CN104986727A - In situ control method for migration of alloy liquid in solid - Google Patents
In situ control method for migration of alloy liquid in solid Download PDFInfo
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- CN104986727A CN104986727A CN201510257257.XA CN201510257257A CN104986727A CN 104986727 A CN104986727 A CN 104986727A CN 201510257257 A CN201510257257 A CN 201510257257A CN 104986727 A CN104986727 A CN 104986727A
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Abstract
The invention provides an in situ control method for migration of alloy liquid in solid. In a vacuum system, voltage is applied to a single alloy-semiconductor heterojunction nano-material, alloy particles are melted under the action of current Joule heating, being driven by the voltage, the alloy liquid flows in a solid semiconductor nano-material, and by adjusting the voltage, the position and the moving direction of the alloy liquid in the nano-material can be controlled. By adjusting and controlling experiment parameters such as the voltage, the germanium nanowire length-diameter ratio and the like, the research result of the system is obtained, and a theoretical model is established; and it is discovered that under the driving action of the voltage, the migration of the alloy liquid is mainly determined by three power mechanisms of electromigration, thermal diffusion and viscous force. The results provide direct evidence for the research of one-dimensional materials, and especially solid-liquid interface kinetics in a two-phase system, and have an important reference value for intelligent manufacture and process of future heterojunction devices.
Description
Technical field
The present invention relates to a kind of method of being moved in solids by bias voltage manipulation alloy liquid, belong to nano material processing technique field.
Background technology
In recent years, along with developing rapidly of nanosecond science and technology, to nano material monomer carry out original position manipulation and physics and chemically Quality Research become the study hotspot of countries in the world gradually.On the basis of traditional microelectric technique and micro-processing method, design the modern measuring instrument of several typical research nano ZnO, comprise SEM, AFM, transmission electron microscope, wherein transmission electron microscope (TEM) is measured with it at the vertical material monomer of nano-precision drilling and in-situ performance and is become a kind of important tool exploring the physical property of monodimension nanometer material.
Up to now, by the on-spot study under Electronic Speculum, have been found that various nano level physical change, comprising fusing, crystallization, growth and mass transfer.The growth theory of these achievements to research nanocrystal has opened up the new visual field.In the effect observed, the physical change in two-phase system has potential application in nano wire processing, microfluid, pipette and semiconductor crystal doping.But, due to technical restriction, the phenomenon that this liquid moves in solids also never in an experiment home position observation arrive.In addition, the generation majority of the physical change before reported is the existence due to temperature gradient field in environment or homogeneous temperature field, and the true environment in this and practical devices has marked difference.
Consider Piezoelectric Driving in transmission electron microscope electricity specimen holder (STM-TEM) can in-situ construction one based on the simple electronic device of single nano material, so just can introduce a controlled electric field and the transition process of in situ detection liquid metals/alloy in solid nano line and the change of its electric property on nano wire.Namely the present invention builds based on this thought.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method that simple and effective original position manipulation alloy liquid moves in solids.
In order to solve the problems of the technologies described above, technical scheme of the present invention is to provide the method that a kind of original position manipulation alloy liquid moves in solids, it is characterized in that: in vacuum system, single alloy-heterojunction semiconductor nano material applies voltage, under the effect of electric current Joule heating, alloying pellet melts, under voltage driven, alloy liquid flows in solid semiconductor nano material, controls the position of alloy liquid in nano material and moving direction by regulation voltage.
