CN105731370A - Large-area two-dimensional ordered gold nanoparticle array and preparation method thereof - Google Patents
Large-area two-dimensional ordered gold nanoparticle array and preparation method thereof Download PDFInfo
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- CN105731370A CN105731370A CN201610096649.7A CN201610096649A CN105731370A CN 105731370 A CN105731370 A CN 105731370A CN 201610096649 A CN201610096649 A CN 201610096649A CN 105731370 A CN105731370 A CN 105731370A
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- 239000010931 gold Substances 0.000 title claims abstract description 149
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 149
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 148
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 87
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 49
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000006185 dispersion Substances 0.000 claims abstract description 23
- 239000002356 single layer Substances 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 239000012528 membrane Substances 0.000 claims abstract description 12
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 22
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 17
- 239000000758 substrate Substances 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- NJSSICCENMLTKO-HRCBOCMUSA-N [(1r,2s,4r,5r)-3-hydroxy-4-(4-methylphenyl)sulfonyloxy-6,8-dioxabicyclo[3.2.1]octan-2-yl] 4-methylbenzenesulfonate Chemical compound C1=CC(C)=CC=C1S(=O)(=O)O[C@H]1C(O)[C@@H](OS(=O)(=O)C=2C=CC(C)=CC=2)[C@@H]2OC[C@H]1O2 NJSSICCENMLTKO-HRCBOCMUSA-N 0.000 claims description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 8
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims description 8
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 8
- -1 polydimethylsiloxane Polymers 0.000 claims description 8
- 239000010453 quartz Substances 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000003921 oil Substances 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000012141 concentrate Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- SJUCACGNNJFHLB-UHFFFAOYSA-N O=C1N[ClH](=O)NC2=C1NC(=O)N2 Chemical compound O=C1N[ClH](=O)NC2=C1NC(=O)N2 SJUCACGNNJFHLB-UHFFFAOYSA-N 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000000243 solution Substances 0.000 description 8
- 238000001878 scanning electron micrograph Methods 0.000 description 7
- VQLYBLABXAHUDN-UHFFFAOYSA-N bis(4-fluorophenyl)-methyl-(1,2,4-triazol-1-ylmethyl)silane;methyl n-(1h-benzimidazol-2-yl)carbamate Chemical compound C1=CC=C2NC(NC(=O)OC)=NC2=C1.C=1C=C(F)C=CC=1[Si](C=1C=CC(F)=CC=1)(C)CN1C=NC=N1 VQLYBLABXAHUDN-UHFFFAOYSA-N 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000012295 chemical reaction liquid Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- KTUQUZJOVNIKNZ-UHFFFAOYSA-N butan-1-ol;hydrate Chemical compound O.CCCCO KTUQUZJOVNIKNZ-UHFFFAOYSA-N 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910003771 Gold(I) chloride Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 150000002343 gold Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 description 1
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
- B82B3/0004—Apparatus specially adapted for the manufacture or treatment of nanostructural devices or systems or methods for manufacturing the same
-
- 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
Abstract
The invention discloses a large-area two-dimensional ordered gold nanoparticle array and a preparation method thereof. The two-dimensional ordered gold nanoparticle array is a large-area single-layer membrane structure formed by orderly arranging multiple spherical gold nanoparticles according to an inerratic hexagonal close-packed structure, and the overall area of the two-dimensional ordered gold nanoparticle array is at least 1 cm<2>. The preparation method of the two-dimensional ordered gold nanoparticle array comprises the steps that the spherical gold nanoparticles are dispersed in absolute ethyl alcohol and then evenly mixed with n-butyl alcohol, and n-butyl alcohol dispersion liquid of the gold nanoparticles is obtained; the n-butyl alcohol dispersion liquid of the gold nanoparticles is dropwise added to the water surface in a vessel along the vessel wall till the water surface is paved with a single layer of the gold nanoparticles; standing of the vessel is conducted till n-butyl alcohol is completely volatilized, absolute ethyl alcohol is continuously and dropwise added to the water surface along the vessel wall till the gold nanoparticles on the water surface are concentrated in one place, and therefore the large-area two-dimensional ordered gold nanoparticle array is obtained. The large-area two-dimensional ordered gold nanoparticle array not only has the centimeter-sized large-area single-layer membrane structure, but also is high in stability, simple in preparation technology, easy to operate, low in cost and very suitable for industrial batched production.
