CN106904570B - One kind being based on plasmon effect electric field-assisted Ag nano wire itself pattern restorative procedure - Google Patents
One kind being based on plasmon effect electric field-assisted Ag nano wire itself pattern restorative procedure Download PDFInfo
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- CN106904570B CN106904570B CN201710130047.3A CN201710130047A CN106904570B CN 106904570 B CN106904570 B CN 106904570B CN 201710130047 A CN201710130047 A CN 201710130047A CN 106904570 B CN106904570 B CN 106904570B
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Abstract
The invention discloses one kind to be based on plasmon effect electric field-assisted metal Ag nano wire itself pattern restorative procedure, apply the technical process of illumination combination electric field using Ag nanowire surface, technique is sprawled using simple fluid, it is stirred by atomic force microscope probe, Ag nano wire is placed between Silver Electrode, surface reconditioning is carried out to the Ag nano wire sample between being placed at Silver Electrode by applying illumination and electric field simultaneously, the defect for reaching 10 nm or so positioned at silver nanoparticle case depth can be repaired using the technology, the surface topography of Ag nano wire after reparation is close to or up to primary morphology, new technological means is provided to improve metal Nano structure defect repair precision and efficiency.
Description
Technical field
The invention belongs to nanometer recovery technique fields, in particular to are based on plasmon in the preparation of Ag nano-material
Effect realizes Ag nano wire itself pattern restorative procedure.More particularly to the local surface phasmon of Ag nano wire defective locations
(LSP) it excites and excites the heat generation and the movement of electric field inducing metal liquid state thin layer defective locations at position, it is final to realize
The new process of Ag nano wire defective locations reparation.
Technical background
With the development of nanophotonics and microelectronics domain, opto-electronic device is sent out towards intelligent with micromation direction
Exhibition, therefore the utilization of low-dimensional metal and nonmetallic micro-nano material becomes the hot subject of World Focusing.Although passing through hydro-thermal at present
The cheap chemical means such as synthesis can obtain a large amount of metal Nano structure with different characteristic, but metal micro-nanostructure
Structure feature is limited by the crystal growth pattern of metallic particles, must can not have the metal nano of any shape characteristic as desired
Structure.Meanwhile during further separating transfer and arrangement to metal nano material, inevitably draw in its material
Enter defect.Therefore, domestic and international a large amount of processes, such as photon pincers, atomic force microscope (AFM) probe visit pressure, current metal is received
The technologies such as rice welding, ultrasonic treatment are widely adopted, the metal micro-nano material pattern synthesized to further adjusting hydrothermal
With structure, while the introducing of defect is reduced.But with the further development of nanophotonics and micro-nano electronics, opto-electronic device
Volume it is smaller and smaller, the requirement to the precision and structure of material is higher and higher, therefore especially needs a kind of accurate and cheap
Control methods reduce or eliminate the defect generated in metal Nano structure growth, separation and transfer process.
Local plasmon excimer effect (LSP) in metal surface there is the optics of height localization characteristic to increase as a kind of
By force, high Electromagnetic enhancement can be generated in excitation area.Since there are ohmic loss, institutes under the action of light field for metal
Very high heat can be generated in the zone of action LSP, and then generated without significant heat in the non-zone of action LSP.And it is located at
The special metal defective locations on metal nanometer line surface can realize the excitation of LSP by way of momentum matching.In swashing for LSP
Under the conditions of hair, metal surface can generate the phase change layer of one layer of class " liquid ".Induction by extra electric field to the phase change layer, control
The liquefied metal surface atom moving direction of Ag nano wire, to further realize and optimize at metal Nano structure defective locations
Reparation manipulation.It can be seen that can be realized in the preparation of Ag nano-material to Ag nanowire surface position using the technology
The reparation of defect, while context is influenced without significant temperature.Therefore, exploitation is simple, efficiently auxiliary based on LSP metal electric field
Lower nano wire itself pattern recovery technique is helped to be feasible and there is very real application value.
Summary of the invention
The present invention proposes a kind of based on LSP electric field-assisted Ag nano wire itself pattern restorative procedure, benefit regarding to the issue above
Surface phase change layer is generated in defective locations heat build-up with LSP, then utilizes the process means regulation phase change layer metal of regulation electric field
Migratory direction, to realize the purpose of Ag nanowire surface defect repair.
To solve the above-mentioned problems, LSP electric field-assisted Ag nano wire is based on the technical solution of the present invention is to provide a kind of
Itself pattern restorative procedure, while applying illumination and electric field and the Ag nano wire sample progress surface between being placed at Silver Electrode is repaired
It is multiple.
