Method of obtaining metal nanoparticles on base surface

FIELD: metallurgy industry.

SUBSTANCE: invention refers to field of nanotechnology, to method of creation of metal nanoparticles on surface of base. Method involves preliminary application of metal thin-film coating on base surface and exposure of resultant coating to high-energy ion beam till coating melting and formation of variform nanoparticles of coating material on base surface. In order to create nanoparticles with diametre up to 100 nm, metal thin-film coating with thickness up to 20 nm from material with melting temperature up to 1500°C is applied on base made of inorganic glass or ceramised glass or oxidised silicium and is exposed to 1-3 pulses of nanosecond duration of powerful ion beam (PIB) composed of 70% C+ and 30% H+ with energy 300 KeV and current density 5-50 A/cm2.

EFFECT: formation of nanoparticles of various forms and sizes without change of base electrical properties with reduce of exposure time to 60-180 nanosec.

2 ex

 

The invention relates to the field of nanotechnology and can be used to create various substrates of metal nanoparticles. The use of such nanoparticles to create a variety of nanoelectronic devices, catalysts, gas sensors will increase the sensitivity of electronic devices to improve the efficiency of the catalytic and chemical processes.

A method of obtaining nanoparticles (Patent RF №2242532, MPK7 SS 4/00, B01J 2/02, B22F 9/00, publ. 20.12.2004), including the dispersion of the molten material, the supply of the liquid droplets of the material in the plasma is formed in an inert gas at a pressure of 10-1-10-4PA, cooling in an inert gas formed in the above-mentioned plasma liquid nanoparticles before hardening and coating the obtained solid nanoparticles to the media.

The disadvantages of this method are the high energy costs required to obtain molten material having a high melting point, a possible formation of an oxide on the surface of the drops when cooling even in an inert gas and a minor (small) adhesion resulting solid nanoparticles with the media.

A method of obtaining nanoparticles of metals (S.J.Henley, J.D.Carey and S.R.P.Silva. Pulsed-laser-induced nanoscale island formation in thin metal-on-oxide films. Physical Review B, V.72, 2005), which consists in applying a layer is of atalla (Au, Ag, Ni, Mo, Ti) to a thickness of 20 nm on the pre-oxidized silicon wafer with subsequent irradiation of 50 pulses of KRF excimer laser with a duration of 25 NS, and a wavelength of 246 nm, causing the melting of the metal layer and the subsequent formation of nanoparticles with a size of 10-40 nm due to Nesmachniy melt the surface of SiO2.

The disadvantages of this method are the need to use multiple effects of radiation on the specified system for nanoparticles, a strong change of the reflection coefficient of the laser radiation by melting a thin metal layer on the first radiation pulses, a high cooling rate of the melt is related to the transparency of the layer of SiO2for a given wavelength, which limits the structural-phase state of the obtained nanoparticles and their shape, in particular nanoparticles are amorphous state and due to the rapid cooling of the particles do not have time to acquire a spherical shape, which is necessary for application in sensors and catalysts.

Closest to the claimed is a method for the Pt nanoparticles with a size of 10-20 nm on the surface of SiO2(Yingbin Hu, David G. Cahill and Robert S. Averback, Dewetting and nanopattern formation of thin Pt films on SiO2 induced by ion beam irradiation, Journal of Applied Physics, V.89, No. 12, 15 June 2001, P.7777-7783)that includes applying a layer of Pt with a thickness from 3 to 10 nm on the pre is sustained fashion oxidized silicon wafer and the subsequent irradiation of this system is continuous (not pulsed) beam krypton ions with an energy of 800 Kev to a dose of not more than 6×10 15ion/cm2however , a single ion impacts with the specified parameters is not enough to melt all the platinum layer and the formation of nanoparticles, and requires additional heating of the silicon wafer up to 620°C.

The disadvantage of this method is the high heat load on the silicon wafer caused by high energy ions and a long exposure time is continuous beam, required for a set dose of 6×10 ion/cm2when the magnitude of the ion current, equal to 100, and the need for additional heating to 620°C. the High thermal load on the surface layers of silicon, resulting in obtaining of metallic nanoparticles with a melting point above 1000°C, leads to the redistribution of dopant in the silicon substrate and the change in its electrical characteristics and, consequently, deterioration of parameters of electronic devices produced on this substrate. As the authors of the minimum time of exposure to the ion beam in this case is 20 minutes.

