CN111112632A - Preparation method of low-melting-point high-electric-conductivity high-heat-conductivity metal nanoparticles - Google Patents
Preparation method of low-melting-point high-electric-conductivity high-heat-conductivity metal nanoparticles Download PDFInfo
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- CN111112632A CN111112632A CN201911405428.3A CN201911405428A CN111112632A CN 111112632 A CN111112632 A CN 111112632A CN 201911405428 A CN201911405428 A CN 201911405428A CN 111112632 A CN111112632 A CN 111112632A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F2009/0804—Dispersion in or on liquid, other than with sieves
- B22F2009/0812—Pulverisation with a moving liquid coolant stream, by centrifugally rotating stream
Abstract
The invention discloses a preparation method of metal nano-particles with low melting point, high electric conductivity and high heat conductivity, which comprises the steps of preparing liquid metal with low melting point, high electric conductivity and high heat conductivity, which is prepared according to a certain proportion, generally composed of elements of gallium, indium, zinc, tin, antimony and bismuth, and a surfactant solution, dripping the liquid metal into a beaker, simultaneously pouring the surfactant solution into the beaker according to a certain proportion, then putting an ultrasonic probe into the solution for a certain depth, opening an ultrasonic crusher, setting parameters such as temperature, time and amplitude, taking the liquid after oscillation after a certain oscillation time, and centrifugally cleaning, thus preparing the metal nano-particles with low melting point, high electric conductivity and high heat conductivity, wherein the particle size distribution of the particles is from 10 nanometers to 1000 nanometers. The preparation method of the metal nano-particles with low melting point, high electric conductivity and high heat conductivity is simple and convenient, and the stable particle state can be kept for a long time in a normal temperature environment. The method has the advantages of simple, quick and efficient preparation process, low cost and easy realization, and can be used for industrial production.
Description
Technical Field
The invention belongs to the field of liquid metal, and particularly relates to a preparation method of metal nanoparticles with low melting point, high electric conductivity and high heat conductivity.
Background
At present, liquid metal is widely applied to the fields of electronics, mechanical engineering, energy sources and the like. In recent decades, with the deep understanding of the physical and chemical properties such as low viscosity, good fluidity, high thermal/electrical conductivity, and good biocompatibility, the application of gallium and gallium-based low melting point (close to or lower than physiological temperature) alloys in the related fields such as biology and chemistry has been more and more emphasized. In the biological field, and in particular in biomedical applications, small droplets are preferred. Therefore, the dispersion of liquid metal into small particles is a very important direction for the development of various fields.
Disclosure of Invention
The invention aims to provide a preparation method of metal nanoparticles with low melting point, high electric conductivity and high heat conductivity aiming at the defects of large particle distribution and easy aggregation in the prior art. The method is easy to operate, controllable in cost and easy to apply to industrial production, and the obtained nanoparticles are distributed intensively and have long storage time.
The purpose of the invention is realized by the following technical scheme: a preparation method of metal nanoparticles with low melting point, high electric conductivity and high thermal conductivity comprises the following steps:
(1) mixing gallium and other metals to obtain a mixture, heating until the gallium and other metals are completely melted and uniformly mixed, and cooling to room temperature to obtain a liquid metal sample; the other metals are formed by mixing one or more of indium, zinc, tin, bismuth and antimony according to any proportion; the gallium accounts for not less than 60% of the atomic percentage of the mixture;
(2) adding an active agent solute into a polar solvent to obtain an active agent solution; the concentration of the active agent solution is 1mM-6 mM;
(3) adding the activator solution obtained in the step (2) into the liquid metal sample obtained in the step (1); (ii) a The volume mass ratio of the active agent solution to the liquid metal sample is 100ml:1 g;
(4) and (4) carrying out ultrasonic oscillation on the mixed solution obtained in the step (3) for 2-12h, wherein the amplitude is 20% -90%, and then carrying out centrifugal cleaning for 2-6 times by using a volatile cleaning agent, wherein the rotating speed is 1000-10000r/min, and the time is 2-8min, so as to obtain the metal nanoparticles.
Further, in the step (1), the liquid metal sample is Ga85.8In14.2Or Ga76In14Sn10。
Further, in the step (2), the active agent solute is selected from the group consisting of N-octadecyl mercaptan, N-dodecyl mercaptan, 3-mercapto-N-nonyl propionamide; the polar solvent is selected from absolute ethyl alcohol and acetone; the concentration of the active agent solution was 2 mM.
Further, in the step (4), the time of the ultrasonic oscillation is 6h, and the amplitude is 50%.
Further, in the step (4), the centrifugal cleaning is performed for 4 times, the rotating speed is 10000r/min, and the time is 5 minutes; the volatile cleaning agent is selected from absolute ethyl alcohol and acetone.
Further, the particle size of the metal nanoparticles is 10nm-1000 nm.
