CN103572312B - Method for preparing self-sustained silicon nanowire array - Google Patents
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Abstract
The invention discloses a method for preparing a self-sustained silicon nanowire array and belongs to the technical field of the preparation of nanometer materials. The method comprises the steps of: fixing a silicon-containing material via metal nets and metal wires to form an electrode covered by the metal nets, then putting the electrode into molten salt at a temperature of 600-1100 DEG C, and exerting a 1.7-2.5V bath voltage onto the electrode which is a carbon-containing electrode for deoxidization in inert atmosphere or under vacuum; reacting and then taking out the electrode, cleaning and peeling to acquire the self-sustained silicon nanowire array. The length of the self-sustained silicon nanowire array can be adjusted through the thickness of the selected material and the reaction time. The nanowire array is formed by crystalline silicon nanowires, and particularly, the nanowires are transversely connected and have a definite range of strength and the structure can remain stable without being supported by any carrier. By adopting the method disclosed by the invention, the self-sustained silicon nanowire array can be rapidly prepared with low cost, and the length of the self-sustained silicon nanowire array can be adjusted. Thus, the method disclosed by the invention is suitable for mass production.
Description
Technical field
The present invention relates to a kind of preparation method of self-holding silicon nanowire array, belong to technical field of nano material.
Background technology
Silicon nanowire array material, due to having structure and the physical property of uniqueness, in signal transducer, biological detection mould
Plate, catalysis/electro-catalysis, photoelectricity physical device, solar cell, lithium ion battery negative etc. field has boundless application
Prospect.At present, the method great majority preparing silicon nanowire array are all based on silicon chip no electroetching, and have also relies on template.
These methods use silicon chip, toxicity corrosive chemical and noble metal, relatively costly.And the silicon nanowire array prepared is not
Can self-sustained, need to be grown in substrate, otherwise cannot become array.These limit the scale of silicon nanowire array
Change preparation and its application.Such as, CN 101302118A reports one using silicon chip is raw material, with silicon oxide pellets is
Template, through 1000 °C of high temperature, Fluohydric acid. corrodes, evaporation silver, then corrodes thus obtaining silicon nanowire array in corrosive liquid
Preparation method, its step is many, and cost of material is high, and preparation technology is relative complex.Report in CN102126724A and using silicon chip be
Raw material, through over cleaning, no electrochemical deposition obtains Silver nano-particle layer, adds Fluohydric acid. and hydrogen peroxide chemical etching, then use nitre
The method that silver obtains nano-wire array is removed in acid.It is equally to be raw material using silicon chip, and process is relative complex.Particularly, adopt
The nano-wire array that silicon chip etching method obtains is unable to control oneself it is necessary to relying on the connection having silicon chip substrate below and keeping tying
Structure.
Melten salt electriochemistry method prepares silicon nanowire array does not also have the report of correlation.Similar report is such as
CN102154659A proposes the method preparing silicon nanowires in fused-salt electrolytic refining industrial silicon, but obtained be silicon nanometer
Line, not nano-wire array.CN 101736354A reports using melten salt electriochemistry method by SiO2Etc. silicon nanometer can be prepared
The material such as granule and one-dimensional silicon nanowires, but do not obtain the silicon nanowire array of two dimension.
Content of the invention
Present invention aim at providing a kind of being capable of self-sustained, have certain area nano-wire array simple and
Cheap preparation method.
