CN102416469B - Method for extracting thin metal nanoparticles - Google Patents
Method for extracting thin metal nanoparticles Download PDFInfo
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- CN102416469B CN102416469B CN 201110379953 CN201110379953A CN102416469B CN 102416469 B CN102416469 B CN 102416469B CN 201110379953 CN201110379953 CN 201110379953 CN 201110379953 A CN201110379953 A CN 201110379953A CN 102416469 B CN102416469 B CN 102416469B
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Abstract
The invention relates to a method for extracting thin metal nanoparticles. The method comprises the following steps of: mixing metal nanoparticle suspension and an organic solvent phase; adding a phase transfer catalyst; severely vibrating, and standing for lamination, wherein the color of a water layer is changed obviously; and forming the purified thin metal nanoparticles on a two-phase liquid surface, wherein the metal nanoparticles are water-based metal nanoparticles, the organic solvent is a solvent by which cyclic ketone and water are mutual exclusive, and the phase transfer catalyst is a quaternary ammonium salt phase transfer catalyst. The preparation method is relatively simple and quick and has extremely low requirements on experiment conditions, and complicated instruments and equipment are not needed.
Description
Technical field
The present invention relates to a kind of extracting method of sheet type metal nanoparticle.
Background technology
Metal nanoparticle is meant by the metallic particles (crystal grain) of diameter in nanometer scale.Because the film that metal nanoparticle forms has the field, a crucial forward position that high specific area, high activity, special rerum natura etc. have become nano materials research.Comparatively speaking, the purification extractive technique of metal nanoparticle has occupied critical role all the time in the research of nano thin-film, and along with Development of Preparation Technology and superlattices and quantum dot notion, can obtain huge development with the proposition of system engineering etc.
At present, the method that nano particle extracts mainly contains laser bombardment method, potassium dichromate oxidation, the purification of oxidation evaporating method etc., and mostly the method that the extraction of metal nanoparticle is purified phoenix feathers and unicorn horns especially is the centrifugal physical method that waits in solution.These methods often need preparation conditions such as special preparation equipment, complicated preparation technology and vacuum, high temperature, and efficient is lower, prepare then difficulty more of nano thin-film at the labyrinth substrate surface.
Therefore, the extracting method of a kind of metal nanoparticle easily and efficiently of exploitation is necessary.The invention provides a kind of novel, cleaning, extracting method of metal nanoparticle efficiently that has application prospect.
Summary of the invention
Technical problem:The extracting method that the purpose of this invention is to provide a kind of sheet type metal nanoparticle, this preparation method are comparatively simple, quick and very low to requirement for experiment condition, do not need complicated instrument and equipment.
Technical scheme:The extracting method of a kind of sheet type metal nanoparticle provided by the invention comprises: will contain difform metal nanoparticle suspension and mix mutually with organic solvent, add phase transfer catalyst, static layering behind the concuss, the generation significant change of water layer color and the sheet type metal nanoparticle after the two-phase liquid level forms one deck purifying.
Described metal nanoparticle is water base middle metal nanoparticle.
Described organic solvent is the solvent of cyclic ketones class and water objectionable intermingling.
Described phase transfer catalyst is a quaternary ammonium salt-type phase transfer catalyst.
Beneficial effect:The present invention has following advantage compared with prior art:
1, the extracting method of a kind of sheet type metal nanoparticle proposed by the invention can be used as a kind of new method that metal nanoparticle is purified, and also can be widely used in the preparation field of metal nanometer thin film.
2, the metal nanoparticle of the purifying of conventional physical, chemical method gained generally needed just can finish in several hours even several days.The present invention uses phase transfer catalyst that metal nanoparticle is extracted, and makes that the metal nano purifying is very fast, can finish in 30 seconds.
3, this method is a kind of method of purifying at mutual exclusive organic and inorganic solution interface, and the metal nanoparticle of the back gained of promptly purifying makes the process of purifying be in the dustfree environment fully in the spontaneous formation of liquid internal.
4, use the metal nanoparticle that this method extracts and have extraordinary repeatability.After the purifying particle appears in inorganic-organic interface place, both made the machinery concussion make film destruction, only need leave standstill a small amount of time, the purifying particle can appear at the interface again once more.
5, use the resulting purified metal nano particle of this method and can be self-assembled into the single or multiple lift metal nanometer thin film in the extremely short time, preparation technology is simple, environmental protection, is convenient to practical operation.
The specific embodiment
Below will describe the extracting method of present embodiment sheet type metal nanoparticle in detail.
The extracting method method of present embodiment sheet type metal nanoparticle mainly may further comprise the steps:
Step (one) is got a certain amount of organic solution, adds to contain difform metal nanoparticle suspension.Described metal nanoparticle suspension is that metal nanoparticle is mixed with the aqueous solution that mass fraction is 0.0025%-0.0045%.