The invention has the beneficial effects that: the method is suitable for gallium-based series alloys, prepares the metal nanoparticles with low melting point, high electric conductivity and high heat conductivity to realize the refinement and the preservation of dispersion scale, and has the following characteristics:
1. the metal nanoparticles prepared from the low-melting-point liquid metal can keep a stable particle state for a long time in a normal-temperature environment under the condition of using an active agent.
2. The nano metal particles have simple and convenient original sample preparation, activator solution preparation and preparation processes, and low cost, and can be used for industrial production.
3. The sample prepared by the invention has uniform distribution and particle size, can reach a lower size value, and provides a sample and an idea for the research of nano metal particles and application thereof in the future.
Drawings
FIG. 1 is a scanning electron micrograph of low melting point, highly electrically conductive, highly thermally conductive metal nanoparticles;
fig. 2 is a particle size distribution diagram of the prepared low-melting-point, high-electric-conductivity and high-heat-conductivity metal nanoparticles.
Detailed Description
The present invention will be further described with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention relates to a preparation method of metal nanoparticles with low melting point, high electric conductivity and high heat conductivity, which comprises the steps of preparing metal with low melting point, high electric conductivity and high heat conductivity, preparing an active agent solution and oscillating an ultrasonic crusher. The low melting point refers to that the melting points of the gallium and other metals used as well as the prepared liquid metal sample and metal nanoparticles are lower than 15 ℃; the high electric conductivity and high heat conductivity mean that the prepared metal nanoparticles are formed by fusing metal elements, so that the prepared nanoparticles also have the metal characteristics of high electric conductivity and high heat conductivity.
An example of a simple method for preparing metal nanoparticles with low melting point, high electrical conductivity and high thermal conductivity is as follows:
example 1
The preparation method of the metal with low melting point, high electric conductivity and high heat conductivity comprises the following steps:
(1.1) respectively weighing gallium and indium according to the proportion by using an analytical balance, wherein the gallium Ga is 85.8 at%, the indium In is 14.2 at%, the purity is equal to or larger than 99.99% according to atomic percentage, and placing the weighed gallium and indium In a glass tube;
(1.2) putting the glass tube into a heating furnace, heating until the gallium and the indium are completely melted and uniformly mixed, and naturally cooling to room temperature to obtain liquid metal Ga85.8In14.2A sample; the liquid metal material Ga85.8In14.2Respectively, the electrical conductivity and the thermal conductivity of (2) are 3.9X 106S/m and 27.5 Wxm-1×K-1。
The preparation method of the active agent solution comprises the following steps:
(2) mixing n-octadecyl mercaptan (purity > 99%) and anhydrous ethanol uniformly to obtain an active agent solution with the concentration of the n-octadecyl mercaptan of 2mM, and introducing nitrogen to remove oxygen for five minutes.
The instrument that ultrasonication appearance vibration was used is ultrasonication appearance and iron stand platform, and the oscillation process includes following step:
(3.1) 0.2g of the liquid metal Ga prepared in the step (1.2) is taken85.8In14.2Dropping the sample into a beaker;
(3.2) taking 20ml of the activator solution prepared in the step (2), and pouring the liquid metal Ga obtained in the step (3.1)85.8In14.2In a sample;
(3.3) immersing the probe of the ultrasonic crusher in the position, close to the bottom of the cup, of the solution obtained in the step (3.2), fixing the probe by using an iron support, setting parameters such as time and amplitude, oscillating for 6 hours, wherein the amplitude is 50%, taking the liquid after oscillation, pouring the liquid into a cleaned centrifugal tube, centrifugally cleaning, setting the rotating speed of the centrifugal machine to 10000r/min, setting the centrifugal time to 5min, pouring out the supernatant after the centrifugation is finished, adding absolute ethyl alcohol, centrifuging again, repeating the process for 4 times, and thus obtaining the metal nanoparticles with low melting point, high electric conductivity and high heat conductivity.
Fig. 1 shows a scanning electron microscope image of metal nanoparticles with low melting point, high electrical conductivity and high thermal conductivity, and the particle distribution can be seen from fig. 1, and the particle size of the obtained particles is 10nm-1000 nm. The particle size distribution is given in fig. 2, and it can be seen from fig. 2 that the obtained nano-metal particles are mostly concentrated around 125 nm.
Example 2
Gallium and indium were weighed out In the same proportions, respectively, and In terms of atomic percentage, gallium Ga was 76 at%, indium In was 14 at%, and tin Sn was 10 at%, and the other steps were the same as In example 1. The obtained liquid metal material Ga76In14Sn10Has an electrical conductivity and a thermal conductivity of 4.024X 10 respectively6S/m and 29.68 Wxm-1×K-1. According to experimental data, the particle size of the metal nanoparticles prepared by the embodiment is 10nm-1000nm, and the metal nanoparticles have the characteristics of low melting point, high electric conductivity and high heat conductivity.
