CN110844879B - In-situ controllable bonding method of amorphous nanowires and porous film - Google Patents
In-situ controllable bonding method of amorphous nanowires and porous film Download PDFInfo
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- CN110844879B CN110844879B CN201911111539.3A CN201911111539A CN110844879B CN 110844879 B CN110844879 B CN 110844879B CN 201911111539 A CN201911111539 A CN 201911111539A CN 110844879 B CN110844879 B CN 110844879B
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Abstract
The invention discloses an in-situ controllable bonding method of amorphous nanowires and a porous film, which comprises the steps of dispersing nanowires on a Transmission Electron Microscope (TEM) sample with a porous film structure, then placing the sample into the TEM, selecting nanowire segments with free ends protruding into holes of the porous film, and carrying out bonding treatment under the observation of the TEM according to a process of nanowire sharpening-nanowire hook-nanowire bonding. The invention utilizes the high-energy electron beam in the transmission electron microscope to perform targeted irradiation, realizes the sharpening and hooking of the amorphous nanowire, is finally bonded with the porous film with high quality, and has the advantages of in-situ, flexibility, controllability, high precision, low-temperature bonding and the like.
Description
Technical Field
The invention belongs to the field of micro-nano material processing, and particularly relates to an in-situ controllable bonding method of an amorphous nanowire and a porous film.
Background
Broadly speaking, bonding techniques are techniques in which two materials are bonded together by a chemical reaction occurring at the interface between the materials. The bonding technology is widely applied to the fields of MEMS devices and Integrated Circuits (ICs), is a high and new technology with full vitality, and has very important significance for the development of new technologies in China. In MEMS and microelectronic fabrication, bonding technology becomes one of the important processes in micromachining, and is an important component in microsystem and IC system packaging technology. At present, with the gradual increase of the integration degree of MEMS and microelectronic circuits, it is further required to implement the operable bonding technology in a smaller nanoscale range, or to perform the operable bonding technology between the nanomaterial and the thin film. The nano wire is a typical one-dimensional nano material, has a large length-diameter ratio, can be used as a functional construction unit of the micro-nano device by welding, and is also suitable for being used as an interconnection lead wire for device packaging and the like by bonding between the nano wire and a film, so that the nano wire has a wide application prospect in the fields of preparation and packaging of the micro-nano device. There have been some relevant studies in the literature currently on nanowire-to-nanowire soldering or fusing (see literature: 1.Xu S, Tian M, Wang J, et al, Small,2005,1: 1221; 2. Shengshou, electron microscopy, 2007, 26: 563; 3.Cheng L, Su J, Zhu X, Mater Lett,2019,237: 286). However, regarding the related art of bonding or interconnection between nanowires and thin films, the prior literature has grown nanowires on the surface of a substrate by self-assembly through a "bottom-up" method, and research attention is focused on the nanowires themselves; however, no relevant report is found on the bonding technology between the nanowire and the thin film through an artificial 'top-down' method, wherein the bonding technology is in situ, flexible, controllable, high in precision and low in temperature.
Disclosure of Invention
Aiming at the problems, the invention provides an in-situ controllable bonding method of an amorphous nanowire and a porous film.
The technical purpose is achieved, the technical effect is achieved, and the invention is realized through the following technical scheme:
an in-situ controllable bonding method of amorphous nanowires and porous films comprises the steps of dispersing nanowires on a Transmission Electron Microscope (TEM) sample with a porous film structure, then placing the sample into the TEM, selecting nanowire segments with free ends protruding into holes of the porous film, and carrying out bonding treatment under in-situ observation of the TEM according to the following method:
(1) sharpening the nanowire: selecting a focused electron beam with proper beam spot size and current density, irradiating the central axis position of the free end of the nanowire, and cutting and sharpening the nanowire;
(2) nanowire hooking: enlarging a beam spot of a focused electron beam, irradiating the nanowire from one side deviating from the central axis, and enabling the tip of the nanowire to generate hook deformation towards the other side until the tip of the nanowire contacts the position to be bonded of the porous film;
(3) and (3) nanowire bonding: when the tip of the nanowire contacts the position to be bonded of the porous film, the size of the electron beam spot is immediately further enlarged, and the position of the beam spot is moved at the same time, so that the bent nanowire segment and the porous film to be bonded are both in the irradiation range of the electron beam, and the nanowire is bonded to the porous film.