Electrodeoxidation technology is applied in the preparation of silicon nanowire array the present invention, develops and using quartz glass is
The method that raw material has the silicon nanowire array of self-sustained in medium of fused salt through the preparation of electro-deoxidation process.The present invention carries
The preparation method of the silicon nanowire array going out, methods described is carried out successively as follows：
1. a kind of preparation method of self-holding silicon nanowire array, methods described is carried out as follows
（1）Silicon-containing solid A is raw material, with metal M2, wire netting M1 with A is contacted fixation, wire netting M1 is fixed on siliceous solid
Body A surface, makes the working electrode B that wire netting covers part A surface or all surfaces；
（2）Prepare fuse salt X as electrolyte, be allowed to melt in crucible simultaneously under inert atmosphere protection or vacuum state
Keep in the range of 600-1100 °C of saline solution constant temperature；
（3）The part that working electrode B wire netting covers is made to be submerged in fused salt as negative electrode；Carbon-containing electrode C is anode.Two
Apply the voltage of 1.7-2.3V, control time makes reaction complete for 0.5-10 hour between electrode；
（4）After the completion of reaction, working electrode B takes out after cooling down in inert atmosphere or vacuum；Using solvent D washing, go
Fall salt, peel wire netting M1 and tinsel M2 off, that is, obtain the nano-wire array product of silicon.
2. the silicon-containing solid A described in is transparent or opaque quartz glass, and its thickness is in 0.1mm-4mm length and width area
The lamellar that do not limit or be have the quartz glass tube that the length of 0.1mm-4mm diameter do not limit or quartz glass bar and other
Any regular or irregularly shaped.
3. the working electrode B form made by is piece or cylinder or is block or other arbitrary shapes；Metal
Net must wrap up close at least one face of electrode material silicon-containing solid A.
4. wire netting M1 used by and metal M2 can be single kind of refractory metal Ni, Mo, W, Ti, Cr, Mn or Co；
Or the metal of several high-temperature corrosion resistance or metal alloy, it is rustless steel, nickel alloy or Kantal alloy；
M1 and M2 is same metal or metal alloy or not same metal or metal alloy；The mesh number of wire netting does not limit, shape
Formula does not limit；
The structure of metal M2 is used for fixing M1 and A, and metal M2 is tinsel, metal holder or metal bolts, corresponding can
To be that tinsel is wound around, metal holder clamps or metal threaded fixation.
5. fuse salt X bath composition is the alkaline-earth halide salt mixture of one or two or more kinds, and ratio does not limit；
Or the alkaline earth oxide containing 0.01-15wt% alkaline earth oxide and the mixture of halide salts, become
Mixture for 2 kinds or more than 3 kinds materials；
Or the mixture of alkaline-earth halide salt and alkali halide salts, the wherein amount of alkali halide salts
For 0.01-50wt%, become the mixture of 2 kinds or more than 3 kinds materials；
Or contain 0.01-15wt% alkaline earth oxide, 0.01-50wt% alkali halide salts, alkali metal halogenation
The mixture of thing salt, alkaline earth oxide and alkaline-earth halide salt, becomes the mixture of 3 kinds or more than 4 kinds materials.
6. alkaline-earth halide salt is CaCl2, BaCl2 or CaF2；Alkaline earth oxide is CaO；
Alkali halide salts are NaCl or KCl.
7. anode carbon-containing electrode C is graphite electrode or carbon resistance rod.
8. the corresponding salt using the alkaline-earth halide salt mixture of one or two or more kinds, cleaning solvent D be water or
Person's 0.01-1mol% hydrochloric acid or can dissolve the organic solvent dimethyl sulfoxide of alkaline-earth halide salt, propylene carbonate or
Ethanol；
The corresponding mixing using the alkaline earth oxide containing 0.01-15wt% alkaline earth oxide and halide salts
Thing, becomes the mixture of 2 kinds or more than 3 kinds materials, and cleaning solvent D is 0.01-1mol% hydrochloric acid；
Correspond to the mixture of alkaline-earth halide salt and alkali halide salts, the amount of wherein alkali halide salts is
0.01-50wt%, becomes the mixture of 2 kinds or more than 3 kinds materials, cleaning solvent D be water or 0.01-1mol% hydrochloric acid or
Organic solvent dimethyl sulfoxide, propylene carbonate or the second of alkaline-earth halide salt and alkali halide salts can be dissolved
Alcohol；
Correspond to and contain 0.01-15wt% alkaline earth oxide, 0.01-50wt% alkali halide salts, alkali metal halogenation
The mixture of thing salt, alkaline earth oxide and alkaline-earth halide salt, becomes the mixture of 3 kinds or more than 4 kinds materials,
Cleaning solvent D is 0.01-1mol% hydrochloric acid.