The present invention is to provide a method for obtaining nanoparticles of metals on the surface of the substrate by exposing the ion beam on the pre-deposited on a substrate a thin-film metal coating for the formation of nanoparticles of various shapes without reaching the surface the displacement of the substrate to high temperature, leading to change of the electrical properties of the substrate while reducing the time of this impact to 60-180 NS.

This technical result is achieved in that in the method for production of metal nanoparticles on the surface of the substrate, based on the impact on pre-printed on the surface of the metal thin-film coating by ion beam of high energy to the melting temperature of the coating and formation on the surface of the substrate, the nanoparticle coating material of various shapes, for nanoparticles with a diameter up to 100 nm, a metal coating from a material with a melting temperature up to 1500°C with thickness up to 20 nm act 1 to 3 pulses of intense ion beam composition 70% C+and 30% of N+with the energy of 300 Kev nanosecond duration with a current density of 5-50 A/cm2while the substrate using inorganic glass, Sitall or oxidized silicon. For nanoparticles of aluminum with a mean diameter of 95 nm is irradiated film of aluminum with a thickness of 15 nm on the substrate made of inorganic glass by an ion beam with a current density of 30 A/cm2one pulse duration of 60 NS. For nanoparticles of Nickel with a diameter of 84 nm is irradiated film of Nickel with a thickness of 5 nm on the substrate made of the glass-ceramic ion beam with a current density of 10 A/cm2one pulse duration of 60 NS. To get the NAS is particles with a mean diameter of less than 80 nm impinges on the thin-film metal coating 2-3 surge pulses of nanosecond duration.

The sizes of the formed nanoparticles of metals set by the thickness of the thin-film metal coating, the melting point of the coating material, the contact angle of wetting of the molten substrate material and the value of the density of the ion beam current. The angle of incidence of the ion beam is set normal to the sample surface. The authors set a powerful ion beam: a composition of 70% With+and 30% of N+energy 300 Kev, a current density of 5-50 A/cm2one-three pulse irradiation time of 60 NS for the metallic coating thickness up to 20 nm and the melting temperature up to 1500°C for nanoparticles with size up to 100 nm. Moreover, the lower limit of the density of the ion beam current corresponds to the irradiation of materials with the lowest thickness of the coating, and the upper limit of the density of the ion current materials irradiation with the greatest coating thickness (20 nm). At the same time to reduce the average size of the formed nanoparticles using the number of pulses of irradiation is greater than 1. During the repeated irradiation is a partial evaporation of the metal nanoparticles, the reduction of its volume and therefore size. The application of this method provides for the formation of nanoparticles of aluminum on a substrate made of inorganic glass, glass-ceramic with a mean diameter of 95 nm upon irradiation of a film of aluminum with a thickness of 15 nm by a single pulse of high-power IO the aqueous beam with a current density of 30 A/cm 2. The increase in the number of pulses of irradiation up to 2 decreases the average diameter of the nanoparticles of aluminum to 90 nm, while increasing to 3 pulses the average diameter decreases to 86 nm.

The formation of metal nanoparticles on the surface of the substrate is achieved by a fast pulse heating not only the metal film and the underlying layers of the substrate, which ensures the presence of the metallic coating in the molten state 1-2 ISS and the formation of nanoparticles of different shapes. When used for metals decisive factors influencing the size and shape of the resulting nanoparticles are metal melting temperature, the contact angle between the edge of the melt and the substrate, the coefficient of surface tension of the melt, the melting temperature and thermal conductivity of the substrate material and the radiation mode of a powerful ion beam. When the contact angle between the edge of the melt and the substrate lower than 90°, the resulting nanoparticles have discopathy or hemispherical shape, and with a contact angle exceeding 90°, almost spherical in shape.

For deposited on a dielectric substrate made of inorganic glass aluminum thin film coatings with thickness up to 20 nm, having a melting point of 660°C, when exposed to 1 pulse MIP observed melting of the coating at all is azimah irradiation (at the current density of the beam in the range of 5-50 A/cm 2). Shorter (compared to the case with continuous ion impact) the presence of aluminum in the liquid state (1-2 µs) due to the smaller depth of the heated layer leads to the formation on the substrate surface of metal nanoparticles with a size of 95 nm and their conglomerates due to the low adhesion of aluminum to the substrate and poor wetting of the aluminum melt the substrate material (inorganic glass, Sitall, oxidized silicon). At the same time, the impact of the MIP with the specified parameters does not change the electrical properties of the substrate. The increase in the number of pulses of irradiation MIP to 2 leads to a reduction in the average diameter of the formed nanoparticles to 90 nm due to partial evaporation of the material of the nanoparticles. Irradiation of 3 surge pulses reduces the average diameter of the nanoparticles to 86 nm.

