CN1924117A - Preparation method of two-dimensional plane gold nano single crystal plate - Google Patents
Preparation method of two-dimensional plane gold nano single crystal plate Download PDFInfo
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- CN1924117A CN1924117A CN 200610068530 CN200610068530A CN1924117A CN 1924117 A CN1924117 A CN 1924117A CN 200610068530 CN200610068530 CN 200610068530 CN 200610068530 A CN200610068530 A CN 200610068530A CN 1924117 A CN1924117 A CN 1924117A
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Abstract
The invention discloses a preparing method of two-dimension plane gold micro-nanometer single-chip disc, which comprises the following steps: (1) allocating mold; blending non-ion surface activator, clad and chlorauric acid solution; obtaining even hexagonal lysotropic liquid crystal; (2) stewing the lysotropic liquid crystal; (3) collecting the product; observing the product with regular trianglar or hexagonal structure through electron microscope; measuring the length at 1-10um and thickness at 10-100nm.
Description
Technical field
The present invention relates to a kind of preparation of nanomaterials, relate in particular to and a kind ofly utilize hexagonal to mix to cause the preparation method that the liquid crystal chemical reduction prepares two-dimensional plane gold nano single crystal plate.
Background technology
Noble metal nanometer material is paid close attention to owing to the peculiar property with aspects such as optics, electricity, acoustics, magnetics and mechanics and possible application prospect cause widely.People have demonstrated great interest to aspheric noble metal nanometer material recently, non-spherical noble metal nano particles such as bar-shaped, dendroid, tubulose and sheet have all obtained certain application, as nano-grade silver powder to the electrical property that improves electric slurry and to reduce the slurry sintering temperature extremely important.Wherein template is a kind of effective ways of this kind of preparation material.And guide its structure to form with the lytropic liquid crystals ordered structure, and have template to be easy to advantages such as removal, reaction conditions gentleness, be a good approach of synthesis of nano structured material.The combined with electrochemical deposition method, Attard etc. utilize the lytropic liquid crystals hexagonal to prepare porous-film (the G S Attard of metal platinum mutually, P N Bartlett, N R BColeman, J M Elliott, J R Owen, J H Wang.Mesoporous Platinum Films from LyotropicLiquid Crystalline Phases.Science, 1997, Vol 278,838-840), Yan etc. then utilize the anti-hexagonal of lytropic liquid crystals to obtain nano wire (L M Huang, H T Wang, the Z B Wang of argent mutually, A Mitra, K N Bozhilov, YS Yan.Nanowire Arrays Electrodeposited from Liquid crystalline Phase.Adv.Mater., 2002, Vol 14,61-64).About preparation gold nano dish, relevant report has also appearred both at home and abroad, for example Lee etc. utilizes ultraviolet light irradiation and heating (70 ℃) to handle (Kim J.U., Cha S.H., Shin K., Jho J.Y., Lee J.C..Preparation ofGold Nanowires and Nanosheets in Bulk Block Copolymer Phases under Mild Conditions.Adv.Mater., 2004,16 (5): 459-464.), Wang etc. utilizes liquid-phase reduction (Sun X., Dong S., Wang E..Large-Scale Synthesis of Micrometer-Scale Single-Crystalline Au Plates of NanometerThickness by a Wet-Chemical Route.Angew.Chem.Int.Ed., 2004,43 (46): 6360-6363; Shankar S.S., Rai A., Ankamwar B., Singh A., Ahmad A., Sastry M..Biological Syntiesis ofTriangular Gold Nanoprisms.Nature Mater., 2004,3:482-488.) etc.Need special preparation condition but above method exists, perhaps resulting product size is less, and shortcoming such as mechanism is indeterminate.
Summary of the invention
The problem to be solved in the present invention is, adopts a kind of lytropic liquid crystals hexagonal phase template simple and easy to operate, and the methods that prepare two-dimensional plane gold nano single crystal plate under a kind of mild conditions in a large number are provided.
The objective of the invention is to be achieved through the following technical solutions.
Two reactional equations that the chemical reduction process of nano material of the present invention relates to are as follows:
Total reaction equation is:
Above-mentioned reaction is to carry out in the polar water zone that is formed by tensio-active agent and aqueous solution of chloraurate in the lytropic liquid crystals, and the nonionogenic tenside that wherein forms liquid crystal promptly is that template is again as reductive agent.
The preparation method of two-dimensional plane gold nano single crystal plate of the present invention, step is as follows:
(1) configuration template is that the nonionogenic tenside of 40-50% and coating cats product and concentration that mass percent is 0.5-4% are 0.01-0.05mol/dm with mass percent
3Chlorauric acid solution mixes, and obtains uniform hexagonal phase lytropic liquid crystals;
(2) above-mentioned lytropic liquid crystals was at room temperature left standstill 24～240 hours;
(3) wash above-mentioned sample with water, tensio-active agent is removed, and under the 3000rpm condition centrifugal 15 minutes, collect centrifugal back gained precipitated product with the copper mesh that is covered with the Formvor film, use transmission electron microscope observing then, products therefrom presents well-regulated equilateral triangle, rescinded angle trilateral and regular hexagon structure, and the length of side is the gold nano single crystal plate of 1～10 μ m.
