bromide, gold chloride, tetrachloro-palladium acid
Sodium, silver nitrate, sodium borohydride, the concentration of aqueous solution of hydroquinones 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.
Golden nanometer particle 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 added to the cetyl bromination aqueous ammonium of 6 milliliter of 0.2 mol/L, stirring 2 successively under agitation
Sodium borohydride aqueous solution is rapidly joined under 1200 revs/min of rotating speeds after minute, solution colour is changed into dark brown from yellow rapidly, obtained
The gold nanoparticle colloid solution that yardstick is 2-3 nanometers is obtained, being placed under 35 degrees Celsius makes residual sodium borohydride decompose completely, its
In, gold chloride, the concentration of sodium borohydride are 0.0005 mol/L, golden nanometer particle place 1-5 hour it is interior with effect most
It is good.
Present disclosure is described in further detail with reference to specific implementation example, but the invention is not restricted to following
The specific examples enumerated.
Embodiment 1
It is prepared by 7.5 × 26 nanometers of rhotanium nanometer rods
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 is added to 10 milliliter of 0.2 mol/L cetyl successively under agitation
In trimethylammonium bromide solution, brown solution is obtained after stirring, 0.2 milliliter of 1 mol/L hydroquinones water is subsequently added
Solution, wherein, cetyl trimethylammonium bromide, gold chloride, tetrachloro-palladium acid sodium, silver nitrate, the concentration of hydroquinones are respectively
0.1 mol/L, 0.0005 mol/L, 0.0005 mol/L, 0.0001 mol/L, 0.01 mol/L；Under agitation
When solution colour becomes colorless settled solution by yellowish-brown, 0.4 milliliter of prefabricated golden nanometer particle seed colloidal solution is added,
Then it is reacted 1 hour in 50 degrees Celsius of baking ovens, obtains green rhotanium nanometer rods colloidal solution；Use high speed centrifugation
Machine after centrifugation 20 minutes, removes colourless solution in centrifuge tube, obtains green precipitate product under the conditions of 14000 revs/min of the rotating speed；
Green precipitate product is cleaned by ultrasonic 3-5 time with 18.2 megaohms of deionized waters, it is obtained as shown in Fig. 2 a, Fig. 2 b, Fig. 3 7.5 ×
26 nanometers of rhotanium nanometer rods；
Embodiment 2
Rhotanium nanometer rods are prepared in various concentrations cetyl trimethylammonium bromide solution
4 parts of various concentrations cetyl trimethylammonium bromide solutions are prepared, A, B, C, D is respectively labeled as, under agitation will
14.1st, 11.6,6.6,4.1 ml deionized waters be added separately to (A) 5, (B) 7.5, (C) 12.5, (D) 15 milliliter 0.2 mole/
Rise in cetyl trimethylammonium bromide solution, then sequentially add 0.1 milliliter of 0.1 mol/L gold chloride, rub for 0.1 milliliter 0.1
That/liter tetrachloro-palladium acid sodium, 0.02 milliliter of 0.1 mol/L silver nitrate aqueous solution, obtain brown solution, then after stirring
The 0.2 milliliter of 1 mol/L hydroquinones aqueous solution is 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, tetrachloro palladium in A-D
Sour sodium, silver nitrate, the concentration of hydroquinones are 0.0005 mol/L, 0.0005 mol/L, 0.0001 mol/L, 0.01
Mol/L；Under agitation when solution colour becomes colorless settled solution by yellowish-brown, 0.4 milliliter of prefabricated gold is added
Nano-particle seed colloidal solution, then reacts it 1 hour in 50 degrees Celsius of baking ovens, obtains green rhotanium nanometer
Sticklac liquid solution；After centrifugation 20 minutes, removed colourless in centrifuge tube under the conditions of 14000 revs/min of the rotating speed with supercentrifuge
Solution, obtains green precipitate product；Green precipitate product is cleaned by ultrasonic 3-5 times with 18.2 megaohms of deionized waters, such as Fig. 6 is made
The rhotanium nanometer rods of shown different scale；
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 tetrachloro-palladium acid sodium, 0.08 milliliter of 0.1 mol/L silver nitrate water
Solution is added in 40 milliliter of 0.2 mol/L cetyl trimethylammonium bromide solution successively under agitation, stirs
After obtain brown solution, wherein, cetyl trimethylammonium bromide, tetrachloro-palladium acid sodium, the concentration of silver nitrate are respectively 0.1 to rub
You/liter, 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；The not mol/L aqueous solution of chloraurate of same amount 0.1 is then respectively adding, wherein,（A）0.04 milliliter,（B）0.06 milliliter,（C）
0.08 milliliter,（D）0.1 milliliter；Then to being separately added into the 0.2 milliliter of 1 mol/L hydroquinones aqueous solution in A-D；In stirring bar