Description
Technical field
The present invention relates to gold nano-material field, particularly relate to a kind of large-area sequential 2 D gold nano grain array and preparation method thereof.
Background technology
Gold nano grain has higher molar absorption coefficient and good biocompatibility, therefore has broad application prospects in fields such as catalysis, senser element, opto-electronic device, biotechnology, biomedicines.Along with the development of gold nano grain technology of preparing is with ripe, high-volume gold nano grain miscellaneous is constantly developed and research；But how to make optimization, functionalization and device that these gold nano grains realize in performance be always up major issue urgently to be resolved hurrily.
Self-assembling technique provides a kind of practicable new way for being directly integrated by assembling primitive for functionalized nano material；Compared with traditional " from top to bottom " preparation technology, self-assembling technique has instrument and equipment simple to operation, need not be expensive, the plurality of advantages such as with low cost.The two dimensional structure array assembled by gold nano grain, strong surface plasmon resonance local fields coupling can be there is between its nano-particle and nano-particle, peripheral electromagnetic field is made to be greatly enhanced, thus showing the physical property different from single gold nano grain and chemical property, this makes sequential 2 D gold nano grain array have broad application prospects in fields such as surface enhanced raman spectroscopy, biosensor, photocatalysis, photoelectric devices.And in existing technology, self-assembling technique is adopted to be typically only capable to prepare micron or the orderly gold nano grain array of millimetre-sized little area two-dimensional, Centimeter Level or greater levels of large-area sequential 2 D gold nano grain array cannot be prepared, and the sequential 2 D gold nano grain array stability that existing self-assembling technique is prepared is poor.
Summary of the invention
In order to solve that existing self-assembling technique can only be prepared the orderly gold nano grain array of little area two-dimensional, and prepared sequential 2 D gold nano grain array stablizes poor technical problem, the invention provides a kind of large-area sequential 2 D gold nano grain array and preparation method thereof, not only there is the large area single-layer membrane structure of square centimeter level, and stability is high, preparation technology is simple, easily operation, with low cost, be very suitable for industrialized mass production.
It is an object of the invention to be achieved through the following technical solutions:
A kind of large-area sequential 2 D gold nano grain array, it is to be at least 1cm by multiple spherical gold nano grains according to the entire area of the rule structurally ordered arrangement of Hexagonal Close-packed2Large area single-layer membrane structure.
Preferably, this sequential 2 D gold nano grain array can shift between silicon base, quartz substrate, polydimethylsiloxane substrate.
A kind of preparation method of large-area sequential 2 D gold nano grain array, including:
Step A, spherical gold nano grain is scattered in dehydrated alcohol, then mixes with n-butyl alcohol, and be uniformly dispersed, thus preparing the n-butyl alcohol dispersion liquid of gold nano grain；Wherein, the consumption of n-butyl alcohol is at least 20 times of dehydrated alcohol consumption；
Step B, it is at least 25cm in water surface area2Water container in, the n-butyl alcohol dispersion liquid of described gold nano grain is dropwise dripped on the water surface in this container along the chamber wall of this container, until the water surface is paved with single layer of gold nano-particle；
Step C, through step B process after, described container is stood, until the n-butyl alcohol in described container volatilizees completely；Continue to drip on the water surface in this container along the chamber wall of described container by dehydrated alcohol again, until the gold nano grain on the water surface concentrates at a place, thus preparing large-area sequential 2 D gold nano grain array described in technique scheme.
Preferably, in stepb, in described container the area of the water surface more than 1cm2。
Preferably, in step, if spherical gold nano grain is the aqueous dispersions adopting spherical gold nano grain, then this spherical gold nano grain first carries out centrifugal treating, and redispersion is in dehydrated alcohol.
Preferably, the aqueous dispersions of described spherical gold nano grain adopts following methods to prepare: join in ethylene glycol solution by gold chloride, diallyl dimethyl ammoniumchloride, hydrochloric acid, and stir, adopt oil bath to be heated to 195 DEG C again to react 30 minutes, being then added in chlorauric acid solution row wet-chemical chamber prepares spherical gold nano particle colloidal sols, finally described spherical gold nano particle colloidal sols is washed, thus preparing the aqueous dispersions of spherical gold nano grain.