As a further improvement of the invention, the pore size of the porous membrane exceeds 250 nm.
As a further improvement of the invention, the amorphous nanowires include various amorphous metal nanowires, amorphous semiconductor nanowires, amorphous insulator nanowires, amorphous alloy nanowires, amorphous composite nanowires, amorphous coaxial structure nanowires, and the like.
As a further improvement of the invention, the step (1) further comprises the step of respectively controlling and adjusting the shape of the cut nanowire tip and the length of the free end by adjusting the size of the electron beam spot and the irradiation time.
As a further improvement of the invention, in the step (1), the beam spot size is 86 +/-20 nm, and the current density is 52 +/-23A/cm2。
As a further improvement of the invention, the step (2) further comprises controlling the direction and position of the nanowire hook by adjusting the radial and axial irradiation positions of the electron beam spot relative to the nanowire respectively.
As a further improvement of the invention, the step (2) further comprises a step of sharpening the nanowire.
As a further improvement of the invention, the size of the electron beam spot in the step (2) is 180 +/-40 nm, corresponding current density of 12 +/-5A/cm2。
As a further improvement of the invention, the step (3) further comprises the steps of controlling and adjusting the length or bonding area of the bonding wire by controlling the irradiation time, and performing the self-plasticity straightening process of the nanowire.
As a further improvement of the invention, the size of the electron beam spot in the step (3) is 360 +/-60 nm, and the corresponding current density is 2.7 +/-0.9A/cm2。
The invention has the beneficial effects that: the invention utilizes the high-energy electron beam in the transmission electron microscope to perform targeted irradiation, realizes the sharpening and hooking of the amorphous nanowire, is finally bonded with the porous film with high quality, and has the advantages of in-situ, flexibility, controllability, high precision, low-temperature bonding and the like.
(1) The invention adopts high-energy electron beams in a transmission electron microscope to carry out bonding processing, completes the core process of sharpening, hooking and bonding of the amorphous nanowire for the first time, and can carry out real-time and in-situ observation on the process progress.
(2) In the invention, high-energy electron beam irradiation is adopted to induce nano processing and bonding, the temperature rise of the sample caused by the irradiation is usually only a few degrees, namely the temperature does not exceed' room temperature +10 ℃, and the low-temperature bonding process is really realized.
(3) The invention can easily control the shape of the tip of the nanowire, the length of the free end, the direction and the position of the hook, the length or the bonding area of the bonding wire and the like by adjusting the parameters such as the beam spot size of the electron beam, the current density, the irradiation position, the irradiation time and the like, and has the characteristics of strong flexibility, controllability and high precision.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
FIG. 2 shows SiO selected in example 1xThe nano wire and high-energy electron beam irradiation induce the process of sharpening, hooking and bonding.
Fig. 3(a, b) are HRTEM images of the bonded region after irradiation in example 1 and EDS spectra at the circles in fig. (a), respectively.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail 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 following detailed description of the principles of the invention is provided in connection with the accompanying drawings.
Example 1: brittle amorphous SiOxBonding of nanowires to TEM micro-grid porous carbon film
1) TEM sample preparation:
firstly, a blade is used for scraping a little SiO from a silicon wafer substratexNanowire powder (<<1mg), then dispersing the mixture for 10 minutes by absolute ethyl alcohol (mass fraction is more than or equal to 99.7 percent) under ultrasonic vibration, and then using a liquid transfer gun to transfer SiO contained in the mixturexAnd dripping 2 drops of the ethanol solution of the nanowires on a porous carbon film attached with a copper grid micro grid, keeping the aperture of the porous carbon film about 1000nm, standing for 15 minutes, and airing to obtain a TEM sample.