Wherein, the described nonionogenic tenside of step (1) is polyoxyethylene-poly-oxypropylene polyoxyethylene copolymer (EO
20PO
70EO
20, Pluronic P123).
Wherein, the described cats product of step (1) is a cetyl trimethylammonium bromide.
Wherein, the mass percent of the described nonionogenic tenside of step (1) is preferably 43-46wt%.
Wherein, the mass percent of the described cats product of step (1) is preferably 1-2wt%.
Wherein, the concentration of the described chlorauric acid solution of step (1) is preferably 0.02～0.04mol/dm
3
Wherein, the described time of repose of step (2) is preferably 48～150h.
Wherein, the described gold nano single crystal disc thickness of step (3) is at 10-100nm.
Wherein, in described step (1), (2) most preferably mass percent be 45% EO
20PO
70EO
20The cetyl trimethylammonium bromide and the 0.03mol/dm of (Pluronic P123) and mass percent 1%
3Chlorauric acid solution mixes, and the standing and reacting time is 120h.
Adopt method of the present invention to prepare two-dimensional plane gold nano single crystal plate, the gold nano single crystal plate that obtains has the trilateral or the hexagonal structure (as shown in Figure 3) of rule, and the length of side is about 1～10 μ m; The monocrystalline character of product and two-dimension plane structure character all utilize transmission electron microscope to characterize (as shown in Figure 4 and Figure 5), can be applied to fields such as electron device and catalysis.
Method of the present invention is compared with the existing technology of lytropic liquid crystals galvanic deposit nano material and other technology for preparing two Vygen dishes utilized, has following advantage:, can control size and particle morphology effectively by ratio and other reaction conditions of control protective material/reductive agent; Easy reaction has been eliminated the uppity mass transfer factor of electrochemical deposition; Be easy to behind the template reaction remove, the reaction conditions gentleness is controlled, does not need other energy expenditure, and this more helps saving cost; Be subjected to the control of liquid crystal ordered module plate structure, the product amount that obtains is big, and structure is distinct, realizes the artificial adjustment to product structure and output.
Description of drawings
The present invention will be further described below in conjunction with accompanying drawing.
Fig. 1 is the phasor of Pluronic P123 and water two component systems, is the basis that how to dispose lyotropic liquid crystal template.
Fig. 2 is that Pluronic P123 mixes the small angle X ray scattering curve that obtains lytropic liquid crystals with aqueous solution of chloraurate (0.03M), shows that further template is the hexagonal phase.
Fig. 3 is the transmission electron microscope photo of product, can observe to have regular triangle or hexagonal nanostructure, and its length of side is about 4～10 μ m, and thickness is 10-100nm.
Fig. 4 is the electron-diffraction diagram of product different shape and single particle, and wherein, a: trilateral, b and c: the rescinded angle trilateral, d: hexagon, e: single particle illustrates that the single nanoparticle of gained is monocrystalline.
Fig. 5 is the declivity observation electromicroscopic photograph of product, and wherein, a, b and c are three difform single crystal plates, and the product when d, e and f correspond respectively to sample inclination-50 ° shows that product has two-dimension plane structure.
Embodiment
The preparation method of embodiment 1. two-dimensional plane gold nano single crystal plates, step is as follows:
(1) selecting mass percent for use is the EO of 40wt%
20PO
70EO
20Cetyl trimethylammonium bromide and the 0.02mol/dm of (Pluronic P123), 0.5wt%
3Chlorauric acid solution mixes, and obtains even hexagonal phase lytropic liquid crystals;
(2) above-mentioned lytropic liquid crystals is at room temperature left standstill reaction times 48h;
(3) wash above-mentioned sample with water, tensio-active agent is removed, and under the 3000rpm condition centrifugal 15 minutes, centrifugal back gained precipitated product collected with the copper mesh that is covered with the Formvor film.With transmission electron microscope observation products therefrom pattern is the mixture of the gold nano single crystal plate of spheroidal particle and regular shape, and the gold nano single crystal plate length of side is 1～5 μ m, and thickness is 10-50nm.
The preparation method of embodiment 2. two-dimensional plane gold nano single crystal plates, step is as follows:
(1) selecting mass percent for use is the EO of 45wt%
20PO
70EO
20Cetyl trimethylammonium bromide and the 0.03mol/dm of (Pluronic P123), 1wt%
3Chlorauric acid solution mixes, and obtains even hexagonal phase lytropic liquid crystals;
(2) above-mentioned lytropic liquid crystals is at room temperature left standstill reaction times 120h;
(3) wash above-mentioned sample with water, tensio-active agent is removed, and under the 3000rpm condition centrifugal 15 minutes, centrifugal back gained precipitated product collected with the copper mesh that is covered with the Formvor film.With transmission electron microscope observation products therefrom pattern is the golden dish type particle of regular shape, and the length of side of single crystal plate is about 4～10 μ m, and thickness is 10-100nm, as shown in Figure 3.This product is further done electron diffraction analysis (as shown in Figure 4) and oblique view experiment (as shown in Figure 5), show that product is golden monocrystalline and has two-dimension plane structure.