Specific step is as follows:
A. it cleans sheet glass: glass sheet surface tentatively being cleaned using sodium sulfate of polyethenoxy ether of fatty alcohol solution,
Remove the greasy dirt and impurity of glass surface.
B. acetone soln is utilized, the organic pollutant of glass sheet surface is removed, then deionized water is cleaned by ultrasonic, finally
It to the silicon wafer of surface cleaning, is dried with nitrogen, is stored in drier.Cleaning water resistance rate used must 16 Ω cm with
On.
C. it is surface-treated: sample being placed in ozone generating-device and handles 30min, is combined between glass and metal to improve
Power.
D. it sputters silver-plated: in sputtering current being 15 ~ 20 mA, sputtering time 150-200s using magnetron sputtering instrument
Under the conditions of, one layer of Silver Electrode is plated in glass surface.
E. nitrogen atmosphere annealing: under nitrogen atmosphere protection, under the conditions of 250 ~ 300 DEG C, anneal sample 0.5-1h, improves silverskin
Binding force between electrode and glass substrate.
F. device is built: being used diameter for 100 μm of probes, is prepared 80-120 μm of diameter by being inscribed in sample surfaces
To electrode.The defective Ag nano wire of trace band is placed in the side of electrode by the method sprawled by liquid stream.It is flat by fine motion
Ag nano wire one end is placed on electrode by platform and probe, and the other end is placed between electrode.
As a kind of improvement of this programme, optical electric field can also be applied: between electrode while apply optical electric field, intensity of illumination
50-100mW/mm2, electric field strength 300-1000V/cm.Time 40-80 min.
Another kind as this programme improves, using atomic force microscope to the pattern of Ag nano wire defective locations after processing
Test and comparison is carried out with primary morphology.
As the further improvement of this programme, sodium sulfate of polyethenoxy ether of fatty alcohol solution washing lotion used in the step a
For the mixed solution of sodium sulfate of polyethenoxy ether of fatty alcohol and ultrapure water that mass fraction is 60%.
Passing through Ag nanowire diameter as the further improvement of this programme, used in the step e is 150-200 nm,
30-50 μm of length.
As the further improvement of this programme, Ag nano wire is by ultrasonic treatment, to generate and improve its surface
Defect.
Preferably, in order to guarantee the monochromaticjty of light source, light source uses laser light source；Power supply is common regulated power supply.
Compared with prior art, microelectrode structure is prepared using of the invention, by applying illumination in Ag nanowire surface
With auxiliary electric field, so that the damage of Ag nanowire surface obtains significant reparation, specific effect is showed themselves in that
1. in the case where 476 nm wavelength lights are shone and are acted on 1000 V/cm auxiliary electric fields, Ag nanowire tip damage field surface
Roughness is substantially reduced.
It is nanophotonics 2. this method provides new effective technology means for metal nano material itself pattern reparation
Development and industrial application with microelectronics domain provide new approaches.
3. the means of the simple illumination of the invention patent and load electric field, operation is easy, equipment requirement is simple；Metal is received
The craft precision of the reparation of rice noodles is higher, while generating temperature Centralized, will not cause significant impact to nano wire adjacent material.
Therefore, which is suitable for the reparation of common metal micro-nano structure, especially suitable for the organic of temperature more sensitivity
The pattern reparation of metal micro-nanostructure in substrate.
Detailed description of the invention
Fig. 1 a be Silver Electrode and be placed in interelectrode Ag nano wire, wherein in figure b I be existing defects plasma,
II is the plasma exciatiaon process through over-illumination, and III is the plasma after the reparation of electric field-assisted；
Fig. 2 is the pattern of Ag nano wire defective locations in repair process under atomic force microscope；
Fig. 3 is 2 scribing position of corresponding diagram, Ag nanowire tip surface undulation height characterization.
Wherein, 1- is illuminated, 2- plasma, 3-Ag electrode, 4-Ag nano wire, 5- silicon dioxide substrate.
Specific embodiment
The purpose of the present invention is to propose to be based on plasmon effect electric field-assisted metal Ag nano wire itself pattern reparation
Method.The present invention is further described with embodiment with reference to the accompanying drawing, but is not belonging to further limit of the invention
It is fixed.
Embodiment one:
1. clean sheet glass is cut into the sample of 2 × 3 cm, it is then immersed in sodium sulfate of polyethenoxy ether of fatty alcohol
In Solutions Solution, 35 DEG C of water bath sonicator 5min；Then ultrasound 10min in deionized water is impregnated after being rinsed 3 times with deionized water.
