CN112853469A - In-situ growth method of refractory superstrong metal monocrystal nanowire - Google Patents

In-situ growth method of refractory superstrong metal monocrystal nanowire Download PDF

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CN112853469A
CN112853469A CN202011621078.7A CN202011621078A CN112853469A CN 112853469 A CN112853469 A CN 112853469A CN 202011621078 A CN202011621078 A CN 202011621078A CN 112853469 A CN112853469 A CN 112853469A
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钟立
李海
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Southeast University
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Abstract

The invention discloses an in-situ growth method of a super-strong metal tungsten single crystal nanowire with a large length-diameter ratio and low defect concentration. The specific method comprises the following steps: applying voltage to two tungsten tips which are in contact with each other based on an in-situ transmission electron microscopy technology to generate current, and locally melting and disconnecting the metal through Joule heating; the molten metal is rapidly solidified in a strong electric field between the two disconnected tips, and the metal tungsten single crystal nano wire with large length-diameter ratio and extremely low defect density is generated under the action of the electric field. The method realizes the one-step growth of the single tungsten single crystal nanowire, has simple steps and high efficiency (the growth time of the single nanowire is far less than 1 s); the prepared nano-wire has the characteristics of uniform size, few defects, high crystallinity, no surface pollution, large elastic strain, high strength and the like.