As seen from the above technical solution provided by the invention, large-area sequential 2 D gold nano grain array that the embodiment of the present invention provides and preparation method thereof first passes through the gold nano grain that on the self-assembling method water surface in container, confluent monolayers is sparse, again dehydrated alcohol is continued dropping on the water surface in this container along chamber wall, so that the gold nano grain on the water surface under the promotion of dehydrated alcohol to drawing close assembly together, when distance between gold nano grain sufficiently closes to, these gold nano grains can under the mastery reaction of Van der Waals for, stably float on the water surface, thus being the formation of according to the rule structurally ordered arrangement of Hexagonal Close-packed, and entire area is at least 1cm2, present the orderly gold nano grain array of large-area two-dimensional of bright golden colour lustre.As can be seen here, the present invention not only has the large area single-layer membrane structure of Centimeter Level, and stability is high, and preparation technology is simple, easily operation, with low cost, is very suitable for industrialized mass production.
Accompanying drawing explanation
In order to be illustrated more clearly that the technical scheme of the embodiment of the present invention, below the accompanying drawing used required during embodiment is described is briefly described, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the premise not paying creative work, it is also possible to obtain other accompanying drawings according to these accompanying drawings.
Fig. 1 adopts Sirion200 field emission scanning electron microscope that the large-area sequential 2 D gold nano grain array prepared by the embodiment of the present invention 1 is shot the vertical view low power electron scanning micrograph obtained.
Fig. 2 adopts Sirion200 field emission scanning electron microscope that the large-area sequential 2 D gold nano grain array prepared by the embodiment of the present invention 1 shoots the vertical view high power electron scanning electron micrograph obtained.
Fig. 3 adopts Sirion200 field emission scanning electron microscope that the large-area sequential 2 D gold nano grain array prepared by the embodiment of the present invention 1 is shot the stravismus low power electron scanning micrograph obtained.
Fig. 4 adopts Sirion200 field emission scanning electron microscope that the large-area sequential 2 D gold nano grain array prepared by the embodiment of the present invention 1 is shot the stravismus high power electron scanning micrograph obtained.
Fig. 5 is that the large-area sequential 2 D gold nano grain array prepared by the embodiment of the present invention 1 is respectively at the suprabasil comparison diagram in kind of the water surface, silicon base, quartz substrate and polydimethylsiloxane.
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.Based on embodiments of the invention, the every other embodiment that those of ordinary skill in the art obtain under not paying creative work premise, broadly fall into protection scope of the present invention.
Below large-area sequential 2 D gold nano grain array provided by the invention and preparation method thereof is described.
(1) a kind of large-area sequential 2 D gold nano grain array
A kind of large-area sequential 2 D gold nano grain array, it is to be at least 1cm by multiple spherical gold nano grains according to the entire area of the rule structurally ordered arrangement of Hexagonal Close-packed2Large area single-layer membrane structure, present beautiful gold lustre, and can shift in existing various substrates, for instance: silicon base, quartz substrate, polydimethylsiloxane substrate etc..
(1) a kind of large-area sequential 2 D gold nano grain array
The preparation method of a kind of large-area sequential 2 D gold nano grain array, it is possible to comprise the following steps:
Step A, obtain spherical gold nano grain, and spherical gold nano grain is scattered in dehydrated alcohol, then mix with n-butyl alcohol, and be uniformly dispersed, thus preparing the n-butyl alcohol dispersion liquid of gold nano grain.
Wherein, the used in amounts of dehydrated alcohol ensures that each spherical gold nano grain Monodispersed obtained is in dehydrated alcohol, and the consumption of n-butyl alcohol is at least 20 times of dehydrated alcohol consumption；Dehydrated alcohol and n-butyl alcohol are liquid, and therefore in this step, the consumption of dehydrated alcohol and the consumption of n-butyl alcohol each mean volume.Dispersion processes can adopt ultrasonic disperse of the prior art.
Specifically, described spherical gold nano grain can adopt the spherical gold nano grain that any method in prior art prepares, it would however also be possible to employ scattered spherical gold nano grain in any form in prior art；If but spherical gold nano grain is the aqueous dispersions adopting spherical gold nano grain, then this spherical gold nano grain needs first to carry out centrifugal treating, and to remove moisture, redispersion is in dehydrated alcohol.In actual applications, the aqueous dispersions of described spherical gold nano grain can adopt following methods to prepare: by gold chloride, diallyl dimethyl ammoniumchloride, hydrochloric acid joins in ethylene glycol solution, and stir, adopt oil bath to be heated to 195 DEG C again to react 30 minutes, it is then added in chlorauric acid solution to carry out wet-chemical chamber prepare spherical gold nano particle colloidal sols, finally described spherical gold nano particle colloidal sols is performed twice at washing, to remove remaining ethylene glycol and diallyl dimethyl ammoniumchloride in colloidal sol, thus can be prepared by the aqueous dispersions of spherical gold nano grain.