2) Screening nanowires:
and (3) loading the TEM sample into a JEOL JEM-2100 transmission electron microscope, wherein the accelerating voltage is 200kV, and then selecting the nanowire segment to be irradiated and processed. As shown in fig. 2(a), the nanowire fragment comprises a free end, and the free end protrudes into a porous carbon film pore; the TEM observation magnification is 50,000 times proper, and the overall appearance and the main details of the nanowire segment can be observed at the same time.
3) The core process of the invention, sharpening, hooking and bonding, is finished by utilizing high-energy electron beams in a transmission electron microscope to carry out targeted irradiation.
3-1) sharpening the nanowire:
as shown by the circles in FIG. 2(a), the spot size was selected to be 86nm and the current density was selected to be 44A/cm at room temperature2The focused electron beam is aligned to the central axis position of the free end of the nano wire to irradiate. As shown in fig. 2(b), the sharpening and cutting process of the free end of the nanowire is realized within 30 s.
In the sharpening stage, the focused electron beam is adopted to be aligned with the central axis position of the free end of the nanowire for irradiation. At the moment, the focused electron beam intensity is in Gaussian distribution with stronger center and weaker edge, the nano curvature of the free end of the nanowire at the sharp corner where the bottom surface and the side surface are intersected is larger, the surface energy is higher, and the nano curvature and the surface energy cause atoms at the sharp corner of the free end to be lost preferentially in a melting and steaming mode, so that the sharpening and cutting processes of the nanowire are realized.
3-2) nanowire hooking:
as shown by the dotted circle in FIG. 2(b), the focused electron beam spot is enlarged to 180nm and the current density is reduced to 10A/cm2Then, the center of the beam spot is moved from the central axis of the nanowire (position shown by a dotted circle) to one side of the nanowire (position shown by a solid circle) for irradiation. As shown in fig. 2(c), the tip of the nanowire is bent and deformed toward the other side, and after 15s, the tip of the nanowire approaches and contacts the porous carbon film, thereby completing the hooking process of the nanowire. In the process of hooking the nanowire, the nanowire is still in the irradiation range of a Gaussian-distributed, non-uniform and quasi-focused electron beam, and the sharpening process of the nanowire is still carried out. As shown in fig. 2(c), the resulting nanowire tip portion is longer after the beam spot is enlarged.
In the nanowire hooking stage, quasi-focusing electron beams with properly enlarged beam spots are used for irradiating one side of the nanowires in an aligning mode. Due to SiOxNanowires are a typical insulator material, and the surface of the nanowires has a certain amount of net charges which cannot be neutralized under electron beam irradiation. When the quasi-focusing electron beam moves to one side of the nanowire, the quantity of electrons on the two sides of the nanowire is different, and the electric field force is also different, so that the electron beam irradiates SiO after the soft mold at ultra-fast speedxThe nanowire undergoes hook deformation.
3-3) nanowire bonding:
as shown in FIG. 2(c), when the nanowire tip contacts the position to be bonded of the porous carbon film, the beam spot of the electron beam is further enlarged to 360nm immediately, and the current density is reduced to 2.5A/cm2Changing the nano-wire segment into an electron beam with uniform intensity, and simultaneously moving the position of the beam spot to ensure that the bent nano-wire segment and the porous carbon film to be bonded are both in the irradiation range of the electron beam. With increasing irradiation time, the nanowire tips snap as shown in FIG. 2(d-i)The bonding area continuously extends and increases along the axis direction of the nanowire, so that the bonding between the nanowire and the porous carbon film is realized. Curved SiO as bonding continuesxThe nano-wire can be self-adjusted and straightened again under the irradiation of the uniform electron beam, and shows strong plastic rheological property.