Preferably, the method specifically comprises the steps:
Step 1: adopt chemical synthesis process to prepare the Ge nanoline of top with gold/germanium alloy particle, the Ge nanoline after synthesis is oxidized in atmosphere, Surface coating layer of oxide layer;
Step 2: prepared Ge nanoline is adhered on the Au needle point of mobile terminal: is fined away in one end of the Au silk of 0.25-0.35 millimeter with scissors, and be stained with Ge nanoline powder at the tip of Au silk, the Au needle point being stained with Ge nanoline powder is arranged on nano-probe sleeve pipe;
Step 3: the fixing Au electrode preparing the other end: with scissors, is fined away in one end of the Au silk of 0.25-0.35 millimeter, and be arranged on electricity specimen holder STM-TEM sleeve pipe;
Step 4: after the vacuum in example of transmission electron microscope room reaches requirement, inserts STM-TEM specimen holder, unlocking electronic bundle, observes and is scattered charge pattern, and controls movable electrode by the control system of STM-TEM specimen holder;
Step 5: while observation is scattered charge pattern, Au needle point finds the Ge nanoline that outstanding, Ge nanoline is moved by STM-TEM control system, Ge nanoline is connected with the Au needle point be arranged on STM-TEM sleeve pipe, the constant voltage of a 10-20V is added between two Au electrodes, and by display monitoring by the electric current between two Au electrodes, make to form stable point cantact between Ge nanoline and two electrodes;
Step 6: home position observation is scattered charge pattern, find that the gold/germanium alloy particle on Ge nanoline top melts under Joule heating effect, and flow in Ge nanoline in the other direction along electric current, in the process, in site measurement electric current, finds that the resistance of Ge nanoline reduces; Utilize STM-TEM control system, change voltage direction, find that the moving direction of gold/germanium alloy liquid also changes, namely moving direction is contrary with the sense of current all the time; Change voltage swing, find that the position of gold/germanium alloy liquid also changes thereupon; Therefore, the moving direction of gold/germanium alloy liquid in solid Ge nanoline and position can be controlled in real time by regulation voltage; When closing voltage, gold/germanium alloy liquid solidifies, volume-diminished.
Preferably, the method is handled by the STM-TEM control system be arranged in transmission electron microscope.
Preferably, the described gold/movement law of germanium alloy liquid in Ge nanoline is: under constant voltage, do retarded motion.
Preferably, the described gold/movement of germanium alloy liquid in Ge nanoline is also applicable to the motion in a semiconductor material of other alloy liquids, but the composition of semi-conducting material is necessary for one of composition comprised in corresponding alloy liquid.
Method provided by the invention is by experiment parameter such as regulation and control voltage, Ge nanoline draw ratio etc., obtain systematic research result, build theoretical model, find under voltage driven, the migration of alloy liquid is primarily of three kinds of power mechanisms, i.e. electromigration power, thermal diffusion and viscosity resistance, acting in conjunction determines.These results are not only one-dimensional material, and the solid liquid interface dynamics research especially in binary system provides direct evidence, and for following heterojunction device intelligence manufacture be processed with important reference value.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture that a Ge nanoline of embodiment 1 is connected between two Au electrodes;
Fig. 2 is that the gold/germanium alloy particle of embodiment 2 melts and the transmission electron microscope picture flowed;
Fig. 3 is that the gold/germanium alloy particle of embodiment 3 melts and passes completely through the transmission electron microscope picture of a Ge nanoline;
Fig. 4 is the transmission electron microscope picture that the flow direction of the gold/germanium alloy particle of embodiment 4 can be controlled by change voltage.
Detailed description of the invention
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
Ge nanoline is adhered on mobile terminal (Au) needle point: with scissors, is fined away in one end of the Au silk of 0.25-0.35 millimeter, and be stained with a small amount of Ge nanoline powder at the tip of Au silk, the Au needle point being stained with Ge nanoline powder is arranged on nano-probe sleeve pipe.Prepare the fixing Au electrode of the other end: fined away one end of the Au silk of 0.25-0.35 millimeter with scissors, and be arranged on STM-TEM sleeve pipe.After the vacuum in example of transmission electron microscope room reaches requirement, insert STM-TEM specimen holder, unlocking electronic bundle, observe and be scattered charge pattern, and control movable electrode by STM-TEM control system.While observation is scattered charge pattern, the Au needle point of mobile terminal finds the Ge nanoline that outstanding, Ge nanoline is moved by STM-TEM control system, Ge nanoline is connected with the Au needle point be arranged on STM sleeve pipe, as shown in Figure 1, between two Au needle points, add the constant voltage of a 10V, and by display monitoring by the electric current between them, make the good point cantact of formation between Ge nanoline and two electrodes.