Step B, it is at least 25cm in water surface area2Water container in, the n-butyl alcohol dispersion liquid of described gold nano grain is dropwise dripped on the water surface in this container along the chamber wall of this container, until the water surface is paved with single layer of gold nano-particle.
Wherein, described container can be various water container of the prior art (such as: beaker), but in container, the area of the water surface needs more than 25cm2, so just can prepare area and be at least 1cm2The orderly gold nano grain array of large-area two-dimensional.
Specifically, when the n-butyl alcohol dispersion liquid of described gold nano grain is dropwise dripped on the water surface in this container along the chamber wall of this container, drop can be sprawled rapidly on the water surface, the water surface can be formed interim n-butanol-water duplicature, owing to n-butyl alcohol can quickly volatilize and dissolve each other with water, therefore this n-butanol-water duplicature can become thin gradually along dispersal direction, this makes gold nano grain constantly can accumulate at thin place, and stably floats on the water surface under the capillary effect of liquid-vapor interface；Along with gold nano grain constantly accumulates on the water surface, gold nano grain under the interaction of dipole-dipole coupling and electrostatic repulsion, can assemble and form straight chain or linear chain structure；When being paved with single layer of gold nano-particle on the water surface, the water surface presenting the gold lustre of dimness, gold nano grain is random and loosely swims on the water surface.
Step C, through step B process after, described container is stood, until the n-butyl alcohol in described container volatilizees completely；Continue to drip on the water surface in this container along the chamber wall of described container by dehydrated alcohol again, until the gold nano grain on the water surface concentrates at a place, thus can be prepared by being at least 1cm according to the rule structurally ordered arrangement of Hexagonal Close-packed and entire area2The orderly gold nano grain array of large-area two-dimensional.
Wherein, tool is according to the quantity of n-butyl alcohol in described container, it is possible to select time of repose neatly, and the n-butyl alcohol that only need to ensure in described container volatilizees completely, for instance: can select under normal circumstances to stand 12 hours.
Specifically, when continuing to drip on the water surface in this container along the chamber wall of described container by dehydrated alcohol, ethanol drop can launch rapidly on the water surface, and an interfacial tension gradient difference is produced at air liquid interface place, and gold nano grain is assembled to a place under the effect of interfacial tension gradient difference, and re-assembly the single layer of gold nano-grain array (i.e. single-layer membrane structure macroscopically) forming dense regular, and present bright golden colour lustre；When distance between gold nano grain sufficiently closes to, the gold nano grain array of this dense regular under the mastery reaction of Van der Waals for, stably can float on the water surface, and can stably shift in existing various substrates.Such as: this sequential 2 D gold nano grain array can be transferred in silicon base, quartz substrate, soft polydimethylsiloxane substrate.
As fully visible, the embodiment of the present invention not only has the large area single-layer membrane structure of Centimeter Level, and stability is high, and preparation technology is simple, easily operation, with low cost, is very suitable for industrialized mass production.
In order to more clearly from show technical scheme provided by the present invention and produced technique effect, large-area sequential 2 D gold nano grain array with specific embodiment, the embodiment of the present invention provided below and preparation method thereof is described in detail.
Embodiment 1
A kind of preparation method of large-area sequential 2 D gold nano grain array, (purity is 99.9% to adopt gold chloride commercially, Sigma's reagent), (molal weight is 100000～200000 to diallyl dimethyl ammoniumchloride, 20wt% aqueous solution, Sigma's reagent), dehydrated alcohol (purity is more than 99.7%), hydrochloric acid solution (concentration is 37%, Sigma's reagent), ethylene glycol (ACS reagent) is raw material；It specifically may comprise steps of:
Step a, take gold chloride as gold presoma, take diallyl dimethyl ammoniumchloride as surfactant, gold chloride, diallyl dimethyl ammoniumchloride, hydrochloric acid joined in ethylene glycol solution, and stirs, thus prepare gold reaction liquid；In this gold reaction liquid, AuCl4-The concentration of the concentration hydrochloric acid of the concentration diallyl dimethyl ammoniumchloride of ion=0.5mM 25mM 5mM.Being placed in by described gold reaction liquid in oil bath and adopt oil bath heating to react 30 minutes to 195 DEG C, do not carry out any stirring during this, obtain presenting the colloidal sol that light wine is red after reaction, this illustrates to have generated octahedra gold nano grain in colloidal sol；Then the colloidal sol that light wine is red adds gold chloride (concentration of gold chloride is 0.0125mM) to described presenting, react two minutes, to remove Pedicellus et Pericarpium Trapae limit on octahedra gold nano grain and drift angle, thus preparing the spherical gold nano particle colloidal sols of redness.Described spherical gold nano particle colloidal sols is performed twice at washing, to remove remaining ethylene glycol and diallyl dimethyl ammoniumchloride in colloidal sol, thus can be prepared by the aqueous dispersions of spherical gold nano grain.
