CN113828790A - Preparation method of gold and core-shell nanocrystal thereof - Google Patents
Preparation method of gold and core-shell nanocrystal thereof Download PDFInfo
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 239000010931 gold Substances 0.000 title claims abstract description 64
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 62
- 239000002159 nanocrystal Substances 0.000 title claims abstract description 44
- 239000011258 core-shell material Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- 239000002253 acid Substances 0.000 claims abstract description 22
- 239000002105 nanoparticle Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 8
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 5
- 239000002270 dispersing agent Substances 0.000 claims abstract description 5
- 239000002135 nanosheet Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 14
- 229910052708 sodium Inorganic materials 0.000 claims description 14
- 239000011734 sodium Substances 0.000 claims description 14
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 12
- 229910052700 potassium Inorganic materials 0.000 claims description 12
- 239000011591 potassium Substances 0.000 claims description 12
- CXWXQJXEFPUFDZ-UHFFFAOYSA-N tetralin Chemical compound C1=CC=C2CCCCC2=C1 CXWXQJXEFPUFDZ-UHFFFAOYSA-N 0.000 claims description 10
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 9
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 9
- KNKRKFALVUDBJE-UHFFFAOYSA-N 1,2-dichloropropane Chemical compound CC(Cl)CCl KNKRKFALVUDBJE-UHFFFAOYSA-N 0.000 claims description 6
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910000510 noble metal Inorganic materials 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- 230000007704 transition Effects 0.000 claims description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- 150000001412 amines Chemical class 0.000 claims description 3
- 229960005070 ascorbic acid Drugs 0.000 claims description 3
- 235000010323 ascorbic acid Nutrition 0.000 claims description 3
- 239000011668 ascorbic acid Substances 0.000 claims description 3
- 239000002055 nanoplate Substances 0.000 claims description 3
- GKFJEDWZQZKYHV-UHFFFAOYSA-N borane;2-methylpropan-2-amine Chemical compound B.CC(C)(C)N GKFJEDWZQZKYHV-UHFFFAOYSA-N 0.000 claims 1
- 238000003786 synthesis reaction Methods 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 229910052723 transition metal Inorganic materials 0.000 abstract description 5
- 150000003624 transition metals Chemical class 0.000 abstract description 4
- 150000002343 gold Chemical class 0.000 abstract description 3
- 238000003917 TEM image Methods 0.000 description 14
- 239000000243 solution Substances 0.000 description 9
- 238000000926 separation method Methods 0.000 description 7
- 238000005406 washing Methods 0.000 description 7
- 230000009467 reduction Effects 0.000 description 4
- PVYPHUYXKVVURH-UHFFFAOYSA-N boron;2-methylpropan-2-amine Chemical compound [B].CC(C)(C)N PVYPHUYXKVVURH-UHFFFAOYSA-N 0.000 description 3
- 239000002070 nanowire Substances 0.000 description 3
- 229910001020 Au alloy Inorganic materials 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 229910001252 Pd alloy Inorganic materials 0.000 description 2
- 238000001311 chemical methods and process Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000007172 homogeneous catalysis Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 229910002710 Au-Pd Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002109 crystal growth method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- -1 gold transition metal Chemical group 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
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- B22—CASTING; POWDER METALLURGY
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- 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
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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Abstract
The application discloses a preparation method of gold nanocrystals, which sequentially comprises the following steps: (1) mixing a reducing agent and a dispersing agent according to the volume ratio of 1-4:0.1-1 to prepare a reaction solution; (2) adding chloroauric acid with preset mass into the reaction liquid, and standing for reaction; when the concentration of the chloroauric acid is 0.1-1mol/L, generating zero-dimensional gold nanoparticles; when the concentration of the chloroauric acid is lower than 0.07mol/L, generating one-dimensional ultra-long gold nanowires; and when the concentration of the chloroauric acid is 0.08-0.09mol/L, generating the two-dimensional gold nanosheet. The method can synthesize a series of gold nanocrystals with different morphologies by only one-step synthesis, and has the characteristics of simple and convenient operation, high yield, easy repetition, systematicness and the like. The application also discloses a preparation method of the gold core-shell nanocrystals, which can be used for constructing novel transition metal nano building blocks on the basis of gold nanocrystals with various morphologies.