2. taking out sample, it is placed on 5 min of soak at room temperature in acetone soln, taking-up is rinsed 3 times with deionized water, and nitrogen is blown
It is dry, it is put into spare in drier.
3. the above-mentioned sample prepared is placed in ozone generating-device and handles 30 min.
4. using magnetron sputtering instrument under conditions of sputtering current is 20mA, sputtering time 150s, in glass surface
Plate one layer of silverskin in face.
5. under the conditions of 250 DEG C, anneal sample 0.5h under nitrogen atmosphere protection, can be observed in glass surface after annealing
To one layer of silverskin.
6. use diameter for 100 μm of probes, by be inscribed in sample surfaces prepare 80 μm of diameter to electrode.Ag is received
Rice noodles are scattered in ethanol solution, dilute to obtain 10 Ag nano wire/μ L Ag nanowire suspensions by suspension.Passing through will
Fluid is added dropwise near electrode, and the defective Ag nano wire of trace band is placed in by fluid in the spontaneous method sprawled in metal surface
The side of electrode；Ag nano wire one end is placed on electrode by micromotion platform and atomic force microscope probe, the other end is placed in
Between electrode, as shown in Figure 1.
Test and comparison is carried out to the pattern of Ag nano wire defective locations after processing and primary morphology using atomic force microscope,
As shown in Figure 2.The surface undulation height of defective locations, as shown in Figure 3.Test result shows that load loads on Ag nano wire
After optical electric field, the defect of Ag nanowire tip position has obtained significant reparation, and Ag nanowire surface restores smooth.
Embodiment two:
1. clean sheet glass is cut into the sample of 2 × 3 cm, it is then immersed in sodium sulfate of polyethenoxy ether of fatty alcohol
In Solutions Solution, 35 DEG C of water bath sonicator 10min；Then ultrasound 15 in deionized water is impregnated after being rinsed 3 times with deionized water
min。
2. taking out sample, it is placed on 10 min of soak at room temperature in acetone soln, taking-up is rinsed 3 times with deionized water, and nitrogen is blown
It is dry, it is put into spare in drier.
3. the above-mentioned sample prepared is placed in ozone generating-device and handles 15min.
4. using magnetron sputtering instrument under conditions of sputtering current is 15mA, sputtering time 200s, in glass surface
Plate one layer of silverskin in face.
5. under the conditions of 300 DEG C, anneal sample 1h under nitrogen atmosphere protection, can be observed in glass surface after annealing
One layer of bright silverskin.
6. use diameter for 100 μm of probes, by be inscribed in sample surfaces prepare 120 μm of diameter to electrode.By Ag
Nano wire is scattered in ethanol solution, dilutes to obtain 15 Ag nano wire/μ L Ag nanowire suspensions by suspension.Pass through
Fluid is added dropwise near electrode, fluid sets the defective Ag nano wire of trace band in the spontaneous method sprawled in metal surface
In the side of electrode；Ag nano wire one end is placed on electrode by micromotion platform and atomic force microscope probe, the other end is set
Between electrode, as shown in Figure 1.
7. applying optical electric field, intensity of illumination 50mW/mm between electrode simultaneously2, electric field strength 300V/cm, time 80min.
Test and comparison is carried out to the pattern of Ag nano wire defective locations after processing and primary morphology using atomic force microscope,
As shown in Figure 2.The surface undulation height of defective locations, as shown in Figure 3.Test result shows that load loads on Ag nano wire
After optical electric field, the defect of Ag nanowire tip position has obtained significant reparation, and Ag nanowire surface restores smooth.
There are the Ag nano wires of notable defect using tip by the present invention, sprawl technique using simple fluid, pass through atom
Force microscope probe is stirred, and Ag nano wire is placed between Silver Electrode.
Surface reconditioning is carried out to the Ag nano wire sample between being placed at Silver Electrode by applying illumination and electric field simultaneously.
It can be observed that Ag nanowire surface is gradually smooth in reaction process, with the progress of reparation, nanowire surface is significant
Defect will be gradually smooth, finally disappear.
The defect for reaching 10 nm or so positioned at silver nanoparticle case depth can be repaired using the technology, the Ag after reparation receives
The surface topography of rice noodles is close to or up to primary morphology.
Present invention employs the technical process that Ag nanowire surface applies illumination combination electric field, heat build-up and electricity using LSP
The mode of field induction Ag nano wire surface layer phase change layer migration, proposes a kind of more effective metal Nano structure defect repair side
Method, the design and preparation process of this method provide new technology hand to improve metal Nano structure defect repair precision and efficiency
Section.
