CN105731370B - A kind of sequential 2 D gold nano grain array of large area and preparation method thereof - Google Patents
A kind of sequential 2 D gold nano grain array of large area and preparation method thereof Download PDFInfo
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- CN105731370B CN105731370B CN201610096649.7A CN201610096649A CN105731370B CN 105731370 B CN105731370 B CN 105731370B CN 201610096649 A CN201610096649 A CN 201610096649A CN 105731370 B CN105731370 B CN 105731370B
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 139
- 239000010931 gold Substances 0.000 title claims abstract description 139
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 139
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 53
- 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 20
- 239000002356 single layer Substances 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 239000012528 membrane Substances 0.000 claims abstract description 12
- 239000002105 nanoparticle Substances 0.000 claims abstract description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 20
- 239000000758 substrate Substances 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 8
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 8
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 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
- 229920005573 silicon-containing polymer Polymers 0.000 claims description 8
- 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 6
- 239000003921 oil Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 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
- 238000003756 stirring Methods 0.000 claims description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 235000013339 cereals Nutrition 0.000 description 95
- 239000000243 solution Substances 0.000 description 11
- 239000002245 particle Substances 0.000 description 7
- 238000001878 scanning electron micrograph Methods 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 5
- 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 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 208000004350 Strabismus Diseases 0.000 description 2
- -1 alkyl dimethyl ammonium chloride Chemical compound 0.000 description 2
- 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
- 229910003771 Gold(I) chloride Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 235000003283 Pachira macrocarpa Nutrition 0.000 description 1
- 240000001085 Trapa natans Species 0.000 description 1
- 235000014364 Trapa natans Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229960001040 ammonium chloride Drugs 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 125000005909 ethyl alcohol group Chemical group 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 230000035800 maturation Effects 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
- 235000009566 rice Nutrition 0.000 description 1
- 235000009165 saligot Nutrition 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
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- 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
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- 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
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- Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Composite Materials (AREA)
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Abstract
The invention discloses sequential 2 D gold nano grain array of a kind of large area and preparation method thereof, the sequential 2 D gold nano grain array is the entire area at least 1cm according to the structurally ordered arrangement of regular Hexagonal Close-packed by multiple spherical gold nano grains2Large area single-layer membrane structure；Its preparation method includes：Spherical gold nano grain is scattered in absolute ethyl alcohol, then is well mixed with n-butanol, the n-butanol dispersion liquid of gold nano grain is made；The n-butanol dispersion liquid of gold nano grain is dripped on the water surface in container along chamber wall, until being paved with single layer of gold nano particle on the water surface；The container is stood, until n-butanol volatilizees completely, then absolute ethyl alcohol is persistently dripped on the water surface along chamber wall, until the gold nano grain on the water surface is concentrated at one, so as to can be prepared by the sequential 2 D gold nano grain array of large area.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.
Description
Technical field
The present invention relates to gold nano-material field, more particularly to a kind of large area sequential 2 D gold nano grain array and
Its preparation method.
Background technology
Gold nano grain has higher molar absorption coefficient and preferable biocompatibility, therefore in catalysis, sensor
The fields such as part, opto-electronic device, biotechnology, biomedicine have broad application prospects.As gold nano grain prepares skill
Continue to develop and the maturation of art, the miscellaneous gold nano grain of high-volume are constantly developed and studied；But how to make these
Gold nano grain realizes that optimization, functionalization and device in performance are always major issue urgently to be resolved hurrily.
Self-assembling technique for will assembling primitive be directly integrated for functionalized nano material provide it is a kind of it is practicable newly
Approach；Compared with traditional " from top to bottom " preparation technology, self-assembling technique has simple to operate, need not be expensive instrument
Device equipment, it is with low cost many advantages, such as.The two dimensional structure array assembled by gold nano grain, its nano particle and nanometer
There can be strong surface plasmon resonance local fields coupling between particle, peripheral electromagnetic field is greatly increased
By force, so as to show the physical properties and chemical property different from single gold nano grain, this causes sequential 2 D gold nano
Grain array has broad application prospects in fields such as SERS, biology sensor, photocatalysis, photoelectric devices.