The multi-metal body catalyst of the present invention is compared with known technology, has the advantage that：
1st, in the present invention, preparing raw material is cheap, and preparation is rapid, and environmental friendliness can be with large-scale production.
2nd, the present invention preparation silicon nanowire array have the characteristics that self-holding it is not necessary to the support of any substrate and structure is steady
Fixed.
3rd, the nanowire length of present invention preparation can reach hundreds of micron, and length and the equal controllable of diameter.No
Metal residual, the few purity of impurity is high.
Brief description
The scanning electron microscope of Fig. 1 silicon nanowire array that condition is prepared described in the embodiment 1 in the present invention
（SEM）Figure.There it can be seen that this sample nano-wire array is hundreds of micron, every nanowire diameter is on 300 nanometers of left sides
The right side, neighbouring nano wire is radially laterally connected with each other.
The energy dispersion X ray spectrum of the nano-wire array of preparation in Fig. 2 embodiment of the present invention 1（EDX）Element become
Divide analysis chart.As can be seen that nano-wire array main component is element silicon.Oxygen element content is considerably less.Other compositions almost do not have
Have.
Fig. 3 is the working electrode B schematic diagram in heretofore described embodiment 1.It is shown that wire netting M1 in schematic diagram
（1）For nickel screen and metallic rod M2（2）For molybdenum filament.The silicon-containing material A of 2 faces clamping relatively（3）For piezoid.It should be noted that
This working electrode B schematic diagram, is only used as an illustration of embodiment.The protection model of the working electrode form that this patent is declared
Enclose, shown in not limited to this figure.
Specific embodiment
Silicon-containing material through wire netting and the fixing electrode forming wire netting covering of tinsel, then will by the inventive method
This electrode is placed in 600-1100 °C of fuse salt, adopts carbon-containing electrode to electrode, applies 1.7- under inert atmosphere or vacuum
The tank voltage deoxidation and reduction of 2.5V；After reaction, cooling is taken out, and through washing, peels off, that is, obtains self-holding silicon nanowire array.Its
Length can be by the raw thickness selected and the time adjustment of reaction.Nano-wire array is made up of crystal silicon nanowires, especially
, there is between nano wire horizontal attachment structure, there is certain intensity it is not necessary to carrier supported and can be steady with holding structure
Fixed.This preparation method can be quickly cheap preparation control oneself silicon nanowire array, yardstick is adjustable it is adaptable to large-scale production.
In order to further illustrate the present invention, enumerate following embodiment, but it is not intended to limit each accessory claim and is determined
The invention scope of justice.Such as, the raw material that silicon nanowire array employing is prepared in proposition of the present invention is silicon-containing material A, and this raw material A is
Fine and close quartz glass material, can be transparent or opaque；Thickness can in 0.1mm-4mm scope, be shaped as length and width area
The lamellar not limited or thickness can not limit in 0.1mm-4mm, length in the quartz glass tube of 0.1mm-4mm scope or diameter
Quartz glass bar.
Embodiment 1
A () JGS3 level optical quartz piece, a size of 20x10x0.5mm, using 2 works of 20 mesh metal nickel screen of 20x10mm
For current collector, it is fixedly clamped with the metal molybdenum filament of diameter 1mm, makes working electrode.
B () under an argon atmosphere in melten salt electriochemistry device, in 850 °C of CaCl2In fused salt, de- using 1.9V voltage electricity
Oxygen, graphite crucible is to electrode, response time about 5h.
After the completion of (c) reaction, propose working electrode from saline solution, after cooling down under an inert atmosphere, take out under water washing
Wash and peel off nickel screen and molybdenum filament and outer layer impurity, the product obtaining is silicon nanowire array.