Step b, take the aqueous dispersions of spherical gold nano grain described in 10～20mL, and carry out centrifugal treating (centrifugal treating speed is 14500 revs/min, and the centrifugal treating time is 45 minutes)；Spherical gold nano grain good for centrifugal treating is scattered in 50 μ L dehydrated alcohol, then mixes with 1mL n-butyl alcohol, and ultrasonic disperse 15 minutes, thus preparing the n-butyl alcohol dispersion liquid of finely dispersed gold nano grain.
Step c, in the beaker filling water, the n-butyl alcohol dispersion liquid of described gold nano grain is dropwise dripped on the water surface in beaker along the wall of cup of this beaker, until the water surface is paved with single layer of gold nano-particle.
Step d, through step c process after, by described beaker stand 12 hours, the n-butyl alcohol in described beaker volatilizees completely；Again 5mL dehydrated alcohol is dropwise dripped on the water surface in beaker along the wall of cup of this beaker, until the gold nano grain on the water surface concentrates at a place, thus can be prepared by being at least 1cm according to the rule structurally ordered arrangement of Hexagonal Close-packed and entire area2The orderly gold nano grain array of large-area two-dimensional.
Further, the large-area sequential 2 D gold nano grain array prepared by the embodiment of the present invention 1 carrying out pattern and performance detection, its concrete testing result is as follows:
(1) adopt naked eyes that the sequential 2 D gold nano grain array prepared of step d in beaker in the embodiment of the present invention 1 is observed, again the sequential 2 D gold nano grain array that step d prepares is transferred in the polydimethylsiloxane substrate of silicon base, quartz substrate and softness respectively, thus the material object contrast photo that shooting is as shown in Figure 5；Wherein, Fig. 5 a is sequential 2 D gold nano grain array photo in kind on the water surface in beaker that in the embodiment of the present invention 1, step d prepares, Fig. 5 b is the sequential 2 D gold nano grain array photo in kind on a quartz substrate that in the embodiment of the present invention 1, step d prepares, Fig. 5 c be sequential 2 D gold nano grain array that in the embodiment of the present invention 1, step d prepares at the suprabasil photo in kind of polydimethylsiloxane, Fig. 5 d is sequential 2 D gold nano grain array that in the embodiment of the present invention 1, step d prepares photo in kind on a silicon substrate.As seen from Figure 5: the sequential 2 D gold nano grain array that in the embodiment of the present invention 1, in beaker, step d prepares is that entire area is at least 1cm2Large area single-layer membrane structure, and present beautiful gold lustre, this sequential 2 D gold nano grain array can be transferred in silicon base, quartz substrate, soft polydimethylsiloxane substrate simultaneously.
(2) adopt Sirion200 field emission scanning electron microscope that the large-area sequential 2 D gold nano grain array prepared by step d in the embodiment of the present invention 1 is observed, and shoot electron scanning micrograph (SEM image) as shown in Figure 1, Figure 2, Figure 3 and Figure 4；Wherein, Fig. 1 is the vertical view low power SEM image of the large-area sequential 2 D gold nano grain array prepared by the embodiment of the present invention 1, Fig. 2 is the vertical view high power SEM image of the large-area sequential 2 D gold nano grain array prepared by the embodiment of the present invention 1, Fig. 3 is the stravismus low power SEM image of the large-area sequential 2 D gold nano grain array prepared by the embodiment of the present invention 1, and Fig. 4 is the stravismus high power SEM image of the large-area sequential 2 D gold nano grain array prepared by the embodiment of the present invention 1.SEM image shown in Fig. 1 to Fig. 4 it can be seen that in the embodiment of the present invention 1 the sequential 2 D gold nano grain array prepared by step d formed according to the rule structurally ordered arrangement of Hexagonal Close-packed by multiple spherical gold nano grains, and this sequential 2 D gold nano grain array is that entire area is at least 1cm2Large area single-layer membrane structure.
