CN106350846B - Prepared by a kind of electrochemical deposition patterns orderly α-Fe2O3The method of nano particles array - Google Patents
Prepared by a kind of electrochemical deposition patterns orderly α-Fe2O3The method of nano particles array Download PDFInfo
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y40/00—Manufacture or treatment of nanostructures
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
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Abstract
Prepared by a kind of electrochemical deposition patterns orderly α Fe2O3The method of nano particles array, using electrochemical workstation, using the ITO conductive substrates after laser interference lithography as working electrode, saturated calomel electrode is as reference electrode, and high-purity iron plate is used as to electrode, with FeCl2And FeCl3Mixed solution as electrolyte, using three-phase electrode system, be immersed in electrolyte simultaneously by working electrode, to electrode, reference electrode, setting required temperature carries out electrochemical deposition.Using chronoamperometry, electrochemical deposition obtains the orderly α Fe of patterning with good dispersion on the working electrode (s2O3Nano particles array.The present invention carries out prepatterned using the exposure of dual-beam list to electrode, is prepared for the nano particles array of large area pattern ordered structure.Using cathodic electrodeposition in electrochemical deposition process, equipment is simple, and manufacturing cost is low, and without being heated at high temperature or making annealing treatment, the chemicals used is nontoxic, the orderly α Fe of prepared patterning2O3Nano particles array favorable reproducibility, it is with good stability.
Description
Technical field
The present invention relates to a kind of prepared using electrochemical deposition to pattern orderly α-Fe2O3The method of nano particles array belongs to
In technical field of nanometer material preparation.
Background technology
This newborn subject of the nanosecond science and technology that have been born in 20th century, nanometer science and technology be one on nanoscale,
Research molecule, atom and the cross discipline of electron motion rule and feature, the final goal that human research develops this subject are
Explore microcosmos and the demand direct operation or the single atom of control according to itself.Nanosecond science and technology have just received since proposition
The extensive concern of scientist is rapidly developed in short decades.Branch of the nanomaterial science as nanosecond science and technology,
Become forward position and the hot spot of scientific research, wherein iron oxygen due to its significance in theory and application upper great potential
Compound nano-particle is widely applied due to its good biocompatibility and hypotoxicity in biomedical sector.Iron aoxidizes
Object is distributed widely in all over the world, and there are the ferriferous oxides of different content in soil, rock, water and organism etc..Iron aoxidizes
Object is that presence is the most extensive, one of most compound of reserves, as important chemical raw material cheap and easy to get, in industry, doctor
Medicine and new energy development and many other key areas have a wide range of applications.
Iron oxide nanoparticle mainly includes Fe3O4、α-Fe2O3、γ-Fe2O3、ε-Fe2O3Deng, they not only have it is general
Skin effect, quantum size effect, bulk effect and the macro quanta tunnel effect that logical nano-particle has, also with super suitable
The characteristics such as magnetic, high-coercive force and low Curie temperature.Due to these unique physicochemical properties, iron oxide nanoparticle exists
Magnetic recording media, cell separation, tumor thermotherapy, Magnetic resonance imaging, targeted drug, photocatalysis, lithium ion battery negative material,
The research fields such as ultracapacitor, environmental protection are in occupation of very important status.
Iron oxide nanoparticle is in practical applications also there are many yet unresolved issues, for example, Fe3O4Magnetism is received
Rice corpuscles is easily reunited due to its magnetic and larger surface energy, is limited its practical application, therefore, it is necessary to nano-particle
It carries out surface to be modified and modify, reduces the generation of agglomeration, could preferably adapt to the developing direction of nanomaterial science.Three oxygen
Change two iron as a kind of very easy semiconductor that obtains and can be stabilized, in photocatalysis, organic matter absorption, lithium ion
Important application is suffered from terms of battery, especially in this field of lithium ion battery negative material, di-iron trioxide occupies
Very important status.Di-iron trioxide is corundum type structure, and energy gap 2.2eV has very strong under visible light
Absorption spectrum is a kind of important n-type semiconductor.Due to di-iron trioxide, property is stablized at room temperature, and synthesis cost is low
It is honest and clean, the advantages that resistance to corrosion is strong, and environmental pollution is small, it is widely used in magnetic recording media, it is ferritic to prepare raw material etc..It receives
The di-iron trioxide of meter ruler cun makes it in the chemically due to having many advantages, such as that the large specific surface area of nano material, size are small
Better than di-iron trioxide bulk material, the chemical property of nanometer di-iron trioxide is more stable, catalytic activity is high, light resistance is good and right
Ultraviolet light has shielding.Nanometer di-iron trioxide be widely used in chemical catalysis, photocatalysis, environmental treatment, lithium ion battery,
Super capacitor material and clinical treatment etc..Fe2O3Nano-particle is urged as important lithium ion battery negative material and light
Agent, it is desirable that itself with good stability and catalytic activity, so the property of ferriferous oxide nano material and pattern are
One of important content through becoming scientific research.