Silicon nanowire array is 2 layers, and every thickness degree is about 200 microns, and, up to 20x10mm, structure is more uniform, and line is straight for area
About 200 nanometers of footpath.For the self-holding nano-wire array of lamellar.In this embodiment, the nano-wire array of preparation is represented with NW-A, its scanning
Ultramicroscope characterization result is listed in Fig. 1, and energy dispersion X ray spectrum result is listed in Fig. 2, and working electrode schematic diagram is listed in Fig. 3.
Embodiment 2
With embodiment 1, simply step（a）Middle employing JGS1 level optical quartz piece replaces JGS3 level optical quartz piece.Synthesis
Nano-wire array represented with NW-B.
Embodiment 3
With embodiment 1, simply step（a）Middle using opaque piezoid replace JGS3 level optical quartz piece.Synthesis
Nano-wire array is represented with NW-C.
Embodiment 4
With embodiment 1, simply step（a）In with diameter 4mm, the quartz pushrod of long 20mm replaces a size of 20x10x0.5mm
Piezoid.Corresponding employing metal nickel screen isometry wraps up the outer surface of quartz pushrod, is tightened using thin molybdenum filament, makes cylindrical work
Make electrode.Response time 10h, the nano-wire array of synthesis is the nano-wire array being arranged in face of cylinder type, is represented with NW-D.
Embodiment 5
With embodiment 1, simply step（a）In with external diameter 8mm, the quartz ampoule of internal diameter 6mm, long 20mm replaces a size of
20x10x0.5mm piezoid.Corresponding employing metal nickel screen isometry wraps up the outer surface of quartz pushrod, is tightened using thin molybdenum filament,
Make cylindrical work electrode（Raw material is tubular）.The nano-wire array of synthesis is the nano-wire array in tubular type for the arrangement,
Represented with NW-E.
Embodiment 6
With embodiment 1, simply step（a）In instead of a size of 20x10x0.5mm's with the piezoid of 10x10x0.3mm
Piezoid.Nickel screen and the also corresponding change of molybdenum filament size, obtain piece type working electrode.Response time is short to be about 2.5h.Synthesize receives
Nanowire arrays NW-F represents.
Embodiment 7
With embodiment 1, simply step（a）In a size of stone of 20x10x0.5mm be instead of with the quartz wedge of 20x10x4mm
English piece.Nickel screen and the also corresponding change of molybdenum filament size, obtain block-type working electrode.Response time 5h, has synthesized nano-wire array NW-
G, response time 10h, synthesis nano-wire array is NW-H.
Embodiment 8
With embodiment 1, simply step（a）Nickel screen be instead of with stainless (steel) wire, molybdenum filament be instead of with nickel wire.Obtain nanometer
Linear array is classified as NW-I.Almost in the same manner as in Example 1.
Embodiment 9
With embodiment 1, simply step（b）In, with the BaCl of 5wt%2And CaCl2Mixture replace CaCl2, reaction condition
Identical.Obtain nano-wire array and be designated as NW-J.
Embodiment 10
With embodiment 1, simply step（b）In, with the CaCl containing 10wt%CaO2Replace CaCl with the mixture of CaO2, reaction
Condition is identical, using the washing of 0.2mol% dilute hydrochloric acid.Obtain nano-wire array and be designated as NW-K.
Embodiment 11
With embodiment 1, simply step（b）In, with the CaCl containing 5wt%KCl and 5wt%NaCl2Instead of pure CaCl2, reaction
Condition is identical.Obtain nano-wire array and be designated as NW-L.
Embodiment 12
With embodiment 1, simply step（b）In, with containing 5wt%CaF2CaCl2Instead of pure CaCl2, reaction condition is identical.
Obtain nano-wire array and be designated as NW-M.
Embodiment 13
With embodiment 1, simply step（b）Graphite electrode be instead of using independent carbon electrode.Reaction condition is identical, is received
Nanowire arrays are designated as NW-N.
