CN106350847B - It is a kind of that Fe is patterned using laser interference induction electrochemical deposition manufacturing cycle3O4The method of nanoparticle - Google Patents
It is a kind of that Fe is patterned using laser interference induction electrochemical deposition manufacturing cycle3O4The method of nanoparticle Download PDFInfo
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Abstract
Fe is patterned using laser interference induction electrochemical deposition manufacturing cycle the present invention relates to a kind of3O4The method of nanoparticle uses laser interference light source using light-induction dielectrophoresis and electrochemical deposition technique to induce light source, to be coated with the ITO conductive substrates of hydrogenation non crystal silicon film as working electrode, saturated calomel electrode is used as reference electrode, high-purity iron plate to electrode, with FeCl2And FeCl3Mixed solution as electrolyte, exposed portion will be made to generate dummy electrodes using photoelectric effect on induction light sources project to hydrogenation non crystal silicon film.Using chronoamperometry in the electrochemical deposition on dummy electrodes, Fe is generated3O4Nanoparticle obtains and the consistent orderly Fe of laser interference pattern3O4Nano particles array.The present invention is prepared for the periodic Fe of large area3O4Nano particles array, equipment is simple, and preparation cost is low, and without high-temperature heating or annealing, the chemicals used is nontoxic, the orderly Fe of the patterning of preparation3O4Nano particles array favorable reproducibility, it is with good stability.
Description
Technical field
Periodic patterning orderly Fe is realized using laser interference induction electrochemical deposition the present invention relates to a kind of3O4Nanometer
The preparation method of array of particles, belongs to technical field of nanometer material preparation.
Background technique
In nature, there are many forms for ferriferous oxide.Magnetic iron ore (Fe3O4) and maghemite (γ-Fe2O3) by
Researcher extensive concern, especially Fe3O4Due to nano-scale, high surface area/volume ratio, superparamagnetism, being easy
Synthesis, surface be easy improvement, hypotoxicity, the biocompatibility that chemical stability is good, good, magnetic recording, catalysis, biological medicine,
There is huge application prospect in terms of biotechnology, sewage treatment.If being superscribed again in its periphery certain with functional groups
Polymer, so that it may have good application in terms of the detection separation of field of medicaments especially cancer cell.People send out in recent years
Now it is less than the Fe of 15nm3O4Nanoparticle has the characteristics that superparamagnetism, this feature is allowed it to as magnetic target substance
Recyclable catalyst is either generated in conjunction with catalyst applied to biological medicine, these application notes study Fe3O4Nanoparticle
Son has critically important scientific meaning and application value.Therefore, Fe3O4The controllable preparation of nanoparticle applies valence with important
Value.
At present about magnetic Fe3O4The preparation method of nanoparticle has very much, is divided into physical method and chemical method, physical method by
It is distributed the disadvantages of coarse in the nano particle diameter of its preparation, prepared nano material can not meet people to its performance study
With the needs of material fining application, therefore people more focus on the preparation of chemical method now, and common chemical method has the precipitation method, micro-
Emulsion method, solvent-thermal method, organic precursor thermal decomposition method and hydro-thermal method etc..
Light-induction dielectrophoresis (Optically induced Dielectrophoresis, ODEP) is also known as photoelectron tweezer
(Optoelectronic Tweezers, OET) is proposed by Pei Yu Chiou group, is a kind of by optical electrode and dielectrophoresis
The novel manipulation technology that method combines.By using for reference optical electrode in the application in xerography field, optics electricity is utilized for the first time
Pole replaces traditional physical electrode, to electrode design and comes into operation from determining operating function, and the period is extremely short, avoids complexity
Electrode production process improves particle manipulation flexibility and reduces processing cost.Due to can produce dynamic optical dummy electrodes,
It realizes the manipulation more complicated to particle, has widened the manipulation thinking of traditional dielectric swimming, there is wide researching value and application
Prospect.Amorphous silicon hydride (Hydrogenated Amorphous Silicon, a-Si:H) film is as crystalline silicon (c-Si)
A kind of derived material has superior photoelectric characteristic, is a kind of important semiconductor material, is widely used in solar battery
With the opto-electronic devices such as thin film transistor (TFT) (a-Si:H TFT) in liquid crystal display, and main photo-conductive film material at present
Material, is used for the electrode of light-induction dielectrophoresis technology.