Invention content
The purpose of the present invention is overcome the deficiencies of the prior art and provide a kind of electrochemical deposition prepare pattern orderly α-
Fe2O3The method of nano particles array.The present invention, using three-phase electrode system, passes through letter using CHI660D electrochemical workstations
Single cathode electrochemical in-situ deposition method prepares the α-Fe with good dispersion and stability2O3Nano particles array is
α-Fe2O3The preparation of nano particles array provides a kind of simple equipment, low cost, efficient preparation method.
The present invention is using chronoamperometry, and deposition has fine dispersion in the ITO conductive substrates after laser interference lithography
α-the Fe of property2O3Prepared by nano-particle patterns orderly nano particles array, mainly includes the following steps that：
(1) cleaning of electrode：ITO conductive substrates are sequentially placed into acetone, absolute ethyl alcohol, deionized water and carry out ultrasound clearly
It washes, it is dry after taking-up, as working electrode；High-purity iron plate (purity range of high-purity iron plate is 99.9%-99.99%) is carried out
It is cleaned by ultrasonic, it is dry after taking-up, as to electrode；Working electrode after cleaning forms three-phase electricity polar body to electrode, reference electrode
System；
(2) prepatterned of electrode：Double light beam laser optical interference circuit system is built, carrying out laser to the ITO cleaned does
Relate to photoetching；
(3) electrolyte quota：Electrolyte is prepared with ferric trichloride, ferrous chloride, deionized water, is stirred continuously until trichlorine
After change iron and ferrous chloride are completely dissolved, which is sealed spare；
(4) electrochemical deposition：Using three-phase electrode system, the ITO conductive substrates of gained are electric as work using in step (2)
Pole, using high-purity iron plate as to electrode, using saturated calomel electrode as reference electrode；The electrolyte that step (3) is prepared is placed in
In electrolytic cell, electrolyte is made uniformly to be soaked in three-phase electrode system, set required temperature, use electrochemical operation stand control cathode
It after current density and sedimentation time carry out electrochemical deposition operation, closes power supply and takes out working electrode, rinsed with deionized water dry
Only, it dries at room temperature to get to the α-Fe being attached in ITO substrate2O3Nano-particle.
Two beam laser interference systems in the step (2) are made of laser, beam splitting, refractive power and orthopedic systems, by
Laser sends out beam of laser, is divided into two beam coherent beams through divided beam system, divided beam system is by high reflective mirror, spectroscope, half-wave
Piece and polarizer group through dioptric system into making two beam coherent light space symmetrs, orthopedic systems converge at sample in two light beams and advance
Row beam shaping makes them be irradiated on sample simultaneously with certain incidence angle, changes two beam spatial light interferometric parameters, parameter packet
Space Angle, incidence angle, phase angle, polarization state, interference light intensity and time for exposure etc. are included, interferes two beam laser interference systems
The characteristic size of pattern is from nanoscale to micrometer-adjustable, so as to which interference obtains different cycles on ITO conductive substrates surface
Optical grating construction.
In the step (3), electrolyte is by FeCl3And FeCl2Mixed solution composition, and in electrochemical deposition process
Electrolyte remains static always.
The electrolyte quota process：Using ferric trichloride as ferric iron source, the FeCl of 4-16mM is prepared3Deionization it is water-soluble
Liquid using ferrous chloride as divalent source of iron, prepares the FeCl of 6-24mM2Deionized water solution；Two kinds of solution of ultrasonic dissolution respectively,
Ultrasonic dissolution again after mixing, obtains clear electrolyte.
The electrochemical deposition process, sedimentation time 1-200s, depositing temperature are 16.5-60 DEG C, and deposition current is
1-10 mA/cm2。
Orderly α-the Fe of patterning of the electrochemical deposition2O3Nano particles array has good on ITO conductive substrates surface
Good adhesion, nano-particle are uniformly dispersed, and agglomeration will not occur.