Embodiment 2
On the basis of embodiment 1, home position observation is scattered charge pattern, find that the gold/germanium alloy particle on Ge nanoline top melts under Joule heating effect, and flow in Ge nanoline in the other direction along electric current, as shown in Figure 2, in the process, in site measurement electric current finds that the resistance of Ge nanoline reduces rapidly.When closing voltage, gold/germanium alloy liquid meeting quick solidification, volume-diminished.Fig. 2 a is depicted as a Ge nano wire and is connected between two Au electrodes; After Fig. 2 b-d is shown as and adds 10V voltage, gold/germanium alloy particle melts and flows to the process in Ge nanoline; After Fig. 2 e is shown as off voltage, gold/germanium alloy liquid meeting quick solidification, volume-diminished.
Embodiment 3
On the basis of embodiment 1, home position observation is scattered charge pattern, finds that the gold/germanium alloy particle on Ge nanoline top melts under Joule heating effect, and flow in Ge nanoline in the other direction along electric current, until pass completely through whole Ge nanoline, as shown in Figure 3.Fig. 3 a shows gold/germanium alloy particle and melts and flow, until arrive the mid point of Ge nanoline; Fig. 3 b shows gold/germanium liquid alloy through mid point until arrive the process of the other end of nano wire.In flow process, alloy liquid does uniformly retarded motion all the time under constant voltage, as shown in Figure 3 c.
Embodiment 4
On the basis of embodiment 1, utilize STM-TEM control system, change voltage direction, find that the moving direction of gold/germanium alloy liquid also changes, namely moving direction is contrary with the sense of current all the time, as shown in Figure 4.Fig. 4 a-f is shown as gold/germanium alloy liquid and moves to the mid point of Ge nanoline and be fractured into two parts, after Fig. 4 g is shown as and removes voltage, gold/germanium alloy liquid quick solidification volume-diminished, Fig. 4 h-j is for after adding backward voltage, gold/germanium alloy refuse is also flowed along with originally contrary direction, until arrive the top of Ge nanoline.Therefore, the moving direction of gold/germanium alloy liquid in solid Ge nanoline and position can be controlled in real time by regulation voltage.
Claims (5)
1. an original position handles the method that alloy liquid moves in solids, it is characterized in that: in vacuum system, single alloy-heterojunction semiconductor nano material applies voltage, under the effect of electric current Joule heating, alloying pellet melts, under voltage driven, alloy liquid flows in solid semiconductor nano material, controls the position of alloy liquid in nano material and moving direction by regulation voltage.
2. a kind of original position as claimed in claim 1 handles the method that alloy liquid moves in solids, it is characterized in that: the method specifically comprises the steps:
Step 1: adopt chemical synthesis process to prepare the Ge nanoline of top with gold/germanium alloy particle, the Ge nanoline after synthesis is oxidized in atmosphere, Surface coating layer of oxide layer;
Step 2: prepared Ge nanoline is adhered on the Au needle point of mobile terminal: is fined away in one end of the Au silk of 0.25-0.35 millimeter with scissors, and be stained with Ge nanoline powder at the tip of Au silk, the Au needle point being stained with Ge nanoline powder is arranged on nano-probe sleeve pipe;
Step 3: the fixing Au electrode preparing the other end: with scissors, is fined away in one end of the Au silk of 0.25-0.35 millimeter, and be arranged on electricity specimen holder STM-TEM sleeve pipe;
Step 4: after the vacuum in example of transmission electron microscope room reaches requirement, inserts STM-TEM specimen holder, unlocking electronic bundle, observes and is scattered charge pattern, and controls traveling electrode by STM-TEM control system;
Step 5: while observation is scattered charge pattern, Au needle point finds the Ge nanoline that outstanding, Ge nanoline is moved by STM-TEM control system, Ge nanoline is connected with the Au needle point be arranged on STM sleeve pipe, the constant voltage of a 10-20V is added between two Au electrodes, and by display monitoring by the electric current between two Au electrodes, make to form stable point cantact between Ge nanoline and two electrodes;
Step 6: home position observation is scattered charge pattern, find that the gold/germanium alloy particle on Ge nanoline top melts under Joule heating effect, and flow in Ge nanoline in the other direction along electric current, in the process, in site measurement electric current, finds that the resistance of Ge nanoline reduces; Utilize STM-TEM control system, change voltage direction, find that the moving direction of gold/germanium alloy liquid also changes, namely moving direction is contrary with the sense of current all the time; Change voltage swing, find that the position of gold/germanium alloy liquid also changes thereupon; Therefore, the moving direction of gold/germanium alloy liquid in solid Ge nanoline and position can be controlled in real time by regulation voltage; When closing voltage, gold/germanium alloy liquid solidifies, volume-diminished.