In the nanowire bonding stage, electron beams with beam spots further enlarged and uniformly distributed intensities are adopted for irradiation. When the tip of the nanowire contacts the porous carbon film, the tip of the nanowire has infinite curvature and high surface energy, and can be rapidly bonded with the porous carbon film, so that point-type bonding between the tip of the nanowire and the porous carbon film is realized. Meanwhile, a negative curvature space is formed near the contact point, and atoms near the tip of the nanowire can be continuously filled into the negative curvature space through directional diffusion, so that linear bonding between the nanowire and the porous carbon film is gradually realized.
And (4) result characterization:
as shown in FIGS. 3(a-b), the structure and composition of the bonding region were further examined by HRTEM characterization and EDS analysis, respectively, to find SiOxThe nanowire and the conductive carbon film are both amorphous structures, and Si-O atoms have been partially diffused onto the porous carbon film, thereby realizing SiOxHigh quality bonding between nanowires and porous carbon films.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. An in-situ controllable bonding method of an amorphous nanowire and a porous film is characterized in that:
dispersing the nanowires on a Transmission Electron Microscope (TEM) sample with a porous film structure, then placing the sample into the TEM, selecting nanowire segments with free ends protruding into pores of the porous film, and carrying out bonding treatment under in-situ observation of the TEM according to the following method:
(1) sharpening the nanowire: selecting a focused electron beam with proper beam spot size and current density, irradiating the central axis position of the free end of the nanowire, and cutting and sharpening the nanowire;
(2) nanowire hooking: enlarging a beam spot of a focused electron beam, irradiating the nanowire from one side deviating from the central axis, and enabling the tip of the nanowire to generate hook deformation towards the other side until the tip of the nanowire contacts the position to be bonded of the porous film;
(3) and (3) nanowire bonding: when the tip of the nanowire contacts the position to be bonded of the porous film, the size of the electron beam spot is immediately further enlarged, and the position of the beam spot is moved at the same time, so that the bent nanowire segment and the porous film to be bonded are both in the irradiation range of the electron beam, and the nanowire is bonded to the porous film.
2. The in-situ controllable bonding method of amorphous nanowires and porous film as claimed in claim 1, wherein: the pore size of the porous film is more than 250 nm.
3. The in-situ controllable bonding method of amorphous nanowires and porous film as claimed in claim 1, wherein: the amorphous nanowires comprise various amorphous metal nanowires, amorphous semiconductor nanowires, amorphous insulator nanowires, amorphous composite nanowires and amorphous coaxial structure nanowires.
4. The in-situ controllable bonding method of amorphous nanowires and porous film as claimed in claim 1, wherein: the step (1) further comprises the step of respectively controlling and adjusting the shape of the tip end of the cut nanowire and the length of the free end by adjusting the size of the beam spot of the electron beam and the irradiation time.
5. According to the rightThe in-situ controllable bonding method of the amorphous nanowire and the porous film according to claim 1, characterized in that: the beam spot size in the step (1) is 86 +/-20 nm, and the current density is 52 +/-23A/cm2。
6. The in-situ controllable bonding method of amorphous nanowires and porous film as claimed in claim 1, wherein: and the step (2) further comprises controlling the direction and the position of the nanowire hook respectively by adjusting the radial and axial irradiation positions of the electron beam spot relative to the nanowire.
7. The in-situ controllable bonding method of amorphous nanowires and porous film as claimed in claim 1, wherein: the step (2) further comprises a step of sharpening the nanowire.
8. The method of claim 1, 6 or 7, wherein the in-situ controllable bonding method of the amorphous nanowires and the porous film comprises: the size of the beam spot of the electron beam in the step (2) is 180 +/-40 nm, and the corresponding current density is 12 +/-5A/cm2。
9. The in-situ controllable bonding method of amorphous nanowires and porous film as claimed in claim 1, wherein: the step (3) further comprises the steps of controlling and adjusting the length or bonding area of the bonding wire by controlling the irradiation time, and performing the self-plasticity straightening process of the nanowire.
10. The in-situ controllable bonding method of amorphous nanowires and porous film as claimed in claim 1 or 9, wherein: the size of the beam spot of the electron beam in the step (3) is 360 +/-60 nm, and the corresponding current density is 2.7 +/-0.9A/cm2。
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