Description
Technical Field
The invention relates to the technical field of chemical synthesis of transition metal solutions, in particular to a preparation method of gold and core-shell nanocrystals thereof.
Background
High quality nanocrystals have been of great interest to researchers because of their unique optical, electronic, magnetic, etc. properties. The gold nanocrystals have potential application prospects in the fields of energy chemistry, biomedicine, food science and the like due to the unique properties of size effect, surface effect, high potential and the like. Therefore, the preparation of the gold nanocrystals with different sizes and morphologies has important research significance.
The method for synthesizing gold nanocrystals by a solution chemistry method comprises: white phosphorus reduction, sodium borohydride reduction, ultrasonic ethanol reduction, amine reduction, and the like. Sun et al first synthesized ultrafine, uniform and monodisperse gold nanocrystals (Nano Res,2008,1,229-234.) by a freezing-point low-temperature two-step injection method using chloroauric acid, oleylamine, tetralin and tert-butylamine-borane complex system. In addition, the gold/palladium alloy has great application value in the field of homogeneous catalysis. However, although researchers have controlled the synthesis of gold nanocrystals with different morphologies through various solution chemistry methods to serve their corresponding scientific experimental studies, controlling the synthesis of each desired class of gold nanocrystals has been challenging.
At present, the synthesis method of gold nanocrystals mainly focuses on a seed crystal two-step growth method, i.e., small-sized gold nanocrystals are synthesized first, centrifuged and then cleaned, and the gold nanocrystals are taken as seed crystals, and precursors of chloroauric acid, a reducing agent, a protective agent (a capping agent) and the like are continuously fed to continuously grow the nanocrystals with different morphologies. However, the two-step crystal growth method cannot flexibly control various shapes of the synthesized gold nanocrystals, and has poor repeatability. In contrast, in a one-step synthesis, all reactants are subjected to successive chemical reactions in a single reactor, which is simple, high in yield, easy to repeat and systematic, while avoiding tedious separations and intermediate purification. Thus, the one-step synthesis method can save time and resources, improve the efficiency of chemical reactions, and provide better chemical yield.
Disclosure of Invention
Therefore, the invention aims to provide a preparation method of gold and a core-shell nanocrystal thereof, so as to overcome the problems in the prior art. The technical scheme of the invention is realized as follows:
a preparation method of gold nanocrystals sequentially comprises the following steps:
(1) mixing a reducing agent and a dispersing agent according to the volume ratio of 1-4:0.1-1 to prepare a reaction solution;
(2) adding chloroauric acid with preset mass into the reaction liquid, and standing for reaction;
when the concentration of the chloroauric acid in the reaction solution is 0.1-1mol/L, generating zero-dimensional gold nanoparticles;
when the concentration of the chloroauric acid in the reaction solution is lower than 0.07mol/L, generating one-dimensional ultra-long gold nanowires;
and when the concentration of the chloroauric acid in the reaction solution is 0.08-0.09mol/L, generating the two-dimensional gold nanosheets.
The further technical scheme is that the dispersing agent comprises one or more of 1, 2-dichloropropane, hexane, tetrahydronaphthalene, chloroform, ethanol or acetone which are mixed in any proportion.
According to a further technical scheme, the reducing agent comprises one or more of long-chain amine, oleylamine, tert-butylamine-borane complex or ascorbic acid which are mixed in any proportion.
The further technical proposal is that the temperature of the standing reaction is 0-70 ℃ and the time is 1-24 h.
The further technical proposal is that the diameter of the zero-dimensional gold nano-particles is 5-20nm, the length of the one-dimensional super-long gold nano-wires is 1-15 mu m, and the length-diameter ratio of the two-dimensional gold nano-sheets is 1-5 mu m.
The further technical proposal is that the zero-dimensional gold nano-particles increase the reaction pressure and generate one-dimensional short gold nano-rods.
The further technical proposal is that the reaction pressure is 10-20 MPa.
The preparation method of the core-shell nanocrystal (namely the gold core-shell nanocrystal) of the gold nanocrystal comprises the step of mixing and reacting the one-dimensional ultra-long gold nanocrystal with a reducing agent and second and third transition series noble metal salts to generate the gold core-shell nanocrystal (namely the gold transition metal core-shell nanocrystal). The reaction process does not need to add protective gas, and has the advantages of low preparation cost, easy operation, repeatability and the like.
