Patent Grant
10746760
A method for moving and transferring nanowires using tapered hair of diameter in micron range relates to movement, transfer and fixation of nanowires, has an important influence on subsequent tests and representation, and particularly relates to in-situ nanomechanical tests and representation of a scanning electron microscope (SEM) and a TEM.
High-performance equipment requires the surfaces of high-performance parts to have nano-level planarity and subnano-level roughness. This harsh ultra-precision machining requirement is close to the limit of physical machining, which needs to be satisfied by developing new ultra-precision machining technologies and equipment. The nano-precision surface manufacturing method is an effective method to satisfy this harsh machining requirement. To develop the new nano-precision surface manufacturing technologies and methods, it is necessary to study an atomic-dimension damage generation and evolution mechanism, a material removal mechanism and a stress-induced damage formation mechanism. In-situ TEM nanomechanics is a scientific method to study the basic principle. In the past, due to the limitation of experimental conditions, it is difficult to conduct in-situ TEM nanomechanical test and representation. One of the important reasons is that the operation of cutting, welding, transferring and moving nanowires by focused ion beams and electron beams will cause pollution and damage to the nanowires. When the nanowires are fixed by the two methods, chemical vapor deposition or physical vapor deposition is generally adopted, which is easy to pollute the nanowires, so that subsequent in-situ test and representation are significantly affected, or even cannot be carried out, and it is also difficult to obtain atomic-demension high-resolution TEM images. In addition, in the process of moving and transferring the nanowires by the two methods, it is easy to produce defects such as cavity, interstitial atom, stacking fault and dislocation ring in the nanowires, which makes it difficult for the SEM and TEM images obtained at micro-nano scale to extend to macroscopic materials.
To eliminate the pollution and the damage to the nanowires caused by the traditional focused ion beams and electron beams in the process of moving, transferring, cutting, welding and fixing the nanowires, it is urgent to develop a novel method of moving, transferring and fixing the nanowires for bringing convenience for subsequent in-situ SEM and TEM nanomechanical test and representation, thereby eliminating the pollution and the damage caused by the operation for the nanowires by the traditional focused ion beams and electron beams.
The present invention adopts a method for moving and transferring nanowires using tapered hair of diameter in micron range, realizing movement and transfer of nanowires using tapered hair.
The present invention adopts the following technical solution:
A method for moving and transferring nanowires using tapered hair of diameter in micron range is provided. The nanowires have a diameter of 60-150 nm. The tapered hair comprises human eyebrow, eyelash, yellow weasel's hair and goat hair, and has a diameter range of 1-100 μm, a tip curvature radius of 0.8-3 μm and a length of 4-10 mm. A plastic film on a copper grid used for a TEM is burned with fire, the copper grid is reserved, and the diameter of the holes is 50-100 μm. Then, the copper grid after ultrasonic cleaning gains the nanowires from the acetone liquid with ultrasonic dispersed nanowires. The copper grid with nanowires and the tapered hair are respectively placed on mobile platforms of two different optical microscopes. Millimeter movement and micron movement of the tapered hair are realized, thereby realizing movement and transfer operation for the nanowires. The tip of the tapered hair is dipped in a small drop of conductive silver epoxy, and the conductive silver epoxy is respectively dropped on both ends of the nanowires; and the radius of the dropped conductive silver epoxy is 4-8 μm. The present invention provides a method for moving and transferring nanowires using tapered hair with diameter in micron range through mobile platforms of two optical microscopes.
The nanowires have a diameter of 60-150 nm. If the diameter of the nanowires is greater than 150 nm, an electron beam is difficult to penetrate through the nanowires and is difficult to obtain a high-resolution TEM micrograph of atomic dimension. If the diameter of the nanowires is less than 60 nm, it is very difficult to operate and seek under the optical microscopes. The diameter range of the nanowires is selected as 60-150 nm after comprehensive consideration of operation and atomic imaging.
The tapered hair comprises human eyebrow, eyelash, yellow weasel's hair and goat hair, and has a diameter of 1-100 μm, a tip curvature radius of 0.8-3 μm and a length of 4-10 mm. The four kinds of materials are obtained relatively easily, and come from human bodies and Chinese brush pens. Furthermore, the hairs are tapered, and are beneficial for operating the nanowires. The diameter range of the four kinds of hairs is 1-100 μm, which is convenient for accurately operating the nanowires. The tapered hair is easy for oblique insertion into the lower part of the nanowires under the optical microscope, thereby realizing the operation for the nanowires. The tip curvature radius is 0.8-3 μm, which is beneficial for utilization of electrostatic attraction between the tapered hair and the nanowires. The length is 4-10 mm in order to ensure that the tapered hair has certain rigidity and flexibility, thereby realizing operation and transfer for the nanowires.