Present invention combination light-induction dielectrophoresis and electrochemical deposition technique are induction light source using laser interference light source, with
The ITO conductive substrates for being coated with amorphous silicon hydride (a-Si:H) film are working electrode, by induction light sources project in amorphous silicon hydride
(a-Si:H) dummy electrodes are generated on film, generates Fe on dummy electrodes with electrochemical deposition technique3O4Nanoparticle is realized
With the consistent periodic patterning Fe of laser interference pattern3O4Nano particles array preparation.It overcomes the deficiencies of the prior art and provide
A kind of orderly Fe efficient, convenient, pattern is controllable3O4The technology of preparing of nano particles array, to promote related nano material system
The development of standby technology.
Summary of the invention
The purpose of the present invention is overcome the deficiencies of the prior art and provide a kind of periodic patterning Fe3O4Nano particles array
Preparation method.The present invention is induction light source using laser interference light source, to be coated with the ITO of amorphous silicon hydride (a-Si:H) film
Conductive substrates are working electrode, and induction light sources project is generated dummy electrodes on amorphous silicon hydride (a-Si:H) film, is passed through
Simple electrochemical deposition method generates Fe on dummy electrodes3O4Nanoparticle is prepared and laser interference pattern consistent week
Phase property Fe3O4Nano particles array is orderly Fe3O4The preparation of nano particles array provide a kind of simple equipment, low cost,
Efficient preparation method.
The invention mainly includes steps:
(1) prepare electrode: surface is coated with amorphous silicon hydride (a-Si:H) film ITO conductive substrates as working electrode；
Using high-purity iron plate as to electrode；Using calomel electrode as reference electrode.
(2) it prepares electrolyte: using Iron(III) chloride hexahydrate as ferric iron source, preparing the FeCl of 12mM3Deionization it is water-soluble
Liquid 50ml prepares the FeCl of 8mM using four hydration ferrous chloride as divalent source of iron2Deionized water solution 50ml；Respectively to two kinds
Solution carries out ultrasonic dissolution, and ultrasonic dissolution again after mixing obtains electrolyte solution.
(3) build electrochemical deposition system: it is the rectangular of 150ml that the 100ml electrolyte that step (2) are prepared, which is placed in capacity,
In quartz beaker, and the three-phase electrode that step (1) prepares is soaked in electrolyte, ITO electrode is placed in outermost, and will not
Plated film side is coated with amorphous silicon hydride (a-Si:H) film towards beaker inside towards walls of beaker.
(4) it builds laser interference system and introduces induction light source: the laser interference light source of appropriate wavelength is selected, according to expection
Pattern period builds laser interference system, obtains periodic patterns induction light source, and light source is introduced on ITO working electrode,
Adjustment optical path makes that light source is induced to be projected in amorphous silicon hydride (a-Si:H) the film back side through beaker, solution and ITO substrate, adjusts
Laser power density generates dummy electrodes.
(5) setting electrochemical workstation parameter carries out electrochemical deposition: at room temperature, using CHI660D electrochemical workstation
It controls cathode-current density and sedimentation time carries out electrochemical deposition, after operation, close power supply and take out working electrode, use deionization
Water flushes three times, and naturally dry is at room temperature to get consistent with laser interference pattern on hydrogenation non crystal silicon film to being attached to
Periodical Fe3O4 nano particles array.
The surface is coated with amorphous silicon hydride (a-Si:H) film ITO conductive substrates as working electrode, and wherein ITO is led
The sheet resistance of electric substrate is 4-5 Ω, and ito thin film is with a thickness of 200-1000nm, transmitance 80-100%；Amorphous silicon hydride (a-Si:
H) film is that PECVD method is deposited on the surface ITO, with a thickness of 100-1000nm, dark-state conductivity >=5E-10S/cm, AM1.5G
Light state conductivity >=7E-5S/cm under illumination condition.Ito thin film edge is covered using mask plate in deposition process, reserves 1-
The ITO of 5mm width not deposition of hydrogenated amorphous silicon (a-Si:H) film, is used as lower conductive electrode.