The second transition series noble metal salt and the third transition series noble metal salt are one of sodium chloropalladate, potassium chloropalladate, sodium chloroplatinate, potassium chloroplatinate, sodium chloroiridate, potassium chloroiridate, sodium chlororhodate, potassium chlororhodate, sodium chloroargentum, potassium chloroargentum, sodium chlororuthenate and potassium chlororuthenate.
Compared with the prior art, the invention has the beneficial effects that:
1. the preparation method of the gold nanocrystal provided by the invention can change the concentration of the chloroauric acid in the reaction liquid by presetting the chloroauric acid with different mass to be put into the reaction liquid, thereby controlling the appearance of the generated nanocrystal. Not only the operation is simple and convenient, but also the control on the appearance of the generated nanocrystalline is very flexible and easy to repeat.
2. The method can synthesize a series of gold nanocrystals with different morphologies by only one-step synthesis, has the characteristics of simple and convenient operation, high yield, easy repeatability, systematicness and the like, and has potential application prospects in the fields of photoelectrocatalysis, homogeneous catalysis and the like.
3. The preparation method of the core-shell nanocrystals of the gold nanocrystals provided by the invention can be used for constructing novel transition metal nano building blocks on the basis of the gold nanocrystals with various morphologies, and the advantages of transition metals are complemented to achieve the maximum synergistic effect.
4. The invention prepares a series of high-quality gold and core-shell nanocrystals thereof, and provides various options on the diversity of the target material.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only preferred embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without inventive exercise.
FIG. 1 is a TEM image of 5nm gold nanoparticles prepared in example 1;
FIG. 2 is a TEM image of 17nm gold nanoparticles prepared in example 2;
FIG. 3 is a TEM image of 11nm gold nanorods prepared in example 3;
FIG. 4 is a TEM image of ultrafine gold nanowires prepared in example 4;
FIG. 5 is a TEM image of the ultra-long gold nanowires prepared in example 5;
FIG. 6 is a TEM image of gold nanoplates prepared in example 6;
FIG. 7 is a TEM image of the ultra-long Au-Pd core-shell nanowire prepared in example 7.
Detailed Description
For clear and complete description of the technical solutions in the present invention, it is obvious that the inventor combines the embodiments to describe, but the following embodiments describe only some embodiments of the present invention, not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Preparing zero-dimensional 5nm gold nanoparticles: firstly, setting the temperature of a vortex oscillation reactor to be 8 ℃; secondly, dissolving 2mmol of chloroauric acid in 20mL of mixed solution (containing oleylamine, tetralin and tert-butylamine-borane complex), and placing the mixed solution on a vortex oscillation reactor for reaction for 1-2 h; finally, centrifugal separation and acetone washing are carried out to obtain the ultrafine gold nanoparticles with the particle size of 5nm, and the yield is 90 +/-5%. As shown in FIG. 1, FIG. 1 is a TEM image of 5nm gold nanoparticles prepared in example 1.
Example 2
Preparing zero-dimensional 12nm gold nanoparticles: dissolving 5mmol of chloroauric acid in 4mL of oleylamine and 1mL of 1, 2-dichloropropane, raising the reaction temperature to 50-70 ℃, standing for reaction for 8-24h, and obtaining gold nanoparticles with the particle size of 12nm through multiple centrifugal separation and acetone washing, wherein the yield is 95 +/-5%. As shown in FIG. 2, FIG. 2 is a TEM image of 12nm gold nanoparticles prepared in example 2.
Example 3:
preparing 11nm gold nano short rods: dissolving 11mmol of chloroauric acid in 20mL of oleylamine and 2mL of 1, 2-dichloropropane, raising the reaction temperature to 50-70 ℃, increasing the reaction pressure for 12 hours, and obtaining the 11nm gold nano short rod through multiple centrifugal separation and acetone washing, wherein the yield is 90 +/-5%. As shown in FIG. 3, FIG. 3 is a TEM image of 11nm gold nanorods prepared in example 3.
Example 4:
preparing one-dimensional superfine gold nanowires: dissolving 4mmol of chloroauric acid in 2 oleylamine and 2mL of hexane, raising the reaction temperature to 50-70 ℃, standing for reaction for 13 hours, and obtaining the superfine gold nanowires through multiple centrifugal separation and acetone washing, wherein the yield is 85 +/-5%. As shown in FIG. 4, FIG. 4 is a TEM image of the ultrafine gold nanowires prepared in example 4.
