CN103572312A - 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 preparation method who the present invention relates to a kind of self-holding silicon nanowire array, belongs to technical field of nano material.
Background technology
Silicon nanowire array material, owing to thering is unique structure and physicals, at signal pick-off, biological detection template, catalysis/electrocatalysis, photoelectricity physical device, solar cell, lithium ion battery negative etc. field has boundless application prospect.At present, the method great majority of preparing silicon nanowire array be all based on silicon chip without electroetching, what have also depends on template.These methods are used silicon chip, toxicity corrosive chemical and precious metal, and cost is higher.And the silicon nanowire array of preparation can not self-sustained, need to be grown in substrate, otherwise just can not become array.These mass-producings that limited silicon nanowire array are prepared with and are applied.Such as, CN 101302118A has reported that an employing silicon chip is raw material, take silicon-dioxide bead as template, through 1000 ° of C high temperature, hydrofluoric acid corrosion, evaporation silver, thereby in corrosive fluid, corrode again the preparation method who obtains silicon nanowire array, its step is many, and raw materials cost is high, preparation technology's relative complex.In CN102126724A, reported that employing silicon chip is raw material, through cleaning, without electrochemical deposition, obtained silver nano-grain layer, added hydrofluoric acid and hydrogen peroxide chemical etching, then removed with nitric acid the method that silver obtains nano-wire array.It is that employing silicon chip is raw material equally, process relative complex.Particularly, adopt the nano-wire array that silicon chip etching method obtains all can not control oneself, below must relying on, have the connection of silicon chip substrate and keep structure.
Molten salt electrochemistry method is prepared silicon nanowire array does not also have relevant report.Similarly report as CN102154659A have proposed to prepare at fused-salt electrolytic refining industrial silicon the method for silicon nanowires, but resulting be silicon nanowires, be not nano-wire array.CN 101736354A has reported that employing molten salt electrochemistry method is by SiO
2deng preparing the materials such as nano silicon particles and One Dimension Silicon nano wire, still do not obtain two-dimentional silicon nanowire array.
Summary of the invention
The object of the invention be to provide a kind of can self-sustained, there is the preparation method of simple and inexpensive of the nano-wire array of certain area.
The present invention is applied to electrodeoxidation technology in the preparation of silicon nanowire array, and developing adopting quartz glass is that raw material has the method for the silicon nanowire array of self-sustained in medium of fused salt through electric deoxidation process preparation.The preparation method of the silicon nanowire array that the present invention proposes, described method is carried out successively as follows:
1. a preparation method for self-holding silicon nanowire array, described method is carried out as follows
(1) silicon-containing solid A is raw material, by metal M 2, wire netting M1 is contacted with A and fix, and wire netting M1 is fixed on silicon-containing solid A surface, makes the working electrode B that wire netting covers A part surface or all surfaces;
(2) prepare melting salt X as electrolytic solution, under inert atmosphere protection or vacuum state, make it to melt in crucible and keep within the scope of 600-1100 ° of C of saline solution constant temperature;
(3) part that working electrode B wire netting is covered is submerged in fused salt as negative electrode; Carbon-containing electrode C is anode.Between two electrodes, apply the voltage of 1.7-2.3V, the period is to make to have reacted for 0.5-10 hour;
(4), after having reacted, working electrode B is cooling rear taking-up in inert atmosphere or vacuum; Adopt solvent D washing, remove salt, peel wire netting M1 and wire M2 off, obtain the nano-wire array product of silicon.
2. the silicon-containing solid A described in is transparent or opaque silica glass, the quartz glass tube that the sheet that its thickness is not limit at 0.1mm-4mm length and width area or the length with 0.1mm-4mm diameter are not limit or quartz glass bar and other any regular or irregularly shaped.
3. made working electrode B form is sheet or cylinder or is block or other arbitrary shapes; Wire netting must wrap up at least one face that closely covers electrode material silicon-containing solid A.
4. wire netting M1 used and metal M 2 can be single kind of refractory metal Ni, Mo, W, Ti, Cr, Mn or Co;
Or the metal of several high-temperature corrosion resistances or metal alloy, it is stainless steel, nickelalloy or Kantal alloy; M1 and M2 are same metal or metal alloy or metal not of the same race or metal alloy; The order number of wire netting is not limit, and form is not limit;
The structure of metal M 2 is used for fixedly M1 and A, and metal M 2 is wire, metal holder or metal bolts, and corresponding can be that wire is wound around, metal holder clamping or metal threaded fixing.