And in existing technology, be typically only capable to prepare micron or millimetre-sized small area sequential 2 D gold nano using self-assembling technique
Array of particles, it is impossible to prepare the sequential 2 D gold nano grain array of Centimeter Level or greater levels of large area, and it is existing
The sequential 2 D gold nano grain array stability that self-assembling technique is prepared is poor.
The content of the invention
In order to solve to prepare small area sequential 2 D gold nano grain array in existing self-assembling technique, and it is made
Standby sequential 2 D gold nano grain array stablizes poor technical problem, and the invention provides a kind of sequential 2 D Jenner of large area
Rice grain array and preparation method thereof, the large area single-layer membrane structure not only with square centimeter level, and also stability is high, prepares
Technique is simple, easily operation, with low cost, is very suitable for industrialized mass production.
The purpose of the present invention is achieved through the following technical solutions：
A kind of sequential 2 D gold nano grain array of large area, it is according to rule six by multiple spherical gold nano grains
The entire area at least 1cm of angle close-packed configuration ordered arrangement2Large area single-layer membrane structure.
Preferably, the sequential 2 D gold nano grain array can be in silicon base, quartz substrate, dimethyl silicone polymer base
Shifted between bottom.
A kind of preparation method of the sequential 2 D gold nano grain array of large area, including：
Step A, spherical gold nano grain is scattered in absolute ethyl alcohol, then mixed with n-butanol, and be uniformly dispersed, so that
The n-butanol dispersion liquid of gold nano grain is made；Wherein, the consumption of n-butanol is at least 20 times of absolute ethyl alcohol consumption；
Step B, in water surface area it is at least 25cm2Water container in, the n-butanol of the gold nano grain is disperseed
Chamber wall of the liquid along the container is dripped on the water surface in the container dropwise, until being paved with single layer of gold nano particle on the water surface；
Step C, by step B processing after, the container is stood, until the container in n-butanol wave completely
Hair；The chamber wall by absolute ethyl alcohol along the container is persistently dripped on the water surface in the container again, until the gold nano on the water surface
Particle concentration is at one, so that the sequential 2 D gold nano grain array of large area described in above-mentioned technical proposal is made.
Preferably, in stepb, the area of the water surface is more than 1cm in the container2。
Preferably, in step, if spherical gold nano grain is the aqueous dispersions using spherical gold nano grain, that
The spherical gold nano grain first carries out centrifugal treating, and redisperse is into absolute ethyl alcohol.
Preferably, the aqueous dispersions of the spherical gold nano grain are made using following methods：By gold chloride, polydiene third
Base alkyl dimethyl ammonium chloride, hydrochloric acid are added in ethylene glycol solution, and are stirred, then using oil bath heating to 195 DEG C of reactions 30
Minute, it is then added to row wet-chemical chamber in chlorauric acid solution and spherical gold nano grain colloidal sol is made, finally to described spherical
Gold nano particle colloidal sols are washed, so that the aqueous dispersions of spherical gold nano grain are made.
As seen from the above technical solution provided by the invention, the two dimension for the large area that the embodiment of the present invention is provided has
Sequence gold nano grain array and preparation method thereof first passes through self-assembling method sparse gold of confluent monolayers on the water surface in container
Nano particle, then absolute ethyl alcohol is added dropwise along along the lasting water surface into the container of chamber wall, so that the gold nano on the water surface
Particle to assembly is drawn close under the promotion of absolute ethyl alcohol together, and when the distance between gold nano grain is sufficiently closed to, these are golden
Nano particle can be stably floated on the water surface under the leading role of Van der Waals for, so as to be formed according to rule
Hexagonal Close-packed it is structurally ordered arrangement and entire area is at least 1cm2, show the large area two of bright golden colour lustre
Tie up orderly gold nano grain array.As can be seen here, the present invention not only has the large area single-layer membrane structure of Centimeter Level, and stably
Property it is high, preparation technology is simple, easily operation, with low cost, is very suitable for industrialized mass production.