Under part when solution colour becomes colorless settled solution by yellowish-brown, then 0.4 milliliter of prefabricated gold nano is added into A-D respectively
Particle seed colloidal solution, then reacts it 1 hour in 50 degrees Celsius of baking ovens, obtains green rhotanium nanometer sticklac
Liquid solution；After centrifugation 20 minutes, colourless solution in centrifuge tube is removed under the conditions of 14000 revs/min of the rotating speed with supercentrifuge,
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
Composition, 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 aqueous solution
It is added to successively under agitation in 40 milliliter of 0.2 mol/L cetyl trimethylammonium bromide solution, is obtained after stirring
Orange solution, wherein, cetyl trimethylammonium bromide, gold chloride, the concentration of silver nitrate be respectively 0.1 mol/L,
0.0005 mol/L, 0.0001 mol/L；The solution of above-mentioned preparation is divided into 4 parts, A, B, C, D is respectively labeled as；Then
The not mol/L tetrachloro-palladium acid sodium water solution of same amount 0.1 is separately added into, wherein,（A）0.02 milliliter,（B）0.04 milliliter,（C）0.06
Milliliter,（D）0.08 milliliter；Then to being separately added into the 0.2 milliliter of 1 mol/L hydroquinones aqueous solution in A-D；In stirring condition
Under when solution colour becomes colorless settled solution by yellowish-brown, then respectively into A-D add 0.4 milliliter of prefabricated Jenner's grain of rice
Sub- seed colloidal solution, then reacts it 1 hour in 50 degrees Celsius of baking ovens, obtains green rhotanium nanometer rods colloid
Solution；With supercentrifuge after centrifugation 20 minutes, colourless solution in centrifuge tube is removed, is obtained under the conditions of 14000 revs/min of the rotating speed
To 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 8
Composition, rhotanium nanometer rods of different sizes；
Embodiment 5
With various concentrations hydroquinones rhotanium nanometer rods are prepared as reducing agent
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 is added to 40 milliliter of 0.2 mol/L cetyl successively under agitation
In trimethylammonium bromide solution, brown solution is obtained, wherein, cetyl trimethylammonium bromide, gold chloride, tetrachloro-palladium acid
Sodium, the concentration of silver nitrate are respectively 0.1 mol/L, 0.0005 mol/L, 0.0005 mol/L, 0.0001 mol/L；Will
The solution of above-mentioned preparation is divided into 6 parts, is respectively labeled as A, B, C, D, E, F；Difference is then added into A-F under agitation
The 1 mol/L hydroquinones aqueous solution is measured, wherein,（A）0.08 milliliter,（B）0.12 milliliter,（C）0.16 milliliter,（D）0.2 milliliter,
（E）0.24 milliliter,（F）0.28 milliliter；When solution colour becomes colorless settled solution by yellowish-brown, then respectively into A-F plus
Enter 0.4 milliliter of prefabricated golden nanometer particle seed colloidal solution, then react it 1 hour in 50 degrees Celsius of baking ovens, obtain
Green rhotanium nanometer rods colloidal solution；With supercentrifuge under the conditions of 14000 revs/min of the rotating speed after centrifugation 20 minutes,
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
Wash 3-5 times, rhotanium nanometer rods of different sizes as shown in Figure 9 are 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 is added to 40 milliliter of 0.2 mol/L cetyl successively under agitation
In trimethylammonium bromide solution, brown solution is obtained after stirring, 0.8 milliliter of 1 mol/L hydroquinones water is subsequently added
Solution, wherein, cetyl trimethylammonium bromide, gold chloride, tetrachloro-palladium acid sodium, silver nitrate, the concentration of hydroquinones are respectively
0.1 mol/L, 0.0005 mol/L, 0.0005 mol/L, 0.0001 mol/L, 0.01 mol/L；Under agitation
When solution colour becomes colorless settled 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 golden nanometer particle seed colloidal solution is then added into A-D under agitation, then by A-D
It is individually positioned in 40, reacts 1 hour in 50,60,70 degrees Celsius of baking ovens, obtains green rhotanium nanometer rods colloidal solution；With
Supercentrifuge after centrifugation 20 minutes, removes colourless solution in centrifuge tube, obtains green under the conditions of 14000 revs/min of the rotating speed
Precipitated product；Green precipitate product is cleaned by ultrasonic 3-5 times with 18.2 megaohms of deionized waters, obtained size as shown in Figure 10 is not
Same 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 changes and modification without departing from the spirit and scope of the present invention.