The electrolyte is FeCl3And FeCl2Mixed solution, FeCl3With FeCl2Molar ratio be 3:2.
The laser interference optical source wavelength is 400-700nm, power density 1-20mW/cm2。
The induction light source is that laser issues the light source with periodical interference figure formed by interference system, is done
The characteristic size of pattern is related to from nanoscale to micrometer-adjustable.
The dummy electrodes are that the photoelectricity generated when inducing light sources project to the film back side amorphous silicon hydride (a-Si:H) is imitated
The exposed portion of amorphous silicon hydride (a-Si:H) film should be made to generate a large amount of photo-generated carriers and impedance reduction, to generate virtual
Electrode.
The model CHI660D of the electrochemical workstation, during sedimentation experiment carries out, electrolyte is in quiet always
Only state, deposition parameter refer to sedimentation time (1-200S, optimization sedimentation time are 50s), depositing current density (1-10mA/cm2)、
Laser power density (1-20mW/cm2)。
The Fe3O4The various forms and size of nanoparticle are controlled by the parameter deposited: it is straight that sedimentation time controls particle
Diameter size；The form of laser power density control particle.
Electrolysis of all hydroxyls all from water needed for the electrochemical deposition process.
The reaction of the electrochemical deposition process can be used following chemical equation to indicate: 2H2O+2e?→H2+2OH? Fe2 ++2Fe3++8OH-=Fe3O4+4H2O
The present invention has the advantage that compared with the conventional method
(1) electrochemical in-situ sedimentation is used, equipment is simple；
(2) preparation cost is cheap, raw material is easy to get；
(3) Fe prepared3O4Nano particle diameter and shape can be controlled by deposition parameter.
(5) Fe prepared3O4Nanoparticle is distributed in cyclic array pattern, and pattern period can be by controlling laser interference
The parameter of system is adjusted, efficient, convenient.
Detailed description of the invention
Fig. 1 is that laser interference of the invention induces electrochemical deposition manufacturing cycle to pattern Fe3O4The process of nanoparticle
Figure；
Fig. 2 is system schematic of the invention；
Fig. 3 is that two beam interference laser interference system schematic diagrames and formation wiregrating induce light source hot spot figure；
Fig. 4 is the patterning periodicity Fe of two beam interferences preparation3O4The SEM of nano particles array schemes；
Fig. 5 is the partial size Fe different with form3O4Nanoparticle SEM figure；
Fig. 6 is the Fe of preparation3O4The X ray diffracting spectrum of nanoparticle.
Specific embodiment
The present invention will be described in detail With reference to embodiment.
As shown in Figure 1, the present invention is using simple laser interference induction electrochemical deposition preparation patterning Fe3O4Nanoparticle
The method of son is as follows:
(1) prepare electrode: surface is coated with amorphous silicon hydride (a-Si:H) film ITO conductive substrates as working electrode；
Using high-purity iron plate as to electrode；Using calomel electrode as reference electrode.Wherein the surface area of ITO conductive substrates is 1cm2, side
Resistance is 4 Ω, and ito thin film is with a thickness of 500nm, transmitance 84%；Amorphous silicon hydride (a-Si:H) film is PECVD method deposition
On the surface ITO, with a thickness of 500nm, dark-state conductivity is 5E-10S/cm, and the light state conductivity under AM1.5G illumination condition is about
7E-5S/cm.Wherein the edge ITO reserves the ITO of 2mm width not deposition of hydrogenated amorphous silicon (a-Si:H) film, is used as down leading
Electrode.
(2) it prepares electrolyte: using Iron(III) chloride hexahydrate as ferric iron source, preparing the FeCl of 12mM3Deionization it is water-soluble
Liquid 50ml prepares the FeCl of 8mM using four hydration ferrous chloride as divalent source of iron2Deionized water solution 50ml；Respectively to two kinds
Solution carries out ultrasonic dissolution, and ultrasonic dissolution again after mixing obtains electrolyte solution, FeCl3With FeCl2Molar ratio be 3:2.