Step (two) adds a small amount of phase transfer catalyst.
Phase transfer catalyst is the quaternary ammonium salt catalyst.The amount of substance concentration of the phase transfer catalyst that is added in organic facies is: 0.01-0.08mol/L.
Step (three), concuss leaves standstill a moment, the metal nanoparticle Guinier-Preston zone after the two-phase interface place forms one or more layers purification.
Experiment one:
(1) gets the 1ml cyclopentanone, add 1 ml silver nano-grain suspension, contain sphere, triangle template, hexagon sheet type silver nano-grain in this suspension;
(2) in above-mentioned mixed solution, add the 0.00806g quaternary ammonium salt phase transfer catalyst, and concuss all dissolves solid;
(3) leave standstill two phase stratification after about 10 seconds, aqueous solution color obviously shoals, and forms the sheet type silver nano-grain Guinier-Preston zone of one deck purifying at the two-phase interface place;
(4) upper and lower two-layer solvent is discarded, treat that volatilize residual solvents is done after, promptly obtain purer sheet type metal nanoparticle.
Experiment two:
(1) gets the 1ml cyclopentanone, add 1 ml gold nano grain suspension, contain sphere, sheet type gold nano grain in this suspension;
(2) in above-mentioned mixed solution, add the 0.00806g quaternary ammonium salt phase transfer catalyst, and concuss all dissolves solid;
(3) leave standstill two phase stratification after about 15 seconds, aqueous solution color obviously shoals, and forms the sheet type gold nano grain Guinier-Preston zone of one deck purifying at the two-phase interface place;
(4) upper and lower two-layer solvent is discarded, treat that volatilize residual solvents is done after, promptly obtain purer sheet type metal nanoparticle.
Experiment three:
(1) gets the 1ml cyclopentanone, add 1 ml silver nano-grain suspension, contain sphere, triangle template, hexagon sheet type silver nano-grain in this suspension;
(2) in above-mentioned mixed solution, add the 0.00464g quaternary ammonium salt phase transfer catalyst, and concuss all dissolves solid;
(3) leave standstill two phase stratification after about 10 seconds, aqueous solution color obviously shoals, and forms the sheet type gold nano grain Guinier-Preston zone of one deck purifying at the two-phase interface place;
(4) upper and lower two-layer solvent is discarded, treat that volatilize residual solvents is done after, promptly obtain purer sheet type metal nanoparticle.
Experiment four:
(1) gets the 1ml cyclohexanone, add 1 ml silver nano-grain suspension, contain sphere, triangle template, hexagon sheet type silver nano-grain in this suspension;
(2) in above-mentioned mixed solution, add the 0.00464g quaternary ammonium salt phase transfer catalyst, and concuss all dissolves solid;
(3) leave standstill two phase stratification after about 10 seconds, aqueous solution color obviously shoals, and forms the sheet type gold nano grain Guinier-Preston zone of one deck purifying at the two-phase interface place;
(4) upper and lower two-layer solvent is discarded, treat that volatilize residual solvents is done after, promptly obtain purer sheet type metal nanoparticle.
In addition, those skilled in the art also can do other and change in spirit of the present invention, and these variations of doing according to spirit of the present invention certainly all should be included in the present invention's scope required for protection.
Claims (2)
1. the extracting method of a sheet type metal nanoparticle, it is characterized in that this method comprises: the metal nanoparticle suspension is mixed mutually with organic solvent, add phase transfer catalyst, static layering behind the concuss, water layer color generation significant change, and form the sheet type metal nanoparticle of purifying at the two-phase liquid level;
Described organic solvent is the solvent of cyclic ketones class and water objectionable intermingling;
Described phase transfer catalyst is a quaternary ammonium salt-type phase transfer catalyst.
2. the extracting method of a kind of sheet type metal nanoparticle as claimed in claim 1 is characterized in that: described metal nanoparticle is water base middle metal nanoparticle.
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| CN 201110379953 CN102416469B (en) | 2011-11-25 | 2011-11-25 | Method for extracting thin metal nanoparticles |
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| CN 201110379953 CN102416469B (en) | 2011-11-25 | 2011-11-25 | Method for extracting thin metal nanoparticles |
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| CN102416469A CN102416469A (en) | 2012-04-18 |
| CN102416469B true CN102416469B (en) | 2013-07-31 |
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| CN1049160C (en) * | 1996-02-07 | 2000-02-09 | 吉林大学 | Preparation method for transition metal oxide nuclear shell type nano meter particle |
| WO2002041826A2 (en) * | 2000-11-24 | 2002-05-30 | Nanosolutions Gmbh | Phase transfer of nanoparticles |
| JP4293181B2 (en) * | 2005-03-18 | 2009-07-08 | セイコーエプソン株式会社 | Metal particle dispersion, method for producing metal particle dispersion, method for producing conductive film-formed substrate, electronic device and electronic apparatus |
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