The preparation method of embodiment 3. two-dimensional plane gold nano single crystal plates, step is as follows:
(1) selecting mass percent for use is cetyl trimethylammonium bromide and the 0.04mol/dm of Pluronic P123, the 4wt% of 50wt%
3Chlorauric acid solution mixes, and obtains even hexagonal phase lytropic liquid crystals;
(2) above-mentioned lytropic liquid crystals is at room temperature left standstill reaction times 240h;
(3) wash above-mentioned sample with water, tensio-active agent is removed, and under the 3000rpm condition centrifugal 15 minutes, centrifugal back gained precipitated product collected with the copper mesh that is covered with the Formvor film.With transmission electron microscope observation products therefrom pattern is the gold nano single crystal plate of regular shape, and the length of side is 2～10 μ m, and thickness is 10-100nm.
Claims (10)
1. the preparation method of a two-dimensional plane gold nano single crystal plate utilizes hexagonal to mix and causes the preparation of liquid crystal chemical reduction method, and equation is as follows
Total reaction equation is:
Concrete steps are as follows:
(1) configuration template is that the nonionogenic tenside of 40-50% and cats product and concentration that mass percent is 0.1-4% are 0.01-0.05mol/dm with mass percent
3Chlorauric acid solution mixes, and obtains uniform hexagonal phase lytropic liquid crystals;
(2) above-mentioned lytropic liquid crystals is at room temperature left standstill 24～240h;
(3) wash above-mentioned sample with water, tensio-active agent is removed, and under the 3000rpm condition centrifugal 15 minutes, collect centrifugal back gained precipitated product with the copper mesh that is covered with the Formvor film, use transmission electron microscope observing then, products therefrom is well-regulated equilateral triangle, rescinded angle trilateral and regular hexagon structure, is that the length of side is the gold nano single crystal plate of 1～10 μ m.
2. the preparation method of a kind of two-dimensional plane gold nano single crystal plate as claimed in claim 1 is characterized in that, the described nonionogenic tenside of step (1) is a polyoxyethylene-poly-oxypropylene polyoxyethylene copolymer.
3. the preparation method of a kind of two-dimensional plane gold nano single crystal plate as claimed in claim 1 is characterized in that, the described cats product of step (1) is a cetyl trimethylammonium bromide.
4. the preparation method of a kind of two-dimensional plane gold nano single crystal plate as claimed in claim 1 or 2 is characterized in that, the mass percent of the described nonionogenic tenside of step (1) is 43-46%.
5. as the preparation method of claim 1 or 3 described a kind of two-dimensional plane gold nano single crystal plates, it is characterized in that the mass percent of the described cats product of step (1) is 1-2%.
6. the preparation method of a kind of two-dimensional plane gold nano single crystal plate as claimed in claim 1 is characterized in that, the concentration of the described chlorauric acid solution of step (1) is 0.02-0.04mol/dm
3
7. the preparation method of a kind of two-dimensional plane gold nano single crystal plate as claimed in claim 1 is characterized in that, the described standing and reacting time of step (2) is 48-150 hour.
8. the preparation method of a kind of two-dimensional plane gold nano single crystal plate as claimed in claim 1 is characterized in that, the gold nano single crystal disc thickness of the described product of step (3) is 10-100nm.
9. as the preparation method of claim 1 or 2 or 3 described a kind of two-dimensional plane gold nano single crystal plates, it is characterized in that selecting mass percent in the described step (1) is 45% the polyoxyethylene-poly-oxypropylene polyoxyethylene copolymer and the cetyl trimethylammonium bromide and the 0.03mol/dm of mass percent 1%
3Chlorauric acid solution mixes.
10. as the preparation method of claim 1 or 7 described a kind of two-dimensional plane gold nano single crystal plates, it is characterized in that described step (2) the standing and reacting time is 120h.
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| CN102872860A (en) * | 2012-10-12 | 2013-01-16 | 安徽理工大学 | Method for preparing nanometer Pd electrocatalyst |
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| CN104275493A (en) * | 2013-07-02 | 2015-01-14 | 济南大学 | Method for preparing gold nanoplates with amino acid as reducing agent |
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| CN104625086A (en) * | 2015-02-10 | 2015-05-20 | 纳米籽有限公司 | Gold nanoparticle triangular plate preparing method and method for preparing gold nanoparticle discs and gold nanoparticle hexagonal pieces on basis of gold nanoparticle triangular plate preparing method |
| CN110616454A (en) * | 2019-03-07 | 2019-12-27 | 北京大学 | Method for vertical heteroepitaxy monocrystal metal film based on monocrystal two-dimensional material/monocrystal copper |
| CN112877782A (en) * | 2021-01-12 | 2021-06-01 | 南京工业大学 | Molecular design strategy of two-dimensional organic single crystal and preparation method thereof |
| CN114559029A (en) * | 2022-03-02 | 2022-05-31 | 广州大学 | Gold nanoparticles, preparation method and application thereof |
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