5. melting salt X bath composition is one or two or more kinds mixture of alkaline earth metal halide salt, and ratio is not limit;
Or the mixture of the alkaline earth metal oxide that contains 0.01-15wt% alkaline earth metal oxide and halide salts, become the mixture of the above materials of 2 kinds or 3 kinds;
Or the mixture of alkaline earth metal halide salt and alkali halide salts, wherein the amount of alkali halide salts is 0.01-50wt%, becomes the mixture of 2 kinds or 3 kinds above materials;
Or containing 0.01-15wt% alkaline earth metal oxide, 0.01-50wt% alkali halide salts, the mixture of alkali halide salts, alkaline earth metal oxide and alkaline earth metal halide salt, becomes the mixture of the above materials of 3 kinds or 4 kinds.
6. alkaline earth metal halide salt is CaCl2, BaCl2 or CaF2; Alkaline earth metal oxide is CaO;
Alkali halide salts is NaCl or KCl.
7. anode carbon-containing electrode C is Graphite Electrodes or carbon electrode.
8. corresponding one or two or more kinds the salt of mixture of alkaline earth metal halide salt that uses, cleaning solvent D is water or 0.01-1mol% hydrochloric acid or organic solvent dimethyl sulfoxide (DMSO), propylene carbonate or the ethanol that can dissolve alkaline earth metal halide salt;
The corresponding alkaline earth metal oxide and the mixture of halide salts that contains 0.01-15wt% alkaline earth metal oxide that use, becomes 2 kinds or the 3 kinds mixture of materials above, and cleaning solvent D is 0.01-1mol% hydrochloric acid;
The mixture of corresponding alkaline earth metal halide salt and alkali halide salts, wherein the amount of alkali halide salts is 0.01-50wt%, the mixture that becomes 2 kinds or 3 kinds above materials, cleaning solvent D is water or 0.01-1mol% hydrochloric acid or can dissolves organic solvent dimethyl sulfoxide (DMSO), propylene carbonate or the ethanol of alkaline earth metal halide salt and alkali halide salts;
Correspondence contains 0.01-15wt% alkaline earth metal oxide, 0.01-50wt% alkali halide salts, the mixture of alkali halide salts, alkaline earth metal oxide and alkaline earth metal halide salt, the mixture that becomes 3 kinds or 4 kinds above materials, cleaning solvent D is 0.01-1mol% hydrochloric acid.
Multi-metal body catalyst of the present invention is compared with known technology, and tool has the following advantages:
1, in the present invention, raw materials is cheap, and rapidly, environmental friendliness, can scale operation in preparation.
2, the silicon nanowire array that prepared by the present invention has self-holding feature, without any need for the support of substrate and Stability Analysis of Structures.
3, the nanowire length that prepared by the present invention can reach hundreds of micron, and length and diameter all can regulate and control.There is no metal residual, the few purity of impurity is high.
Accompanying drawing explanation
Fig. 1 is scanning electronic microscope (SEM) figure that describes the silicon nanowire array that condition prepares in the embodiment 1 in the present invention.Therefrom can find out, this sample nano-wire array is hundreds of micron, and every nanowire diameter is in 300 nanometer left and right, and contiguous nano wire radially laterally interconnects.
The elemental composition analysis chart of the energy dispersion X ray spectrum (EDX) of the nano-wire array of preparation in Fig. 2 embodiment 1 of the present invention.Can find out, nano-wire array main component is element silicon.Oxygen element content is considerably less.Other compositions almost do not have.
Fig. 3 is the working electrode B schematic diagram in embodiment 1 described in the present invention.That in schematic diagram, show is wire netting M1(1) be nickel screen and metallic rod M2(2) be molybdenum filament.2 silicon-containing material A(3 that relatively clamp) be quartz plate.It should be noted that, this working electrode B schematic diagram, only as an illustration of embodiment.The protection domain of the working electrode form that this patent is declared, is not limited to shown in this figure.
Embodiment
The inventive method is the electrode through wire netting and the covering of the fixing formation of wire wire netting by silicon-containing material, then this electrode is placed in to the melting salt of 600-1100 ° of C, electrode is adopted to carbon-containing electrode, under inert atmosphere or vacuum, apply the bath voltage deoxidation and reduction of 1.7-2.5V; Cooling taking-up after reaction, through washing, peels off, and obtains self-holding silicon nanowire array.Its length can be by the raw thickness selected and the Timing of reaction.Nano-wire array is comprised of crystalline silicon nano wire, special, has horizontal syndeton between nano wire, has certain intensity, does not need carrier supported and can keep Stability Analysis of Structures.This preparation method is the self-holding silicon nanowire array of preparation of cheapness fast, and yardstick is adjustable, is applicable to scale production.