Embodiment 14
With embodiment 1, simply step（c）Middle employing 0.2mol% salt acid elution replaces water washing.The nano-wire array obtaining
It is designated as NW-O.
Embodiment 15
With embodiment 1, simply step（c）Middle employing dimethyl sulfoxide washing replaces water washing.The nano-wire array obtaining
It is designated as NW-P.
Embodiment 16
With embodiment 1, simply step（b）In, replace 850 °C using 1100 °C of temperature.The nano-wire array obtaining is designated as
NW-Q.
Embodiment 17
With embodiment 1, simply step（b）In, replace 850 °C using 600 °C of temperature.Meanwhile, with containing 20%KCl and 20%
The CaCl of NaCl2Instead of pure CaCl2.The nano-wire array obtaining is designated as NW-R.
Embodiment 18
With embodiment 1, simply step（b）In, 1.9V voltage is replaced using 2.3V voltage, the nano-wire array obtaining is designated as
NM-S.
Embodiment 19
With embodiment 1, simply step（b）In, 1.9V voltage is replaced using 1.7V voltage, the nano-wire array obtaining is designated as
NM-T.
The appearance and size structured data of the nano-wire array obtaining, is listed in table 1.Pattern adopts scanning electron microscope
（SEM）Detection, and composed with the adnexa energy dispersion X-ray in SEM（EDX）What confirmation obtained is simple substance silicon materials.
The structural information of several nano-wire array of table 1.
Note：D4L20 represents the cylinder of diameter 4mm length 20mm, and F8L20 represents the cylindrical tube of diameter 8mm length 20mm.
Claims (6)
1. a kind of preparation method of self-holding silicon nanowire array it is characterised in that：Methods described is carried out as follows,
(1) silicon-containing solid A is raw material, with tinsel M2, wire netting M1 with A is contacted fixation, wire netting M1 is fixed on silicon-containing solid
A surface, makes the working electrode B that wire netting covers part A surface or all surfaces；
(2) prepare fuse salt X as electrolyte, be allowed to melt in crucible and keep under inert atmosphere protection or vacuum state
In the range of 600-1100 DEG C of saline solution constant temperature；
(3) part that working electrode B wire netting covers is made to be submerged in fused salt as negative electrode；Carbon-containing electrode C is anode；Two electrodes
Between apply the voltage of 1.7-2.3V, control time makes reaction complete for 0.5-10 hour；
(4), after the completion of reacting, working electrode B takes out after cooling down in inert atmosphere or vacuum；Using solvent D washing, remove salt,
Peel wire netting M1 and tinsel M2 off, that is, obtain the nano-wire array product of silicon；
Described wire netting M1 adopts the 20 mesh metal nickel screens of 20x10mm；
Described wire netting M1 is nickel screen and tinsel M2 is molybdenum filament；
Described silicon-containing solid A is transparent or opaque quartz glass；
Fuse salt X bath composition is the alkaline-earth halide salt mixture of one or two or more kinds, and ratio does not limit；
Or the alkaline earth oxide containing 0.01-15wt% alkaline earth oxide and the mixture of halide salts, become 2
Kind or the mixture of more than 3 kinds materials；
Or the mixture of alkaline-earth halide salt and alkali halide salts, the amount of wherein alkali halide salts is
0.01-50wt%, becomes the mixture of 2 kinds or more than 3 kinds materials；
Or contain 0.01-15wt% alkaline earth oxide, 0.01-50wt% alkali halide salts, alkali halide
The mixture of salt, alkaline earth oxide and alkaline-earth halide salt, becomes the mixture of 3 kinds or more than 4 kinds materials；
Alkaline-earth halide salt is CaCl2、BaCl2Or CaF2；Alkaline earth oxide is CaO；
Alkali halide salts are NaCl or KCl.
2. the preparation method of silicon nanowire array as claimed in claim 1 is it is characterised in that described quartz glass thickness exists
Quartz glass tube or stone that the 0.1mm-4mm length and width area lamellar not limited or the length with 0.1mm-4mm diameter do not limit
English Glass rod.