(3) it builds electrochemical deposition system: the 100ml electrolyte that (2) are prepared is placed in the rectangular quartz that capacity is 150ml
In beaker, and step (1) preparation three-phase electrode is soaked in electrolyte, ITO electrode is placed in outermost, and will non-plated film one
Side is coated with amorphous silicon hydride (a-Si:H) film towards beaker inside towards walls of beaker.As shown in Fig. 2, being system of the invention
Including electrochemical workstation 1, computer 2, laser light source 3, interference system 4, the ITO for being coated with amorphous silicon hydride (a-Si:H) film
Electrode 5, calomel electrode 6, high-purity iron plate 7, FeCl3And FeCl2Solution 8.Electrochemical workstation 1 is connect with computer 2, laser light
Source 3 is incident in interference system 4, and the ITO electrode 5 of amorphous silicon hydride (a-Si:H) film, calomel electrode 6 and high-purity will be coated with
Iron plate 7 is placed in FeCl3 and FeCl2 solution 8, at the same by the cathode of electrochemical workstation 1 and be coated with amorphous silicon hydride (a-Si:
H) ITO electrode 5 of film connects, and reference electrode is connect with calomel electrode 6, positive to connect with high-purity iron plate 7.
(4) it builds laser interference system and introduces induction light source: selecting 457nm wavelength laser as interference light source, build 5
μm period wiregrating laser interference system obtains 5 μm of period wiregratings induction light sources, and light source is introduced on ITO working electrode,
Adjustment optical path makes that light source is interfered to be projected on amorphous silicon hydride (a-Si:H) film through beaker, solution and ITO substrate.Induce light
Source, which is projected in the photoelectric effect generated when the film back side amorphous silicon hydride (a-Si:H), makes amorphous silicon hydride (a-Si:H) film
Exposed portion generates a large amount of photo-generated carriers and impedance reduces, to generate the wiregrating dummy electrodes that the period is 5 μm.
As shown in the left figure of Fig. 3, two beam interferences of the invention realize Fe3O4The laser interference system of nano particles array preparation
System schematic diagram.The laser interference system of use forms beam splitting system by high reflective mirror, spectroscope.By laser issue beam of laser by
Beam splitter is divided into two beam coherent beams, makes two beam coherent light space symmetrs through catoptric system, and make them with certain incidence angle
It is irradiated on amorphous silicon hydride (a-Si:H) film simultaneously, 5 μm of wiregrating induction light sources is formed, as shown in Fig. 3 right figure.
(5) setting electrochemical workstation parameter carries out electrochemical deposition: at room temperature, using CHI660D electrochemical workstation
Control cathode-current density 2mA/cm2Respectively in condition 1) sedimentation time 50s and laser power density 2mW/cm2；2) when depositing
Between 100s and laser power density 5mW/cm2；3) sedimentation time 200s and laser power density 10mW/cm2；It is heavy to carry out electrochemistry
Product, after operation, close power supply take out working electrode, flushed three times with deionized water, at room temperature naturally dry, obtain print 1,
2 and 3.
(6) with scanning electron microscope SEM test sample 1 to get to the period being attached on hydrogenation non crystal silicon film be 5
μm nanoparticle wiregrating.As shown in figure 4, for the wire grid pattern Fe of two beam interferences preparation3O4The SEM of nano particles array schemes,
Left figure is large area periodicity wiregrating distribution map, and right figure is multicycle wiregrating enlarged drawing.The periodical wiregrating figure that visible deposition goes out
Case Fe3O4The nano particles array period is 5 μm and induces light source with 5 μm of wiregrating stripeds that Fig. 3 double light beam laser interference system is formed
Unanimously.
(7) it with the nanoparticle in scanning electron microscope SEM test sample 1,2 and 3, obtains as shown in figure 5, for partial size
The Fe different with form3O4Nanoparticle SEM figure, wherein left figure print 1 is hexahedron and triangular pyramid；Middle pattern piece 2 is snowflake
Shape；Right figure print 3 is scale stratiform, as sedimentation time is from 50s-200s, laser power density from 2mW/cm2-10mW/cm2
Variation, prepared Fe3O4Particle diameter becomes larger, and form changes.