As fully visible, the embodiment of the present invention not only has the large area single-layer membrane structure of Centimeter Level, and stability is high, and preparation technology is simple, easily operation, with low cost, is very suitable for industrialized mass production.
The above; being only the present invention preferably detailed description of the invention, but protection scope of the present invention is not limited thereto, any those familiar with the art is in the technical scope that the invention discloses; the change that can readily occur in or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (6)
1. a large-area sequential 2 D gold nano grain array, it is characterised in that it is to be at least 1cm by multiple spherical gold nano grains according to the entire area of the rule structurally ordered arrangement of Hexagonal Close-packed2Large area single-layer membrane structure.
2. large-area sequential 2 D gold nano grain array according to claim 1, it is characterised in that this sequential 2 D gold nano grain array can shift between silicon base, quartz substrate, polydimethylsiloxane substrate.
3. the preparation method of a large-area sequential 2 D gold nano grain array, it is characterised in that including:
Step A, spherical gold nano grain is scattered in dehydrated alcohol, then mixes with n-butyl alcohol, and be uniformly dispersed, thus preparing the n-butyl alcohol dispersion liquid of gold nano grain；Wherein, the consumption of n-butyl alcohol is at least 20 times of dehydrated alcohol consumption；
Step B, it is at least 25cm in water surface area2Water container in, the n-butyl alcohol dispersion liquid of described gold nano grain is dropwise dripped on the water surface in this container along the chamber wall of this container, until the water surface is paved with single layer of gold nano-particle；
Step C, through step B process after, described container is stood, until the n-butyl alcohol in described container volatilizees completely；Continue to drip on the water surface in this container along the chamber wall of described container by dehydrated alcohol again, until the gold nano grain on the water surface concentrates at a place, thus preparing the large-area sequential 2 D gold nano grain array as according to any one of claim 1 to 2.
4. preparation method according to claim 3, it is characterised in that in stepb, in described container, the area of the water surface is more than 1cm2。
5. the preparation method according to claim 3 or 4, it is characterised in that in step, if spherical gold nano grain is the aqueous dispersions adopting spherical gold nano grain, then this spherical gold nano grain first carries out centrifugal treating, and redispersion is in dehydrated alcohol.
6. preparation method according to claim 5, it is characterized in that, the aqueous dispersions of described spherical gold nano grain adopts following methods to prepare: join in ethylene glycol solution by gold chloride, diallyl dimethyl ammoniumchloride, hydrochloric acid, and stir, adopt oil bath to be heated to 195 DEG C again to react 30 minutes, being then added in chlorauric acid solution row wet-chemical chamber prepares spherical gold nano particle colloidal sols, finally described spherical gold nano particle colloidal sols is washed, thus preparing the aqueous dispersions of spherical gold nano grain.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610096649.7A CN105731370B (en) | 2016-02-22 | 2016-02-22 | A kind of sequential 2 D gold nano grain array of large area and preparation method thereof |
Applications Claiming Priority (1)
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| CN106958006A (en) * | 2017-04-10 | 2017-07-18 | 江西科技师范大学 | Multicomponent alloy not close arranges the preparation method of spherical nanoparticle array |
| CN108982464A (en) * | 2018-04-17 | 2018-12-11 | 中国科学院合肥物质科学研究院 | A kind of high distribution density nano gap oldered array and the preparation method and application thereof |
| CN114603152A (en) * | 2022-01-25 | 2022-06-10 | 广东食品药品职业学院 | Preparation method of gold nanoparticle monomolecular film layer structure |
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| CN106958006A (en) * | 2017-04-10 | 2017-07-18 | 江西科技师范大学 | Multicomponent alloy not close arranges the preparation method of spherical nanoparticle array |
| CN108982464A (en) * | 2018-04-17 | 2018-12-11 | 中国科学院合肥物质科学研究院 | A kind of high distribution density nano gap oldered array and the preparation method and application thereof |
| CN114603152A (en) * | 2022-01-25 | 2022-06-10 | 广东食品药品职业学院 | Preparation method of gold nanoparticle monomolecular film layer structure |
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