For Nickel, having a melting point of 1453°C, a higher ratio of surface tension and a lower value of adhesion to the substrate, there is the formation of nanoparticles with a smaller average diameter (up to 84 nm). While the number of nanoparticles formed on the unit area of the surface of the substrate, is increased in comparison with aluminum.

To implement the proposed method of obtaining particular importance is the choice of thickness of the thin-film metal coating and radiation mode. The most effect is ate for aluminum coating thickness of 15 nm was irradiated powerful ion beam with an ion current density of 30 A/cm 2one impulse; for Nickel coating thickness of 5 nm irradiation MIP with j=10 A/cm2one pulse.

The method of obtaining metal nanoparticles on the surface of the substrate is as follows.

Example 1. On the surface of the substrate from a glass-ceramic ARTICLE-50 under vacuum (5·10-6-1·10-5mm Hg) at a temperature not exceeding 150°C, is applied by the method of thermal evaporation of thin-film coating of aluminum of a thickness of 15 nm. After cooling, the substrate is coated with an aluminum coating is installed in the device located in a vacuum chamber technology accelerator "Temp" and is irradiated with a powerful ion beam directed normal to the sample surface and consisting of 30% H+and 70% With+, with an energy of 300 Kev, the average current density of 30 A/cm2duration 60 NS. When this occurs, the melting of the thin-film coating of aluminum and the formation of nanoparticles of aluminum. The size and shape of the nanoparticles was determined using optical and atomic force microscopy. The average diameter and density of the nanoparticles obtained in a single exposure MIP, was 90 nm and 108cm-2respectively.

When exposed to similar floor 2 surge pulses get the aluminum nanoparticles with an average diameter of 90 nm, and the irradiation of 3 pulses the average diameter of the nanoparticles is meniaetsa to 86 nm.

Example 2. On the surface of the substrate from a glass-ceramic ARTICLE-50 under vacuum (5·10-6-1·10-5mm Hg) at a temperature not exceeding 150°C, is applied by the method of thermal evaporation of thin-film coating of Nickel with a thickness of 5 nm. After cooling the substrate with the coating installed in the device located in a vacuum chamber technology accelerator "Temp", and was irradiated with high-power pulsed ion beam directed normal to the sample surface and consisting of 30% H+and 70% With+, with an energy of 300 Kev, a current density of 10 A/cm2duration 60 NS. When this occurs, the melting of the thin film coatings of Nickel and the formation of nanoparticles of Nickel. The size and shape of the nanoparticles was determined using optical and atomic force microscopy. The average diameter and density of the nanoparticles obtained in a single exposure MIP, was 84 nm and 3.5·109cm-2respectively.

When exposed to similar floor 2 surge pulses get the Nickel nanoparticles with an average diameter of up to 81 nm.

Thus, the inventive method provides for the formation of metal nanoparticles on the surface of the substrate using high-power pulsed ion beam of nanosecond duration, resulting in a reduction in heat and preservation of the properties of the substrate that is set for the manufacture of high-precision electronic devices.

1. A method for production of metal nanoparticles on the surface of the substrate, including the impact on pre-deposited on the surface of the substrate metal thin-film coating by ion beam of high energy to the melting temperature of the coating and formation on the surface of the substrate, the nanoparticle coating material of various shapes, characterized in that for nanoparticles with a diameter up to 100 nm, a metal coating from a material with a melting temperature up to 1500°C with thickness up to 20 nm effect 1-3 pulses of nanosecond duration with a powerful ion beam composition 70% C+and 30% of N+with the energy of 300 Kev with a current density of 5-50 A/cm2while the substrate using inorganic glass, Sitall or oxidized silicon.

2. The method according to claim 1, characterized in that for obtaining the aluminum nanoparticles with a mean diameter of 95 nm is irradiated film of aluminum with a thickness of 15 nm, deposited on a substrate made of inorganic glass, one pulse of high-power ion beam with a current density of 30 A/cm2and a duration of 60 NS.

3. The method according to claim 1, characterized in that to obtain the Nickel nanoparticles with an average diameter of up to 84 nm is irradiated film of Nickel with a thickness of 5 nm deposited on a substrate made of a glass-ceramic, one pulse of high-power ion beam with a current density of 10 A/cm2and a duration of 60 NS.

4. The method according to claim 1, the tives such as those that for nanoparticles with an average diameter of less than 80 nm impinges on the thin-film metal coating 2-3 pulses MIL nanosecond duration.



 

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