A plastic film on a copper grid used for a TEM is burned with fire, the copper grid is reserved, and the diameter of the holes is 50-100 μm. To transfer the nanowires, the tapered hair shall be inserted into the lower part of the nanowires, so that the nanowires are moved, extracted and transferred relatively accurately. Therefore, a layer of plastic film that covers the copper grid needs to be removed. Because the plastic film is very thin, the plastic film can be quickly removed by a burning method, which is very clean and may not cause pollution to subsequent operation. Because the length of the nanowires is generally in micron range, the diameter of the holes of the copper grid is selected as 50-100 μm, so that the nanowires can be placed and will not fall into the holes of the copper grid.
Ultrasonic dispersion is conducted on the nanowires in acetone for 1-2 min. The acetone has strong decontamination and dispersion capabilities, and has more obvious effect by means of the ultrasonic action. Therefore, ultrasonic dispersion is conducted with the acetone for a short time of 1-2 min.
The copper grid is clamped with tweezers and is subjected to ultrasonic cleaning in an acetone solution for 0.5-1 min; then, the copper grid after ultrasonic cleaning gains the nanowires from the acetone liquid with ultrasonic dispersed nanowires; and after the acetone solution evaporates, the nanowires are distributed on the surface of the copper grid. The copper grid is clamped with the tweezers and is subjected to ultrasonic cleaning in the acetone so as to clean traces and pollution left by burning the copper grid. The cleaned copper grid gains the nanowires from the acetone solution with diffused nanowires, so as to reserve more uniformly distributed nanowires on the copper grid.
The copper grid with distributed nanowires and the tapered hair are respectively placed on mobile platforms of two different optical microscopes. The tapered hair is bonded to the tip of a tapered rod with conductive silver epoxy; and a flat end is fixed to the mobile platform of the microscope with the conductive silver epoxy. The copper grid is placed on the mobile platform of the optical microscope, and the optical microscope is used to seek and operate the nanowires. The tapered hair is connected with the mobile platform of another optical microscope. Macroscopic and microscopic movement functions of the mobile platform of another optical microscope are mainly used to realize accurate movement, extraction and transfer operation for the nanowires. The millimeter-micron combined movement function of another optical microscope is used to realize the operation for the nanowires.
Millimeter movement and micron movement of the tapered hair are realized through coarse control and fine control knobs of the mobile platform of the optical microscope, thereby realizing movement and transfer operation for the nanowires. A coarse control knob of the optical microscope is mainly used to realize rapid millimeter movement of the tapered hair, and a fine control knob is used to realize micron movement of the tapered hair, thereby realizing the operation for the nanowires.
The nanowires are observed in the optical microscope in which the copper grid is placed; movement and transfer operation is conducted by means of the tapered hair; the copper grid is replaced with an in-situ mechanical test micro apparatus used for an SEM or a TEM; the nanowires are placed in a proper position on the micro apparatus; the tip of the tapered hair is dipped in a small drop of conductive silver epoxy, and the conductive silver epoxy is respectively dropped on both ends of the nanowires; and the radius of the dropped conductive silver epoxy is 4-8 μm. The nanowires are found under the optical microscope and are focused. The mobile platform of another optical microscope is used to realize oblique insertion of the tapered hair into the lower part of the nanowires. The nanowires are lifted so that the electrostatic attraction between the nanowires and the copper grid is decreased. Then, the nanowires are extracted to leave the surface of the copper grid through the electrostatic attraction between the tapered hair and the nanowires. The copper grid is replaced with an in-situ mechanical test micro apparatus of the SEM or TEM, and the nanowires are placed in the tension position. The tip of the tapered hair is dipped in a drop of conductive silver epoxy which is slightly dropped on one end of the nanowires, and is dipped in another small drop of conductive silver epoxy which is dropped on the other end. The size radius of the dropped conductive silver epoxy is 4-8 μm. The nanowires are not polluted, and also have good bonding strength after solidification.