Brief description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, being used required in being described below to embodiment
Accompanying drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for this
For the those of ordinary skill in field, on the premise of not paying creative work, other can also be obtained according to these accompanying drawings
Accompanying drawing.
Fig. 1 is to the large area prepared by the embodiment of the present invention 1 using the field emission scanning electron microscopes of Sirion 200
Sequential 2 D gold nano grain array shot obtained from overlook low power electron scanning micrograph.
Fig. 2 is to the large area prepared by the embodiment of the present invention 1 using the field emission scanning electron microscopes of Sirion 200
Sequential 2 D gold nano grain array shot obtained from overlook high power electron scanning electron micrograph.
Fig. 3 is to the large area prepared by the embodiment of the present invention 1 using the field emission scanning electron microscopes of Sirion 200
Sequential 2 D gold nano grain array shot obtained from squint low power electron scanning micrograph.
Fig. 4 is to the large area prepared by the embodiment of the present invention 1 using the field emission scanning electron microscopes of Sirion 200
Sequential 2 D gold nano grain array shot obtained from squint high power electron scanning micrograph.
Fig. 5 is the sequential 2 D gold nano grain array of the large area prepared by the embodiment of the present invention 1 respectively in the water surface, silicon
Comparison diagram in kind in substrate, quartz substrate and dimethyl silicone polymer substrate.
Embodiment
With reference to the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Ground is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based on this
The embodiment of invention, the every other implementation that those of ordinary skill in the art are obtained under the premise of creative work is not paid
Example, belongs to protection scope of the present invention.
Sequential 2 D gold nano grain array of large area provided below the present invention and preparation method thereof is described.
(1) the sequential 2 D gold nano grain array of a kind of large area
A kind of sequential 2 D gold nano grain array of large area, it is according to rule six by multiple spherical gold nano grains
The entire area at least 1cm of angle close-packed configuration ordered arrangement2Large area single-layer membrane structure, beautiful golden light is presented
Pool, and can be shifted in existing various substrates, for example：Silicon base, quartz substrate, dimethyl silicone polymer substrate etc..
(1) the sequential 2 D gold nano grain array of a kind of large area
A kind of preparation method of the sequential 2 D gold nano grain array of large area, may comprise steps of：
Step A, obtain spherical gold nano grain, and spherical gold nano grain be scattered in absolute ethyl alcohol, then with positive fourth
Alcohol is mixed, and is uniformly dispersed, so that the n-butanol dispersion liquid of gold nano grain is made.
Wherein, the used in amounts of absolute ethyl alcohol ensures each spherical gold nano grain Monodispersed obtained in absolute ethyl alcohol,
And the consumption of n-butanol is at least 20 times of absolute ethyl alcohol consumption；During absolute ethyl alcohol and n-butanol are liquid, therefore this step
The consumption of absolute ethyl alcohol and the consumption of n-butanol each mean volume.Decentralized processing can use ultrasonic disperse of the prior art.
Specifically, described spherical gold nano grain can be using spherical gold nano made from any method in the prior art
Particle, it would however also be possible to employ the spherical gold nano grain disperseed in any form in the prior art；But if spherical gold nano
Grain is the aqueous dispersions using spherical gold nano grain, then the spherical gold nano grain needs first to carry out centrifugal treating, to go
Moisture removal, redisperse is into absolute ethyl alcohol.In actual applications, the aqueous dispersions of the spherical gold nano grain can use with
Lower section method is made：Gold chloride, diallyl dimethyl ammoniumchloride, hydrochloric acid are added in ethylene glycol solution, and stirred,
Reacted 30 minutes to 195 DEG C using oil bath heating again, be then added to progress wet-chemical chamber in chlorauric acid solution and be made spherical
Gold nano particle colloidal sols, are finally washed twice to the spherical gold nano grain colloidal sol, to remove remaining second in colloidal sol
Glycol and diallyl dimethyl ammoniumchloride, so as to can be prepared by the aqueous dispersions of spherical gold nano grain.