In the electrochemical deposition process working electrode and to interelectrode vertical operation distance be 3-10cm.
All hydroxyls are all from the electrolysis of water needed for the electrochemical deposition process.
α-the Fe of the electrochemical deposition2O3Nano-particle can uniformly be scattered in deionization by the method for ultrasound
In water.
Laser output wavelength used is 1064nm, and Gauss beam reshaping is into uniform beam, laser energy density
0.42J/cm2。
The electrode is using surface area as 1cm2ITO conductive substrates as working electrode, be immersed in saturation KCl solution
Saturated calomel electrode as reference electrode, high-purity iron plate after sand paper grinding process is used as to electrode.
The electrolyte is FeCl3And FeCl2Mixed solution, FeCl3With FeCl2Molar ratio be 3:2.
The model CHI660D of the electrochemical workstation, during sedimentation experiment carries out, electrolyte is always in quiet
Only state, deposition parameter refer to sedimentation time, reaction temperature, depositing current density, concentration of electrolyte, and temperature is filled using magnetic agitation
Included temperature controlling instruments is put to be controlled.
α-the Fe of the electrochemical deposition2O3Nano particles array has good dispersibility, has on ITO substrate surface
There is good adhesion, agglomeration will not occur.
α-the Fe2O3The grain size and shape of nano-particle can be controlled by deposition parameter.
The sheet resistance of the ITO conductive substrates be 8 Ω, thickness 0.7mm, transmitance 84%.
All hydroxyls are all from the electrolysis of water needed for the electrochemical deposition process.
The cathode reaction of the electrochemical deposition process can be used following chemical equation to represent：
2H2O+2e→H2+2OH
4Fe3++3O2+12e→2Fe2O3
4Fe2++3O2+6H2O→4Fe(OH)3
The anode reaction of the electrochemical deposition process can be used following chemical equation to represent：
Fe2+- e→Fe3+
Fe3++3OH→Fe(OH)3
2Fe(OH)3→Fe2O3+3H2O
The present invention has the advantage that compared with the conventional method：
(1) using electrochemical in-situ sedimentation, equipment is simple；
(2) manufacturing cost is cheap, raw material is easy to get；
(3) reaction condition is mild, the α-Fe of preparation2O3Nano-particle has good dispersibility；
(4) α-Fe prepared2O3Nano particle diameter and shape can be controlled by deposition parameter.
(5) α-Fe prepared2O3The period of nano particles array can be adjusted by the parameter of laser interference lithography.
Electrochemical deposition technique is applied to pattern the preparation aspect of orderly nano particles array by the present invention, is overcome existing
The deficiency of technology, provide a kind of efficient, convenient, regular appearance, structure-controllable α-Fe2O3The preparation skill of nano particles array
Art, to promote the development of related nano material preparation technology.
Description of the drawings
Fig. 1 is the preparation flow figure of the present invention；
Fig. 2 is that the present invention realizes the system schematic for patterning orderly nano particles array and preparing using two beam interferences；
Fig. 3 is the electrochemical deposition experimental provision schematic diagram of the present invention；
Fig. 4 is the X ray diffracting spectrum of the orderly nano particles array of patterning prepared, and abscissa is X ray incidence angle
Twice of degree, ordinate are the intensity of X ray；
Fig. 5 is the orderly α-Fe of patterning prepared by two beam interferences2O3The SEM figures of nano particles array.Wherein figure (a) is
Orderly α-Fe when amplification factor is 2500 times2O3The SEM figures of nano particles array, (b) is amplification factor when being 5000 times orderly α-
Fe2O3The SEM figures of nano particles array, (c) is amplification factor orderly α-Fe when being 10000 times2O3The SEM of nano particles array
Figure, (d) is amplification factor orderly α-Fe when being 20000 times2O3The SEM figures of nano particles array.
Specific embodiment
The present invention will be described in detail With reference to embodiment.
The present invention is using electrochemical workstation, using the ITO conductive substrates after laser interference lithography as working electrode, saturation
Calomel electrode is as reference electrode, and high-purity iron plate is used as to electrode, with FeCl2And FeCl3Mixed solution as electrolyte, adopt
It with three-phase electrode system, is immersed in electrolyte simultaneously by working electrode, to electrode, reference electrode, setting required temperature carries out
Electrochemical deposition.Using chronoamperometry, electrochemical deposition obtains having the patterning of good dispersion orderly on the working electrode (s
α-Fe2O3Nano particles array.