3. the preparation method of silicon nanowire array as claimed in claim 1 or 2 is it is characterised in that made working electrode B
Form is piece or cylinder or is bulk；Wire netting must wrap up close at least the one of electrode material silicon-containing solid A
On individual face.
4. the preparation method of silicon nanowire array as claimed in claim 1 is it is characterised in that wire netting M1 used is single kind
W metal replaced by refractory metal Mo, W, Ti, Cr, Mn or Co, rustless steel, nickel alloy or Kantal alloy；Tinsel M2 is single
Metal molybdenum replaced by a kind of refractory metal W, Ti, Cr, Mn or Co, rustless steel, nickel alloy or Kantal alloy；
The structure of tinsel M2 is used for fixing M1 and A, and tinsel M2 is metal holder or metal bolts replace tinsel, corresponding
It is that tinsel is wound around, metal holder clamps or metal threaded fixation.
5. silicon nanowire array preparation method as claimed in claim 1 is it is characterised in that anode carbon-containing electrode C is graphite electricity
Pole or carbon resistance rod.
6. silicon nanowire array preparation method according to claim 1 it is characterised in that
The corresponding salt using the alkaline-earth halide salt mixture of one or two or more kinds, cleaning solvent D is water or 0.01-
1mol% hydrochloric acid or organic solvent dimethyl sulfoxide, propylene carbonate or ethanol that alkaline-earth halide salt can be dissolved；
The corresponding mixture using the alkaline earth oxide containing 0.01-15wt% alkaline earth oxide and halide salts,
Become the mixture of 2 kinds or more than 3 kinds materials, cleaning solvent D is 0.01-1mol% hydrochloric acid；
Correspond to the mixture of alkaline-earth halide salt and alkali halide salts, the amount of wherein alkali halide salts is
0.01-50wt%, becomes the mixture of 2 kinds or more than 3 kinds materials, cleaning solvent D be water or 0.01-1mol% hydrochloric acid or
Person can dissolve organic solvent dimethyl sulfoxide, propylene carbonate or the second of alkaline-earth halide salt and alkali halide salts
Alcohol；
Correspond to and contain 0.01-15wt% alkaline earth oxide, 0.01-50wt% alkali halide salts, alkali halide
The mixture of salt, alkaline earth oxide and alkaline-earth halide salt, becomes the mixture of 3 kinds or more than 4 kinds materials, washes
Washing solvent D is 0.01-1mol% hydrochloric acid.
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| CN101736354A (en) * | 2008-11-06 | 2010-06-16 | 北京有色金属研究总院 | Method for preparing one or more of silicon nano power, silicon nanowires and silicon nanotubes by electrochemical method |
| CN102154659A (en) * | 2011-03-10 | 2011-08-17 | 东北大学 | Preparation method of silicon nanowire by electrorefining industrial silicon by fused salt |
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| WO2005110057A2 (en) * | 2004-01-06 | 2005-11-24 | The Regents Of The University Of California | Crystallographic alignment of high-density nanowire arrays |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101736354A (en) * | 2008-11-06 | 2010-06-16 | 北京有色金属研究总院 | Method for preparing one or more of silicon nano power, silicon nanowires and silicon nanotubes by electrochemical method |
| CN102154659A (en) * | 2011-03-10 | 2011-08-17 | 东北大学 | Preparation method of silicon nanowire by electrorefining industrial silicon by fused salt |
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Effective date of registration: 20191111 Address after: 215600 A 207 room A building center of Zhangjiagang Free Trade Zone, Suzhou Free Trade Zone, Jiangsu Co-patentee after: Dalian Institute of Chemical Physics, Chinese Academy of Sciences Patentee after: Zhangjiagang Institute of industrial technology, Dalian Institute of Chemical Physics, China Academy of Sciences Address before: 116023 No. 457, Zhongshan Road, Liaoning, Dalian Patentee before: Dalian Institute of Chemical Physics, Chinese Academy of Sciences |