Claims (5)
1. one kind is based on plasmon effect electric field-assisted metal Ag nano wire itself pattern restorative procedure, it is characterised in that:
Apply illumination and electric field simultaneously and surface reconditioning is carried out to the Ag nano wire sample between being placed at Silver Electrode；Include the following steps:
A. clean sheet glass is cut into the sample of 2 × 3cm, is then immersed in sodium sulfate of polyethenoxy ether of fatty alcohol solution
In, 35 DEG C of water bath sonicator 5-10min；Then ultrasound 10-15min in deionized water is impregnated after being rinsed 3 times with deionized water；
B. sample is taken out, soak at room temperature 5-10min in acetone soln is placed on, is taken out, is rinsed repeatedly with deionized water, nitrogen is blown
It is dry, it is put into spare in drier；
C. the above-mentioned sample prepared is placed in progress room temperature processing in ozone generating-device；
D. using magnetron sputtering instrument under conditions of sputtering current is 15-20mA, sputtering time 150-200s, in glass table
Plate one layer of silverskin in face；
E. under nitrogen atmosphere protection, under the conditions of 250-300 DEG C, anneal sample 0.5-1h；
F. it uses diameter for 100 μm of probes, 80-120 μm of diameter of electrode is prepared by being inscribed in sample surfaces, passes through fine motion
Ag nano wire one end is placed on electrode by platform and atomic force microscope probe, and the other end is placed between electrode.
2. restorative procedure according to claim 1, it is characterised in that: further include step g, apply photoelectricity simultaneously between electrode
, intensity of illumination 50-100 mW/mm2, electric field strength 300-1000 V/cm, 40-80 min of time.
3. restorative procedure according to claim 1, it is characterised in that: further include step h, using atomic force microscope to place
The pattern of Ag nano wire defective locations and primary morphology carry out test and comparison after reason.
4. restorative procedure according to claim 1, it is characterised in that: the step c must use ozone generating-device, often
Temperature processing 15-30min.
5. restorative procedure according to claim 1, it is characterised in that: the step f uses diameter for 100 μm of probes, leads to
Cross be inscribed in sample surfaces prepare 80-120 μm of diameter to electrode, disperse Ag nano wire in ethanol solution, by outstanding
Turbid dilutes to obtain 10-15 root Ag nano wire/μ L Ag nanowire suspension, by the way that fluid to be added dropwise near electrode, fluid
In the spontaneous method sprawled in metal surface, the defective Ag nano wire of trace band is placed in the side of electrode；Pass through micromotion platform
Ag nano wire one end is placed on electrode with atomic force microscope probe, the other end is placed between electrode.
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| CN107538012A (en) * | 2017-07-17 | 2018-01-05 | 哈尔滨工业大学深圳研究生院 | A kind of nano wire or nano-device and the metallurgical method being connected of nano metal electrode |
| CN113634743B (en) * | 2021-08-04 | 2022-08-26 | 湖南大学 | Ostwald nano welding method |
| CN114150197B (en) * | 2021-11-11 | 2022-09-13 | 烟台南山学院 | Physical contact rapid reversible color change liquid metal composite material and application thereof |
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| US20030048619A1 (en) * | 2001-06-15 | 2003-03-13 | Kaler Eric W. | Dielectrophoretic assembling of electrically functional microwires |
| DE102006043386A1 (en) * | 2006-09-11 | 2008-03-27 | Technische Universität Dresden | Electrical features improvement method for nano-electronic structure, involves arranging nanoelectronic structure between two electrodes, applying metallic salt solution on nanowires and nanotubes |
| CN101704503B (en) * | 2009-04-30 | 2015-11-25 | 中国计量学院 | A kind of method of one-dimensional nano material graft controlledly synthesis |
| US20120228013A1 (en) * | 2011-03-07 | 2012-09-13 | Endicott Interconnect Technologies, Inc. | Defective conductive surface pad repair for microelectronic circuit cards |
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| CN101591004A (en) * | 2009-06-26 | 2009-12-02 | 厦门大学 | A kind of method for modifying and processing of amorphous silicon oxide nano wire |
| CN101591003A (en) * | 2009-06-26 | 2009-12-02 | 厦门大学 | A kind of electron beam focusing radiation processing method of amorphous silicon oxide nano wire |
| CN101602484A (en) * | 2009-06-26 | 2009-12-16 | 厦门大学 | A kind of welding method of amorphous silicon oxide nano wire |
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