The present invention carries out prepatterned using the exposure of dual-beam list to electrode, is prepared for large area pattern ordered structure
Nano particles array.Using cathodic electrodeposition in electrochemical deposition process, equipment is simple, and manufacturing cost is low, without high temperature
Heating or annealing, the chemicals used is nontoxic, the orderly α-Fe of prepared patterning2O3Nano particles array weight
Existing property is good, with good stability.
The present invention is prepared using simple electrochemical in-situ deposition method and patterns orderly α-Fe2O3Nano particles array, such as
Shown in Fig. 1, include the following steps：
(1) electrode is cleaned by ultrasonic：It is 1cm by surface area2ITO conductive substrates be respectively placed in acetone, anhydrous second
It is cleaned by ultrasonic in alcohol, deionized water, each 180s, it is dry after taking-up, as working electrode；After high-purity iron plate is polished with sand paper
It is cleaned by ultrasonic 180s, it is dry after taking-up, as to electrode；By the calomel electrode being immersed in saturation KCl solution take out, spend from
Sub- water flushes three times, as reference electrode.
(2) prepatterned of electrode：Double light beam laser optical interference circuit system is built, carrying out laser to the ITO cleaned does
Relate to photoetching.
(3) electrolyte is prepared：Using Iron(III) chloride hexahydrate as ferric iron source, the FeCl of 12mM is prepared3Deionization it is water-soluble
Liquid 50ml using four hydration ferrous chloride as divalent source of iron, prepares the FeCl of 8mM2Deionized water solution 50ml；Respectively to two kinds
Solution carries out ultrasonic dissolution, and ultrasonic dissolution again after mixing finally obtains clear electrolyte solution.
(4) setting electrochemical workstation parameter carries out electrochemical deposition：Using three-phase electrode system, with laser interference lithography
ITO conductive substrates afterwards are as working electrode, using high-purity iron plate as to electrode, using saturated calomel electrode as reference electrode into
Row electrochemical in-situ deposits；The 100ml electrolyte that step (3) is prepared is placed in the electrolytic cell that capacity is 150ml, is allowed to uniform
Three-phase electrode system is soaked in, is warming up to 16.5-60 DEG C；It is controlled using the chronoamperometry of CHI660D electrochemical workstations cloudy
Electrode current density is 1-10mA/cm2, after sedimentation time carries out electrochemical deposition operation for 1-200s, work is taken out after closing power supply
Make electrode, flushed three times with deionized water, after being dried at room temperature for, you can obtain the patterned pattern for being attached to ITO substrate
Change orderly α-Fe2O3Nano particles array ordered structure.
It is prepared as shown in Fig. 2, being patterned with sequence structure nano particles array for the two beam interferences realization that the present invention uses
System schematic.The laser interference system of use forms beam splitting system by high reflective mirror, spectroscope.It is sent out by laser (Laser)
Go out beam of laser, turned back light path by speculum, then two beam coherent beams are divided by divided beam system, divided beam system be by high reflective mirror,
Spectroscope, half-wave plate and polarizer group through dioptric system into making two beam coherent light space symmetrs, orthopedic systems are assembled in two light beams
Beam shaping is carried out before sample, them is made to be irradiated on sample simultaneously with certain incidence angle, forms grating fringe.
As shown in figure 3, the experimental provision schematic diagram for the present invention, using three-phase electrode system, with the ITO substrate after cleaning
For working electrode, the calomel electrode being immersed in saturation KCl solution is reference electrode, and high-purity iron plate is in FeCl to electrode3With
FeCl2Molar ratio 3：Electrochemical in-situ deposition is carried out in 2 mixed solution.
As shown in figure 4, the X ray diffracting spectrum for deposited samples, abscissa is twice of X ray incident angle, indulges and sits
It is designated as the intensity of X ray.
As shown in figure 5, the orderly α-Fe of patterning prepared for two beam laser interference lithographies2O3The SEM of nano particles array
Figure, wherein orderly α-Fe when figure (a) be amplification factor is 2500 times2O3The SEM figures of nano particles array, (b) is for amplification factor
Orderly α-Fe at 5000 times2O3The SEM figures of nano particles array, (c) is amplification factor orderly α-Fe when being 10000 times2O3Nanometer
The SEM figures of array of particles, (d) is amplification factor orderly α-Fe when being 20000 times2O3The SEM figures of nano particles array.