After 2-4 h in the air, the conductive silver epoxy is solidified to conduct in-situ nanomechanical test and representation of the SEM or the TEM. After standing in the air for 2-4 h, the conductive silver epoxy is solidified. The nanowires are firmly fixed to the micro apparatus without physical and chemical vapor deposition pollution and damage to the nanowires caused by ion beams and electron beams, so as to conduct in-situ nanomechanical test and representation of the SEM or the TEM.
The present invention has the effects and the benefits that the movement and the transfer of the nanowires are realized using the tapered hair of diameter in micron range; and the nanowires are fixed through the conductive silver epoxy, thereby avoiding pollution and damage caused by the operation for the nanowires by traditional focused ion beams and electron beams.
Specific embodiments of the present invention are further described below in combination with accompanying drawings and the technical solution.
A method for moving and transferring nanowires using tapered hair of diameter in micron range realizes movement and transfer of nanowires using tapered hair, wherein:
(1) the nanowires have a diameter of 60-150 nm;
(2) the tapered hair comprises human eyebrow, eyelash, yellow weasel's hair and goat hair, and has a diameter of 1-100 μm, a tip curvature radius of 0.8-3 μm and a length of 4-10 mm;
(3) a plastic film on a copper grid used for a TEM is burned with fire, the copper grid is reserved, and holes have a diameter of 50-100 μm;
(4) ultrasonic dispersion is conducted on the nanowires in acetone for 1-2 min;
(5) the copper grid is clamped with tweezers and is subjected to ultrasonic cleaning in an acetone solution for 0.5-1 min; then, the copper grid after ultrasonic cleaning gains the nanowires from the acetone liquid with ultrasonic dispersed nanowires; after the acetone solution evaporates, the nanowires are distributed on the surface of the copper grid;
(6) the copper grid with nanowires and the tapered hair are respectively placed on mobile platforms of two different optical microscopes. The tapered hair is bonded to the tip of a tapered rod with conductive silver epoxy; and a flat end is fixed to the mobile platform of the microscope with the conductive silver epoxy;
(7) millimeter movement and micron movement of the tapered hair are realized through coarse control and fine control knobs of the mobile platform of the optical microscope, thereby realizing movement and transfer operation for the nanowires;
(8) the nanowires are observed in the optical microscope in which the copper grid is placed; movement and transfer operation is conducted by means of the tapered hair; the copper grid is replaced with an in-situ mechanical test micro apparatus used for an SEM or a TEM; the nanowires are placed in a test position on the micro apparatus; the tip of the tapered hair is dipped in a small drop of conductive silver epoxy, and the conductive silver epoxy is respectively dropped on both ends of the nanowires; and the radius of the dropped conductive silver epoxy is 4-8 μm;
(9) after 2-4 h in the air, the conductive silver epoxy is solidified to conduct in-situ nanomechanical test and representation of the SEM or the TEM.
SiC single crystal nanowires with a diameter of 80-100 nm are selected as the operation objects. Human eyebrow and goat hair in the Chinese brush pen of goat hair (shown in
The solidified micro apparatus is placed in the in-situ mechanical test system of PI 95 TEM PicoIndenter. The system is inserted into FEI Tecnai F20 FETEM to conduct the TEM nanomechanical tension test. Operation voltage of the TEM is 200 kV. A displacement control mode is used; loading rate is 10 nm/s; and tension load is exerted to the nanowires. The nanowires have a diameter of 80-100 nm. The fractured force during fracture is 110 μN, and the fracture strength of the nanowires is 12 GPa. The dynamic tension process of the nanowires is recorded as a video by the in-situ mechanical test system. Key atomic-dimension high-resolution TEM images during fracture can be extracted from the video, thereby realizing in-situ TEM mechanical tension test and representation experiment of the nanowires.
| Number | Date | Country | Kind |
|---|---|---|---|
| 2017 1 1094075 | Nov 2017 | CN | national |
| Filing Document | Filing Date | Country | Kind |
|---|---|---|---|
| PCT/CN2017/111168 | 11/15/2017 | WO | 00 |
| Publishing Document | Publishing Date | Country | Kind |
|---|---|---|---|
| WO2019/090799 | 5/16/2019 | WO | A |
| Number | Date | Country |
|---|---|---|
| WO 0070325 | Nov 2000 | CN |
| 1689961 | Nov 2005 | CN |
| 101039870 | Sep 2007 | CN |
| 101949957 | Jan 2011 | CN |
| 107219243 | Sep 2017 | CN |
| WO 2016112171 | Jul 2016 | WO |
| Number | Date | Country | |
|---|---|---|---|
| 20200081033 A1 | Mar 2020 | US |