Example 3
Gallium, indium, tin and zinc are respectively weighed according to the mixture ratio, and according to atomic percentage, gallium Ga is 77 at%, indium In is 13 at%, tin Sn is 8 at%, and Zn is2 at%, the other steps were the same as in example 1. The obtained liquid metal material Ga77In13Sn8Zn2Has a conductivity of 3-5X 106And (5) S/m. According to experimental data, the particle size of the metal nanoparticles prepared by the embodiment is 10nm-1000nm, and the metal nanoparticles have the characteristics of low melting point, high electric conductivity and high heat conductivity.
Example 4
Gallium, indium and tin were weighed out In the proportions such that, In atomic percentage, gallium Ga was 62 at%, indium In was 25 at% and tin Sn was 13 at%, respectively, and the other steps were the same as In example 1. The obtained liquid metal material Ga62In25Sn13Has a conductivity of 3-5X 106And (5) S/m. According to experimental data, the particle size of the metal nanoparticles prepared by the embodiment is 10nm-1000nm, and the metal nanoparticles have the characteristics of low melting point, high electric conductivity and high heat conductivity.
The above-described embodiments are intended to illustrate rather than to limit the invention, and any modifications and variations of the present invention are within the spirit of the invention and the scope of the appended claims.
Claims (6)
1. A preparation method of metal nanoparticles with low melting point, high electric conductivity and high heat conductivity is characterized by comprising the following steps:
(1) mixing gallium and other metals to obtain a mixture, heating until the gallium and other metals are completely melted and uniformly mixed, and cooling to room temperature to obtain a liquid metal sample; the other metals are formed by mixing one or more of indium, zinc, tin, bismuth, antimony and the like according to any proportion; the gallium accounts for not less than 60 at% of the mixture.
(2) Adding an active agent solute into a polar solvent to obtain an active agent solution; the concentration of the active agent solution is 1mM-6 mM.
(3) Adding the activator solution obtained in the step (2) into the liquid metal sample obtained in the step (1); the volume mass ratio of the active agent solution to the liquid metal sample is 100ml:1 g.
(4) And (4) carrying out ultrasonic oscillation on the mixed solution obtained in the step (3) for 2-12h, wherein the amplitude is 20% -90%, and then carrying out centrifugal cleaning for 2-6 times by using a volatile cleaning agent, wherein the rotating speed is 1000-10000r/min, and the time is 2-8min, so as to obtain the metal nanoparticles.
2. The method for preparing low-melting-point high-conductivity high-thermal-conductivity metal nanoparticles according to claim 1, wherein in the step (1), the liquid metal sample is Ga85.8In14.2Or Ga76In14Sn10。
3. The method for preparing low-melting-point high-electrical-conductivity high-thermal-conductivity metal nanoparticles according to claim 1, wherein in the step (2), the active agent solute is selected from N-octadecyl mercaptan, N-dodecyl mercaptan, 3-mercapto-N-nonyl propionamide; the polar solvent is selected from absolute ethyl alcohol and acetone; the concentration of the active agent solution was 2 mM.
4. The method for preparing low-melting-point metal nanoparticles with high electrical conductivity and high thermal conductivity according to claim 1, wherein in the step (4), the ultrasonic oscillation time is 6h and the amplitude is 50%.
5. The method for preparing metal nanoparticles with low melting point, high electrical conductivity and high thermal conductivity according to claim 1, wherein in the step (4), the centrifugal cleaning is performed 4 times, the rotation speed is 10000r/min, and the time is 5 minutes; the volatile cleaning agent is selected from absolute ethyl alcohol and acetone.
6. The low melting point, high electrical conductivity, high thermal conductivity metal nanoparticle of claim 1, wherein the metal nanoparticle has a particle size of 10nm to 1000 nm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113388769A (en) * | 2021-06-11 | 2021-09-14 | 东莞市兆科电子材料科技有限公司 | Slurry alloy heat conduction material |
| CN115106536A (en) * | 2022-07-26 | 2022-09-27 | 无锡威孚环保催化剂有限公司 | Preparation method of monodisperse spherical gallium micro-nano particles |
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| CN103068939A (en) * | 2010-08-26 | 2013-04-24 | 原子能和替代能源委员会 | Liquid metal emulsion |
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Patent Citations (5)
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| JP2003286502A (en) * | 2002-03-28 | 2003-10-10 | Dowa Mining Co Ltd | Low-melting metal powder and manufacturing method therefor |
| CN101786167A (en) * | 2009-10-31 | 2010-07-28 | 西南科技大学 | Method for preparing superfine low melting point alloy particles |
| CN103068939A (en) * | 2010-08-26 | 2013-04-24 | 原子能和替代能源委员会 | Liquid metal emulsion |
| CN110373248A (en) * | 2019-08-20 | 2019-10-25 | 中国科学院兰州化学物理研究所 | A kind of preparation and application of Nano-Ga base fluid state metal lubrication additive |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113388769A (en) * | 2021-06-11 | 2021-09-14 | 东莞市兆科电子材料科技有限公司 | Slurry alloy heat conduction material |
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Application publication date: 20200508 |