Step B, in water surface area it is at least 25cm2Water container in, the n-butanol of the gold nano grain is disperseed
Chamber wall of the liquid along the container is dripped on the water surface in the container dropwise, until being paved with single layer of gold nano particle on the water surface.
Wherein, described container can be various water containers of the prior art (for example：Beaker), but the water surface in container
Area need be more than 25cm2, so can just prepare area at least 1cm2Large-area two-dimensional orderly gold nano grain battle array
Row.
Specifically, when the chamber wall by the n-butanol dispersion liquid of the gold nano grain along the container drips to the container dropwise
When on the interior water surface, drop can be sprawled rapidly on the water surface, interim n-butanol-water duplicature can be formed on the water surface, due to just
Butanol can quickly volatilize with it is miscible with water, therefore the n-butanol-water duplicature can become gradually thin along dispersal direction, and this makes
Obtaining gold nano grain can constantly accumulate at thin place, and stably be floated in the presence of liquid-vapor interface surface tension
On the water surface；As gold nano grain is constantly accumulated on the water surface, gold nano grain can be in dipole-dipole coupling and electrostatic reprimand
Under the interaction of power, assembling forms straight chain or linear chain structure；When being paved with single layer of gold nano particle on the water surface, presented on the water surface
Go out the gold lustre of dimness, gold nano grain is random and loosely swims on the water surface.
Step C, by step B processing after, the container is stood, until the container in n-butanol wave completely
Hair；The chamber wall by absolute ethyl alcohol along the container is persistently dripped on the water surface in the container again, until the gold nano on the water surface
Particle concentration is at one, so as to can be prepared by being at least according to the structurally ordered arrangement of regular Hexagonal Close-packed and entire area
1cm2The orderly gold nano grain array of large-area two-dimensional.
Wherein, tool can neatly select time of repose according to the quantity of n-butanol in the container, need to only ensure described
N-butanol in container volatilizees completely, for example：It can select to stand 12 hours under normal circumstances.
Specifically, when the chamber wall by absolute ethyl alcohol along the container is persistently dripped on the water surface in the container, ethanol
Drop can rapidly deploy on the water surface, and one interfacial tension gradient difference of generation at air liquid interface, and gold nano grain is on boundary
To assembling at one in the presence of face tension gradient difference, and re-assembly to form the single layer of gold nano-grain array of dense regular (i.e.
Single-layer membrane structure macroscopically), and show bright golden colour lustre；When the distance between gold nano grain is sufficiently closed to
When, the gold nano grain array of this dense regular can stably float on the water surface under the leading role of Van der Waals for
On, and stably can be shifted in existing various substrates.For example：The sequential 2 D gold nano grain array can be transferred to
Silicon base, quartz substrate, in soft dimethyl silicone polymer 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, system
Standby technique 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, below with tool
Sequential 2 D gold nano grain array for the large area that body embodiment is provided the embodiment of the present invention and preparation method thereof is carried out
It is described in detail.