Description

In-situ growth method of refractory superstrong metal monocrystal nanowire
Technical Field
The invention discloses an in-situ growth method of ultra-strong metal tungsten single crystal nanowires with low defects and large length-diameter ratio. The method has the advantages of simple process, convenient operation, low cost and high efficiency; the grown tungsten single crystal nanowire has the characteristics of uniform size, high crystallinity, no surface pollution, few defects, large elastic strain, high strength (close to theoretical ultimate strength) and the like. The invention overcomes the technical bottleneck of growing refractory metal nanowires by using the traditional preparation method, is particularly suitable for preparing refractory high-strength metal single crystal nanowires, and belongs to the field of micro-nano processing and manufacturing.
Background
With the development of miniaturization of devices, micro-nano scale materials have received wide attention in the last decade. The metal nano wire is in a one-dimensional nano structure, has intrinsic anisotropy, not only has excellent electrical and thermal properties, but also has unique mechanical properties such as high strength and excellent deformation performance, so that the metal nano wire has wide application prospect in micro/nano devices. The traditional metal nanowire preparation method mainly comprises a gas phase synthesis method and a liquid phase synthesis method (Liuqing, Daifeng, Zhang, flood and, Zhang subsists and Wang, preparation of the metal nanowire and application thereof in electronic materials [ J ]. chemical reports 2020:1-44), but the experimental process is more complicated, the use of chemical medicines often causes surface pollution and low crystallinity of the nanowire, and meanwhile, the nanowire is easy to damage in the template removing process, so that higher defects are brought, and the elastic strain limit and the yield strength of the material are reduced; in addition, these preparation methods are often limited to metals having low melting points, and it is difficult to prepare metal nanowires having high melting points and low vapor pressures.
The tungsten nanowire has extremely excellent field emission performance, has great advantages in gate electrodes of integrated circuits and diffusion of deposition films, is expected to serve under severe conditions of high temperature, high stress, strong corrosion and the like, and is thus widely concerned. However, among all metals, tungsten has the highest melting point and the lowest vapor pressure (elevation, hastily, wangshilai. preparation of metal tungsten nanowire arrays [ J ] materials research report, 2008(06): 577-. At present, researchers have made a lot of work to study the growth of BCC tungsten metal nanowires, mainly based on the reduction of oxides (LeeYH, Choi C H, JangYT, Kim EK, Ju BK, Min NK, Ahn JH. tungsten nanowires and the field electron emission properties [ J ]. Applied Physics Letters,2002,81(4): 745. 747. and Vaddiraju S, Chandrasekaran H, Sunkara M K. vapor phase synthesis of structural steel nanowires [ J ]. Journal of the American Chemical Society,2003, 10736: 125-3.) and the decomposition of metal complexes (Thong J L, Oon C H, Ydon C, growth of the BCC tungsten metal nanowires [ J.: 2002, 4823. the growth of these nanowires often requires higher concentrations of oxides [ J ], (23) and growth of the metal complexes [ J., [ 2002, J.),4823. J ], and inevitably causes surface carbon contamination. In-situ welding techniques (Wang J, Zeng Z, Weinberger C R, et al. in situ atomic-scale actuation with simultaneous formation of nano scale body-centered cubic structure [ J ]. Nature Materials,2015,14(6): 594.; Zhong, L., Sansoz, F., He, Y. et al. slip-activated surface with row-temperature substrate-orientation in metallic nano crystalline Materials,2017,16, 439. 445.) although the fabrication of single metallic tungsten nanopillars can be achieved, the maximum aspect ratio is generally less than 5. Meanwhile, the two ends of the nano-column prepared by in-situ welding are fixed, so that the transfer of a single nano-column is difficult to realize.
How to prepare a single high-quality metal tungsten nanowire with a large length-diameter ratio and a free end shows great advantages in transfer technology and equipment application (Wood M, Zhang B. Bipolar electrochemical method for dynamic in situ control of single metal nanowire growth [ J ]. ACS Nano,2015,9(3): 2454-2464.). The metallic tungsten single crystal nano-wire grown by the in-situ technology is not reported in documents at home and abroad, can overcome the defects of the existing method, can obtain the metallic tungsten nano-wire with the characteristics of high strength, large elastic strain, uniform size, no pollution on the surface, few defects and the like at room temperature, and has wide application prospect in the aspects of electronic micro-nano processing, devices, sensors and the like.
Disclosure of Invention
The technical problem is as follows: the invention aims to provide a preparation method of a super-strong metal tungsten single crystal nanowire. The method overcomes the limitation of the existing method, and the tungsten single crystal nano wire with high strength, large elastic strain, uniform size, no surface pollution and less defects is obtained at room temperature. The method has potential application prospect in the aspects of electronic micro-nano processing, devices, sensing and the like.
The technical scheme is as follows:
the in-situ growth method of the superstrong tungsten single crystal nanowire is based on an in-situ transmission electron microscopy technology, a protrusion on the fracture surface of a metal tungsten wire is mutually contacted with a tungsten needle point etched in an electrochemical manner, and voltage is applied to generate current for joule heating; reducing the contact area of the two tungsten tips to increase the current density at the contact point until the contact point is melted and disconnected; the molten metal is rapidly solidified in an electric field with enhanced curvature between two disconnected tungsten tips, and the metal tungsten single crystal nanowire is generated at the tip of the needle tip under the action of the electric field, wherein the whole growth process is far less than 1 s.
Selecting a material with a curvature radius of 2.5-5 x 10-7m, applying a voltage of 8-10V to the tip of the probe, and setting the corresponding electric field intensity to 107-8V/m。
The superstrong metal tungsten monocrystal nanowire has no surface pollution, average diameter smaller than 50nm, length-diameter ratio up to 30, elastic strain up to 5.3% and corresponding bending strength up to 20.6 GPa.
Has the advantages that:
(1) the preparation method is simple, effective, safe, good in repeatability and controllable in shape and size
The metal single crystal nanowire can be effectively grown by breaking contact through the controller, high temperature, high pressure and other substances are avoided, the growth of the refractory metal single crystal nanowire without a catalyst at room temperature can be effectively realized by controlling applied voltage and current, the minimum diameter can be less than 10nm, the maximum length-diameter ratio can exceed 30, and multiple experiments show that the growth method of the metal single crystal nanowire has repeatability. (see attached figures 1 and 2)
(2) Refractory metal tungsten single crystal and pollution-free nano wire
The refractory metal tungsten single crystal nanowire prepared by the in-situ method is a nanowire with a large length-diameter ratio, which is rapidly directionally solidified and grown under the action of a metal melt under the action of a field effect in a high vacuum environment, so that the pollution of other substances is avoided, and the grown nanowire has the characteristics of uniform size, high crystallinity, no pollution on the surface, few defects and the like. (see FIG. 3).