(8) X-ray diffractometer test sample 1 is used, as shown in fig. 6, being the X ray diffracting spectrum of deposited samples, abscissa 9
For 2 angles θ (degree), ordinate 10 is intensity.Wherein four main peaks and Fe3O4Standard diagram is consistent, determines that nanoparticle main ingredient is
Fe3O4。
Claims (6)
1. a kind of pattern Fe using laser interference induction electrochemical deposition manufacturing cycle3O4The method of nanoparticle, feature
It is: is induction light source using laser interference light source, to be coated with the ITO conductive substrates of amorphous silicon hydride (a-Si:H) film as work
Make electrode, by induction light sources project on amorphous silicon hydride (a-Si:H) film, to generate dummy electrodes, is situated between using photoinduction
Electrophoresis and electrochemical deposition technique, generate Fe on dummy electrodes3O4Nanoparticle, is realized and laser interference pattern is consistent has
Sequence patterns Fe3O4Nano particles array preparation；
The laser interference optical source wavelength is 400-700nm, power density 1-20mW/cm2；
The ITO conductive substrates to be coated with amorphous silicon hydride (a-Si:H) film is working electrodes, wherein ITO conductive substrates
Sheet resistance be 4-5 Ω, with a thickness of 200-1000nm, transmitance 80-100%；Amorphous silicon hydride (a-Si:H) film is PECVD
Method is deposited on the surface ITO, with a thickness of 100-1000nm, dark-state conductivity >=5E-10S/cm, and the light under AM1.5G illumination condition
State conductivity >=7E-5S/cm, covers ito thin film edge using mask plate in deposition process, and the ITO for reserving 1-5mm width does not sink
Product amorphous silicon hydride (a-Si:H) film, is used as lower conductive electrode；
The Fe3O4The various forms and size of nanoparticle are controlled by deposition parameter: it is big that sedimentation time controls particle diameter
It is small, sedimentation time 1-200s；Laser power density controls particle shape, laser power density 1-20mW/cm2。
2. according to the method described in claim 1, it is characterized by: the Fe3O4The various forms and size of nanoparticle are by sinking
Parameter is accumulated to control: sedimentation time controls particle diameter size, sedimentation time 50s.
3. according to the method described in claim 1, it is characterized by: the induction light source is that laser is issued by interference system
What is formed has the light source of periodical interference figure, and the characteristic size of interference figure is from nanoscale to micrometer-adjustable.
4. according to the method described in claim 1, it is characterized by: the dummy electrodes are induction light sources project to hydrogenated amorphous
It is a large amount of that the photoelectric effect generated when the film back side silicon (a-Si:H) generates the exposed portion of amorphous silicon hydride (a-Si:H) film
Photo-generated carrier and impedance reduction, to generate dummy electrodes.
5. according to the method described in claim 1, it is characterized by: all hydroxyls needed for the electrochemical deposition process
All from the electrolysis of water.
6. according to the method described in claim 1, it is characterized by: described generate orderly Fe on dummy electrodes3O4Nanoparticle
Array pattern is consistent with laser interference pattern.
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| CN108226095B (en) * | 2017-12-27 | 2020-09-08 | 南京大学 | Electrochemical impedance spectrum measuring device and method for single nano particle |
| CN109970023A (en) * | 2017-12-28 | 2019-07-05 | 中国科学院沈阳自动化研究所 | A kind of manufacturing method of flexible micro-electrode |
| CN109119332B (en) * | 2018-07-30 | 2022-07-22 | 长春理工大学 | Method for preparing patterned ordered bimetal nanoparticle array by adopting annealing method |
| CN110284160B (en) * | 2019-08-14 | 2021-03-23 | 吉林大学 | Photoinduction metal electrochemical 3D printing device and method |
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| Electrochemical synthesis of Fe3O4 nanoparticles in alkaline aqueous solutions containing complexing agents;S. Franger et al.;《J Solid State Eletrochem》;20140213;第8卷;摘要 |
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