Embodiment 1
The preparation method of the sequential 2 D gold nano grain array of a kind of large area, using gold chloride commercially
(purity is 99.9%, Sigma's reagent), diallyl dimethyl ammoniumchloride (molal weight is 100000~200000,
The 20wt% aqueous solution, Sigma's reagent), absolute ethyl alcohol (purity be more than 99.7%), (concentration is 37% to hydrochloric acid solution, Sigma
Reagent), ethylene glycol (ACS reagents) is raw material；It specifically may comprise steps of：
Step a, gold chloride is taken as golden presoma, take diallyl dimethyl ammoniumchloride as surfactant, will
Gold chloride, diallyl dimethyl ammoniumchloride, hydrochloric acid are added in ethylene glycol solution, and are stirred, so that it is anti-that gold is made
Answer liquid；In the golden reaction solution, AuCl4-The concentration of the Nong Du ﹕ hydrochloric acid of the Nong Du ﹕ diallyl dimethyl ammoniumchlorides of ion=
0.5mM ﹕ 25mM ﹕ 5mM.The golden reaction solution is placed in oil bath using oil bath heating to 195 DEG C and reacted 30 minutes, during this
Without any stirring, obtain that the red colloidal sol of light wine is presented after reaction, octahedra gold nano has been generated in this explanation colloidal sol
Particle；Then gold chloride (concentration of gold chloride is 0.0125mM), reaction two are added into the red colloidal sol of the presentation light wine
Minute, to remove water chestnut side and the drift angle on octahedra gold nano grain, so that red spherical gold nano grain colloidal sol is made.It is right
The spherical gold nano grain colloidal sol is washed twice, to remove remaining ethylene glycol and diallyl dimethyl in colloidal sol
Ammonium chloride, so as to can be prepared by the aqueous dispersions of spherical gold nano grain.
Step b, the aqueous dispersions for taking 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)；The good spherical gold nano grain of centrifugal treating is scattered in 50 μ L
In absolute ethyl alcohol, then mix with 1mL n-butanols, and ultrasonic disperse 15 minutes, so that finely dispersed gold nano grain is made
N-butanol dispersion liquid.
Step c, in the beaker of water is filled, by wall of cup of the n-butanol dispersion liquid of the gold nano grain along the beaker by
Drip on the water surface in beaker, until being paved with single layer of gold nano particle on the water surface.
Step d, after step c processing, the beaker is stood 12 hours, the n-butanol in the beaker is waved completely
Hair；The wall of cup by 5mL absolute ethyl alcohols along the beaker is dripped on the water surface in beaker dropwise again, until the gold nano grain on the water surface
Concentrate at one, so as to can be prepared by according to the structurally ordered arrangement of regular Hexagonal Close-packed and entire area at least 1cm2's
The orderly gold nano grain array of large-area two-dimensional.
Further, shape is carried out to the sequential 2 D gold nano grain array of the large area prepared by the embodiment of the present invention 1
Looks and performance detection, its specific testing result are as follows：
(1) sequential 2 D gold nano grain array made from step d in beaker in the embodiment of the present invention 1 is entered using naked eyes
Row observation, then sequential 2 D gold nano grain array made from step d is transferred to silicon base, quartz substrate and softness respectively
In dimethyl silicone polymer substrate, so as to shoot contrast photo in kind as shown in Figure 5；Wherein, Fig. 5 a are the embodiment of the present invention 1
In kind photo of the sequential 2 D gold nano grain array in beaker on the water surface made from middle step d, Fig. 5 b are implemented for the present invention
The photo in kind of sequential 2 D gold nano grain array on a quartz substrate made from step d in example 1, Fig. 5 c are implemented for the present invention
In kind photo of the sequential 2 D gold nano grain array made from step d in dimethyl silicone polymer substrate in example 1, Fig. 5 d are
The photo in kind of sequential 2 D gold nano grain array on a silicon substrate made from step d in the embodiment of the present invention 1.Can by Fig. 5
To find out：Sequential 2 D gold nano grain array is that entire area is at least made from step d in beaker in the embodiment of the present invention 1
1cm2Large area single-layer membrane structure, and beautiful gold lustre is presented, while the sequential 2 D gold nano grain array energy
Enough it is transferred to silicon base, quartz substrate, in soft dimethyl silicone polymer substrate.