3. a kind of original position as claimed in claim 1 handles the method that alloy liquid moves in solids, it is characterized in that: the method is handled by the STM-TEM control system in transmission electron microscope.
4. a kind of original position as claimed in claim 1 handles the method that alloy liquid moves in solids, it is characterized in that: the described gold/movement law of germanium alloy liquid in Ge nanoline is: under constant voltage, do retarded motion.
5. a kind of original position as claimed in claim 1 handles the method that alloy liquid moves in solids, it is characterized in that: the described gold/movement of germanium alloy liquid in Ge nanoline is also applicable to the motion in a semiconductor material of other alloy liquids, but the composition of semi-conducting material is necessary for one of composition comprised in corresponding alloy liquid.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105480941A (en) * | 2015-12-30 | 2016-04-13 | 嘉兴学院 | Aluminum nano-wire array preparation method |
| CN106124543A (en) * | 2016-07-08 | 2016-11-16 | 东南大学 | Nano material based in situ TEM exchange electrical performance testing device and method |
| CN106744675A (en) * | 2017-01-22 | 2017-05-31 | 郑州大学 | A kind of nano material cutting off processing method |
| CN109164121A (en) * | 2018-08-01 | 2019-01-08 | 华东师范大学 | The preparation method of self assembly in-situ liquid chamber for transmission electron microscope characterization |
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| CN103586590A (en) * | 2013-11-12 | 2014-02-19 | 温州大学 | Nanometer welding method based on joule heat |
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| DMITRI GOLBERG, PEDRO M.F.J. COSTA, MASANORI MITOME ET AL.: "Nanotubes in a Gradient Electric Field as Revealed by STM TEM Technique", 《NANO RESEARCH》, vol. 1, 31 July 2008 (2008-07-31), pages 166 - 175 * |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105480941A (en) * | 2015-12-30 | 2016-04-13 | 嘉兴学院 | Aluminum nano-wire array preparation method |
| CN106124543A (en) * | 2016-07-08 | 2016-11-16 | 东南大学 | Nano material based in situ TEM exchange electrical performance testing device and method |
| CN106124543B (en) * | 2016-07-08 | 2019-04-09 | 东南大学 | Nano material exchange electrical performance testing device and method based in situ TEM |
| CN106744675A (en) * | 2017-01-22 | 2017-05-31 | 郑州大学 | A kind of nano material cutting off processing method |
| CN106744675B (en) * | 2017-01-22 | 2018-11-09 | 郑州大学 | A kind of nano material cutting off processing method |
| CN109164121A (en) * | 2018-08-01 | 2019-01-08 | 华东师范大学 | The preparation method of self assembly in-situ liquid chamber for transmission electron microscope characterization |
| CN109164121B (en) * | 2018-08-01 | 2020-10-16 | 华东师范大学 | Preparation method of self-assembly in-situ liquid cavity for transmission electron microscope characterization |
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Application publication date: 20151021 |