So, if these modifications and variations of the present invention belong within the scope of the claims in the present invention and its equivalent technologies, then originally
Invention is also intended to comprising including these changes and modification.
Claims (3)
1. a kind of rhotanium nanometer rods with excellent near-infrared absorption and PhotoelectrocatalytiPerformance Performance, it is characterized in that：
(1) the rhotanium nanometer rods described in are that one kind is constructed jointly by gold, two kinds of elements of palladium and gold, palladium are equal inside particle
The nano-particle of even distribution, its granular size is homogeneous, yardstick is adjustable, composition is easily-controllable, good dispersion；
（2）Rhotanium nanometer rods have excellent near-infrared absorption and PhotoelectrocatalytiPerformance Performance, and its colloid color is green.
2. a kind of rhotanium nanometer rods with excellent near-infrared absorption and PhotoelectrocatalytiPerformance Performance described in claim 1
Preparation method, comprises the following steps：
（1）Compound concentration is the achromaticity and clarification cetyl trimethylammonium bromide aqueous solution of 0.02-0.3 mol/Ls；
（2）Aqueous solution of chloraurate is added to the cetyl trimethylammonium bromide aqueous solution, sodium borohydride aqueous solution is subsequently added,
The golden nanometer particle seed colloidal solution of 2-3 nanometers of acquisition, wherein, gold chloride, the concentration of sodium borohydride are respectively 0.0001-
0.001 mol/L, 0.0001-0.001 mol/Ls；
（3）Under agitation, gold chloride, tetrachloro-palladium acid sodium, silver nitrate, the hydroquinones aqueous solution are added to hexadecane successively
In the base trimethylammonium bromide aqueous solution, acquisition prepares the growth solution of rhotanium nanometer rods, wherein, gold chloride, tetrachloro-palladium acid
Sodium, silver nitrate, the concentration of hydroquinones be respectively 0.00005-0.005 mol/Ls, 0.00005-0.005 mol/Ls,
0.00001-0.0005 mol/Ls, 0.005-0.05 mol/Ls；
（4）By a certain amount of step（2）The golden nanometer particle seed colloidal solution of acquisition is added to step（3）The growth solution of preparation
In, reacted 0.5-3 hours in 40-70 degrees Celsius of baking oven, obtain green rhotanium nanometer rods colloidal solution；
（5）Rhotanium nanometer rods colloidal solution is centrifuged under the conditions of 10000-14500 revs/min of rotating speed with supercentrifuge,
Colourless solution in centrifuge tube is removed after 5-60 minutes, green precipitate product is obtained；
（6）It is cleaned by ultrasonic the green precipitate product obtained with 18.2 megaohms of deionized waters, the different gold-palladium of yardstick, composition is made and closes
Gold nanorods.
3. preparation method described in claim 2, it is characterised in that rhotanium nanometer rods are to employ chemistry in aqueous altogether
Reduce to grow with Seed inducement and be combined method preparation, its easy to operation, experimental repeatability is good.
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