(3) The nano wire has high strength and large elastic strain
The grown single crystal nanowire is qualitatively subjected to a bending test, the nanowire is bent to be close to 90 degrees without fracture, the elastic strain is about 5.3 percent, the bending strength is about 20.6GPa, (the theoretical fracture strength is about 37.6GPa, the [111] growth direction), and the nanowire can be recovered after the stress is removed (see figure 4). The strength of the metal nanowires is much higher (about one order of magnitude) than that of the metal nanowires reported so far, as shown in table 1.
Drawings
FIG. 1 is a schematic diagram of an in-situ growth device and an in-situ TEM image of a metal single crystal tungsten nanowire.
FIG. 2 TEM images of different sizes of metal single crystal tungsten nanowires.
FIG. 3 is an HRTEM image of the metal single crystal tungsten nanowire.
Figure 4 bending test of metal single crystal tungsten nanowires.
Detailed Description
The technical solution of the present invention is further explained below with reference to the specific embodiments and the accompanying drawings.
The in-situ growth method of the superstrong tungsten single crystal nanowire comprises the following specific steps: based on an in-situ transmission electron microscopic technology, a bulge on the fracture surface of a metal tungsten wire is mutually contacted with a tungsten needle point etched electrochemically, and voltage is applied to generate current for joule heating; reducing the contact area of the two tungsten tips to increase the current density at the contact point until the contact point is melted and disconnected; the molten metal is rapidly solidified in an electric field with enhanced curvature between two disconnected tungsten tips, and the metal tungsten single crystal nanowire is generated at the tip of the needle tip under the action of the electric field, wherein the whole growth process is far less than 1 s. The optimum electric field intensity and current vary with the radius of curvature of the tip, the physical properties (melting point, fluidity) of different metals, for tungsten metalSelecting a material with a curvature radius of 2.5-5 x 10-7m, applying a voltage of 8-10V (corresponding to an electric field intensity of about 10)7-8V/m) can prepare the nano-wire with larger long diameter.
The invention relates to a method for growing superstrong metal tungsten single crystal nanowires, which is based on an electron microscopy technology and utilizes the action of Joule heating and a strong electric field to grow single metal tungsten single crystal nanowires by a one-step method. The method overcomes the limitation of the existing method, and has the characteristics of high strength, large elastic strain, uniform size, no surface pollution and few defects under the room temperature condition. The metal single crystal nanowire has wide application prospects in the aspects of electronic micro-nano processing, devices, sensing and the like.
Examples
The method comprises the following specific steps:
(1) respectively installing a fracture surface of a tungsten metal wire (0.25mm, the purity of 99.9 wt.%) and a tungsten needle tip subjected to electrochemical etching at two ends of an in-situ electrical sample rod (Nanofactory STM-TEM holder), and placing the tungsten needle tip and the tungsten needle tip into an electron microscope (Titan 80-300), wherein the radius of curvature of the tip is 3 x 10-7m, radius of curvature of the sample end convex surface is 8 x 10-7m, contacting the tip end of the needle tip with the protruding surface of the sample end through a piezoelectric controller (Mains 220V), and applying constant voltage (8V) to generate current to carry out Joule heating;
(2) reducing the contact area of the two tips by moving the tungsten tip, wherein the current density of the contact point is increased to melt and break along with the reduction of the contact area; the molten metal is rapidly solidified in an electric field with enhanced curvature between two disconnected tungsten tips, and the metal single crystal nano wire is obtained at the tip of the needle tip under the action of the electric field. The whole growth process is far less than 1 s. The optimum electric field intensity and current vary with the curvature radius of the tip and the physical properties (melting point and fluidity) of the metal, and for tungsten, the curvature radius is 2.5-5 × 10-7m, applying a voltage of 8-10V (corresponding to an electric field intensity of about 10)7-8V/m) can prepare the nano-wire with larger long diameter.
Fig. 1a-c are schematic diagrams illustrating in-situ growth of a metal tungsten single crystal nanowire, which is implemented by applying 8V voltage, contacting a tip of a needle tip with a protruding surface of a sample, wherein two ends of the contacted tip form a molten state under the action of joule heat, current density gradually increases to a contact point to be melted and disconnected as a contact area decreases, and at the moment of disconnection, molten metal is solidified and grown under the action of an electric field with enhanced curvature between two disconnected tungsten tips, and finally the metal single crystal nanowire is formed on the side surface of the tip of the needle tip. The growth process of the nanowires was observed in situ by Transmission Electron Microscopy (TEM) as shown in fig. 1 d-e. The metal single nanowire prepared by the method has better controllability, the average diameter range of the nanowire is about 10-60nm, and the length range of the nanowire is about 20-1000nm, as shown in figure 2. As can be seen from the high resolution HRTEM of the nanowire in different observation directions, the metal single crystal nanowire has the characteristics of high crystallinity, uniform size, no surface pollution, few defects and the like, and the growth direction of the nanowire is [111], as shown in FIG. 3.
The mechanical properties of the metal nanowire are qualitatively tested in fig. 4, and bending experiments show that the metal nanowire has excellent mechanical properties, the nanowire is bent to approximately 90 degrees without fracture, the elastic strain is about 5.3%, the bending strength is about 20.6GPa, and the strength of the metal nanowire is much higher (about one order of magnitude) than that of the metal nanowire reported at present, as shown in table 1.
Table 1. statistics of test results of different metal nanowire strengths in published articles.
Figure BDA0002876155240000051

Claims (3)

1. An in-situ growth method of ultra-strong tungsten single crystal nanowires is characterized in that based on an in-situ transmission electron microscopy technology, a protrusion on the fracture surface of a metal tungsten wire is mutually contacted with a tungsten needle point etched electrochemically, and voltage is applied to generate current for Joule heating; reducing the contact area of the two tungsten tips to increase the current density at the contact point until the contact point is melted and disconnected; the molten metal is rapidly solidified in an electric field with enhanced curvature between two disconnected tungsten tips, and the metal tungsten single crystal nanowire is generated at the tip of the needle tip under the action of the electric field, wherein the whole growth process is far less than 1 s.
2. The in-situ growth method of ultra-strong tungsten single crystal nanowires of claim 1, wherein the radius of curvature is 2.5-5 x 10-7m, applying a voltage of 8-10V to the tip of the probe, and setting the corresponding electric field intensity to 107-8V/m。
3. The superstrong metal tungsten single crystal nanowire obtained by the in-situ growth method of the superstrong tungsten single crystal nanowire according to claim 1 or 2, wherein: no pollution on the surface, average diameter less than 50nm, length-diameter ratio up to 30, elastic strain up to 5.3%, and corresponding bending strength up to 20.6 GPa.
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