Claims (10)
1. prepared by a kind of electrochemical deposition pattern orderly α-Fe2O3The method of nano particles array, it is characterised in that including following
Step：
（1）The cleaning of electrode：ITO conductive substrates are sequentially placed into acetone, absolute ethyl alcohol, deionized water and are cleaned by ultrasonic,
It is dry after taking-up, as working electrode；High-purity iron plate is cleaned by ultrasonic, it is dry after taking-up, as to electrode；After cleaning
Working electrode forms three-phase electrode system to electrode, reference electrode；
（2）The prepatterned of electrode：Double light beam laser optical interference circuit system is built, laser interference is carried out to the ITO cleaned
It carves；
（3）Electrolyte quota：Electrolyte is prepared with ferric trichloride, ferrous chloride, deionized water, is stirred continuously until ferric trichloride
After being completely dissolved with ferrous chloride, which is sealed spare；
（4）Electrochemical deposition：Using three-phase electrode system, with step（2）The ITO conductive substrates of middle gained as working electrode,
Using high-purity iron plate as to electrode, using saturated calomel electrode as reference electrode；By step（3）The electrolyte of preparation is placed in electrolysis
In slot, electrolyte is made uniformly to be soaked in three-phase electrode system, set required temperature, use electrochemical operation stand control cathode current
After density and sedimentation time carry out electrochemical deposition operation, close power supply and take out working electrode, rinsed well with deionized water, room
The lower drying of temperature is to get to the α-Fe being attached in ITO substrate2O3Nano-particle.
2. according to the method described in claim 1, it is characterized in that：The step（2）In two beam laser interference systems by
Laser, beam splitting, refractive power and orthopedic systems composition, send out beam of laser by laser, are divided into two beam coherent lights through divided beam system
Beam, divided beam system are into making two beam coherent light spaces pair through dioptric system by high reflective mirror, spectroscope, half-wave plate and polarizer group
Claim, orthopedic systems carry out beam shaping before two light beams converge at sample, them is made to be irradiated to sample simultaneously with certain incidence angle
On product, change two beam spatial light interferometric parameters, parameter is Space Angle, incidence angle, phase angle, polarization state, interference light intensity and exposure
Between light time, make the characteristic size of two beam laser interference system interference figures from nanoscale to micrometer-adjustable, so as to be led in ITO
Interference obtains the optical grating construction of different cycles on electric substrate surface.
3. according to the method described in claim 1, it is characterized in that：The step（3）In, electrolyte is by FeCl3And FeCl2's
Mixed solution forms, and electrolyte remains static always in electrochemical deposition process.
4. according to the method described in claim 3, it is characterized in that：The electrolyte quota process：Using ferric trichloride as trivalent
Source of iron prepares the FeCl of 4-16 mM3Deionized water solution, using ferrous chloride as divalent source of iron, prepare the FeCl of 6-24 mM2
Deionized water solution；Two kinds of solution of ultrasonic dissolution respectively, ultrasonic dissolution again after mixing, obtain clear electrolyte.
5. according to the method described in claim 1, it is characterized in that：The electrochemical deposition process, sedimentation time 1-200
S, depositing temperature 16.5-60oC, deposition current are 1-10 mA/cm2。
6. according to the method described in claim 1, it is characterized in that：Orderly α-the Fe of patterning of the electrochemical deposition2O3It receives
Grain of rice subarray has good adhesion on ITO conductive substrates surface, and nano-particle is uniformly dispersed, and will not occur to reunite existing
As.
7. according to the method described in claim 1, it is characterized in that：Working electrode and to electricity in the electrochemical deposition process
The vertical operation distance of interpolar is 3-10 cm.
8. according to the method described in claim 1, it is characterized in that：All hydrogen-oxygens needed for the electrochemical deposition process
Root is all from the electrolysis of water.
9. according to the method described in claim 1, it is characterized in that：α-the Fe of the electrochemical deposition2O3Nano-particle can be with
It is uniformly scattered in deionized water by the method for ultrasound.
10. according to the method described in claim 2, it is characterized in that：Laser output wavelength used be 1064 nm, Gauss light
Beam is shaped to uniform beam, and laser energy density is 0.42 J/cm2。
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