(2) using the field emission scanning electron microscopes of Sirion 200 to big prepared by step d in the embodiment of the present invention 1
The sequential 2 D gold nano grain array of area is observed, and the scanning electron shot as shown in Figure 1, Figure 2, Figure 3 and Figure 4 shows
Micro mirror photo (SEM image)；Wherein, Fig. 1 is the sequential 2 D gold nano grain battle array of the large area prepared by the embodiment of the present invention 1
The vertical view low power SEM image of row, Fig. 2 is the sequential 2 D gold nano grain array of the large area prepared by the embodiment of the present invention 1
Vertical view high power SEM image, Fig. 3 is the sequential 2 D gold nano grain array of the large area prepared by the embodiment of the present invention 1
Low power SEM image is squinted, Fig. 4 is the oblique of the sequential 2 D gold nano grain array of the large area prepared by the embodiment of the present invention 1
Depending on high power SEM image.It can be seen that as the SEM image shown in Fig. 1 to Fig. 4：In the embodiment of the present invention 1 prepared by step d two
Orderly gold nano grain array is tieed up to be formed according to the structurally ordered arrangement of regular Hexagonal Close-packed by multiple spherical gold nano grains,
And the sequential 2 D gold nano grain array is entire area 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, system
Standby technique is simple, easily operation, with low cost, is very suitable for industrialized mass production.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, the change or replacement that can be readily occurred in,
It should all be included within the scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Enclose and be defined.
Claims (5)
1. a kind of preparation method of the sequential 2 D gold nano grain array of large area, it is characterised in that including：
Step A, spherical gold nano grain is scattered in absolute ethyl alcohol, then mixed with n-butanol, and be uniformly dispersed, so as to be made
The n-butanol dispersion liquid of gold nano grain；Wherein, the consumption of n-butanol is at least 20 times of absolute ethyl alcohol consumption；
Step B, in water surface area it is at least 25cm2Water container in, by the n-butanol dispersion liquid of the gold nano grain along should
The chamber wall of container is dripped on the water surface in the container dropwise, until being paved with single layer of gold nano particle on the water surface；
Step C, by step B processing after, the container is stood, until the container in n-butanol volatilize completely；Again
Chamber wall by absolute ethyl alcohol along the container is persistently dripped on the water surface in the container, until the gold nano grain collection on the water surface
Knot is at one, so that the sequential 2 D gold nano grain array of large area is made；
The sequential 2 D gold nano grain array of described large area is close according to regular hexagonal by multiple spherical gold nano grains
The entire area at least 1cm of the structurally ordered arrangement of row2Large area single-layer membrane structure.
2. the area of the water surface is big in preparation method according to claim 1, it is characterised in that in stepb, the container
In 1cm2。
3. preparation method according to claim 1 or 2, it is characterised in that in step, if spherical gold nano grain
It is the aqueous dispersions using spherical gold nano grain, then the spherical gold nano grain first carries out centrifugal treating, redisperse to nothing
In water-ethanol.
4. preparation method according to claim 3, it is characterised in that the aqueous dispersions of the spherical gold nano grain are used
Following methods are made：Gold chloride, diallyl dimethyl ammoniumchloride, hydrochloric acid are added in ethylene glycol solution, and stir equal
It is even, then reacted 30 minutes to 195 DEG C using oil bath heating, it is then added to row wet-chemical chamber in chlorauric acid solution and is made spherical
Gold nano particle colloidal sols, are finally washed to the spherical gold nano grain colloidal sol, so that spherical gold nano grain is made
Aqueous dispersions.
5. preparation method according to claim 1 or 2, it is characterised in that the sequential 2 D gold nano grain array can
Shifted between silicon base, quartz substrate, dimethyl silicone polymer substrate.
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| 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 |
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| CN103590037A (en) * | 2013-11-20 | 2014-02-19 | 苏州大学 | Gold nanoparticle monofilm preparation method and device thereof |
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| CN103590037A (en) * | 2013-11-20 | 2014-02-19 | 苏州大学 | Gold nanoparticle monofilm preparation method and device thereof |
| CN105252016A (en) * | 2015-11-11 | 2016-01-20 | 西安电子科技大学 | Preparation method of gold nanoparticle self-assembled transplantable single-layer thin film |
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