Example 5:
preparing one-dimensional ultra-long gold nanowires. Dissolving 0.3mmol of chloroauric acid in 4mL of oleylamine and 2mL of 1, 2-dichloropropane, raising the reaction temperature to 50-70 ℃, standing for reaction for 1-24h, and obtaining the ultra-long gold nano-wire with the yield of 95 +/-5% through multiple centrifugal separation and acetone washing. As shown in FIG. 5, FIG. 5 is a TEM image of the ultra-long gold nanowire prepared in example 5.
Example 6:
preparing two-dimensional gold nanoplates: dissolving 0.48mmol of chloroauric acid in 4mL of oleylamine and 2mL of 1, 2-dichloropropane, raising the reaction temperature to 50-70 ℃, standing for reaction for 10-17h, and obtaining the gold nanosheets with the yield of 80 +/-5% through multiple centrifugal separation and acetone washing. As shown in FIG. 6, FIG. 6 is a TEM image of the gold nanoplatelets prepared in example 6.
Example 7:
first, 1-20mg of gold nanowires, 0.L mL of ascorbic acid (0.01-0.5mmol/L) and 100. mu.L of sodium chloropalladate (mmol/L) were mixed uniformly and allowed to stand for 1-24 hours. And centrifugally separating and washing to obtain the ultralong gold/palladium alloy nanowire. If the concentration of the sodium chloropalladate is continuously increased, a thicker palladium layer can be epitaxially grown on the gold nanorods, and the yield is 90 +/-5%. As shown in fig. 7, fig. 7 is a TEM image of the ultra-long au/pd core-shell nanowire obtained in example 7.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. The preparation method of the gold nanocrystal is characterized by sequentially comprising the following steps of:
(1) mixing a reducing agent and a dispersing agent according to the volume ratio of 1-4:0.1-1 to prepare a reaction solution;
(2) adding chloroauric acid with preset mass into the reaction liquid, and standing for reaction;
when the concentration of the chloroauric acid in the reaction solution is 0.1-1mol/L, generating zero-dimensional gold nanoparticles;
when the concentration of the chloroauric acid in the reaction solution is lower than 0.07mol/L, generating one-dimensional ultra-long gold nanowires;
and when the concentration of the chloroauric acid in the reaction solution is 0.08-0.09mol/L, generating the two-dimensional gold nanosheets.
2. The method as claimed in claim 1, wherein the dispersant comprises one or more selected from 1, 2-dichloropropane, hexane, tetralin, chloroform, ethanol and acetone.
3. The method for preparing gold nanocrystals, as recited in claim 1, wherein the reducing agent comprises one or more of long chain amine, oleylamine, tert-butylamine borane complex, or ascorbic acid mixed at any ratio.
4. The method for preparing gold nanocrystals according to claim 1, wherein the temperature of the standing reaction is 0-70 ℃ and the time is 1-24 hours.
5. The method for preparing gold nanocrystals, as recited in claim 1, wherein the zero dimensional gold nanoparticles have a diameter of 5-20nm, the one-dimensional ultra-long gold nanowires have a length of 1-15 μm, and the aspect ratio of the two-dimensional gold nanoplates is 1-5 μm.
6. The method as claimed in claim 1, wherein the zero dimensional gold nanoparticles increase reaction pressure to form one dimensional short gold nanorods.
7. The method for preparing gold nanocrystals according to claim 6, wherein the reaction pressure is 10 to 20 MPa.
8. The method for preparing core-shell nanocrystals of gold nanocrystals according to claim 1 or 5, wherein the one-dimensional ultra-long gold nanowires are mixed with a reducing agent and a second and third transition noble metal salts to react to form the gold core-shell nanocrystals.
9. The method for preparing core-shell nanocrystals of gold nanocrystals, as recited in claim 8, wherein the second and third transition noble metal salts are one of sodium chloropalladate, potassium chloropalladate, sodium chloroplatinate, potassium chloroplatinate, sodium chloroiridate, potassium chloroiridate, sodium chlororhodate, potassium chlororhodate, sodium chloroargentum, potassium chloroargentum, sodium chlororuthenate, and potassium chlororuthenate.
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