In order to further illustrate the present invention, enumerate following embodiment, but it does not limit the defined invention scope of each accessory claim.Such as, the raw material that silicon nanowire array employing is prepared in the present invention's proposition is silicon-containing material A, this raw material A is fine and close silica glass material, can be transparent or opaque; Thickness can be in 0.1mm-4mm scope, be shaped as the quartz glass bar that sheet that length and width area do not limit or thickness can not limit in 0.1mm-4mm, length at quartz glass tube or the diameter of 0.1mm-4mm scope.
(a) JGS3 level optical quartz sheet, is of a size of 20x10x0.5mm, adopts 2 of the 20 order metal nickel screens of 20x10mm to be fixedly clamped with the metal molybdenum filament of diameter 1mm as electric current collection body, makes working electrode.
(b) under argon gas atmosphere in molten salt electrochemistry device, at the CaCl of 850 ° of C
2in fused salt, adopt the deoxidation of 1.9V voltage electricity, plumbago crucible is to electrode, about 5h of reaction times.
(c), after having reacted, working electrode is proposed from saline solution, cooling under inert atmosphere after, take out and under waterly to wash and to peel off nickel screen and molybdenum filament and outer impurity, the product obtaining is silicon nanowire array.
Silicon nanowire array is 2 layers, and every layer thickness is about 200 microns, and area can reach 20x10mm, and structure is more even, linear diameter approximately 200 nanometers.For the self-holding nano-wire array of sheet.The nano-wire array of preparing in this embodiment represents with NW-A, and its scanning electronic microscope characterization result is listed in Fig. 1, and energy dispersion X ray spectrum the results are shown in Fig. 2, and working electrode schematic diagram is listed in Fig. 3.
With embodiment 1, just in step (a), adopt JGS1 level optical quartz sheet to replace JGS3 level optical quartz sheet.Synthetic nano-wire array represents with NW-B.
With embodiment 1, just in step (a), adopt opaque quartz plate to replace JGS3 level optical quartz sheet.Synthetic nano-wire array represents with NW-C.
Embodiment 4
With embodiment 1, just in step (a) with diameter 4mm, the replacement of the quartz pushrod of long 20mm is of a size of the quartz plate of 20x10x0.5mm.The outside surface of the axle parcel quartz pushrods such as corresponding employing metal nickel screen, adopts thin molybdenum filament tighten, makes cylindrical working electrode.Reaction times 10h, synthetic nano-wire array is the nano-wire array that is arranged in cylindrical surface type, with NW-D, represents.
Embodiment 5
With embodiment 1, just in step (a) with external diameter 8mm, internal diameter 6mm, the silica tube replacement of long 20mm is of a size of the quartz plate of 20x10x0.5mm.The outside surface of the axle parcel quartz pushrods such as corresponding employing metal nickel screen, adopts thin molybdenum filament tighten, makes cylindrical working electrode (raw material is tubular).Synthetic nano-wire array is to arrange the nano-wire array that is tubular type, with NW-E, represents.
Embodiment 6
With embodiment 1, just in step (a), with the quartz plate of 10x10x0.3mm, replaced being of a size of the quartz plate of 20x10x0.5mm.Nickel screen and molybdenum filament size be corresponding change also, obtains sheet type working electrode.Reaction times is short is about 2.5h.Synthetic nano-wire array NW-F represents.
Embodiment 7
With embodiment 1, just in step (a), with the quartz wedge of 20x10x4mm, replaced being of a size of the quartz plate of 20x10x0.5mm.Nickel screen and molybdenum filament size be corresponding change also, obtains piece type working electrode.Reaction times 5h, has synthesized nano-wire array NW-G, reaction times 10h, and synthesis of nano linear array is classified NW-H as.
Embodiment 8
With embodiment 1, just step (a) has replaced nickel screen with stainless (steel) wire, with nickel wire, has replaced molybdenum filament.Having obtained nano-wire array is NW-I.Almost in the same manner as in Example 1.
Embodiment 9
With embodiment 1, just in step (b), with the BaCl of 5wt%
2and CaCl
2mixture replace CaCl
2, reaction conditions is identical.Obtain nano-wire array and be designated as NW-J.
Embodiment 10
With embodiment 1, just in step (b), with the CaCl containing 10wt%CaO
2replace CaCl with the mixture of CaO
2, reaction conditions is identical, adopts the washing of 0.2mol% dilute hydrochloric acid.Obtain nano-wire array and be designated as NW-K.
Embodiment 11
With embodiment 1, just in step (b), with the CaCl containing 5wt%KCl and 5wt%NaCl
2replaced pure CaCl
2, reaction conditions is identical.Obtain nano-wire array and be designated as NW-L.
Embodiment 12
With embodiment 1, just in step (b), to contain 5wt%CaF
2caCl
2replaced pure CaCl
2, reaction conditions is identical.Obtain nano-wire array and be designated as NW-M.
Embodiment 13
With embodiment 1, just step (b) adopts independent carbon dioxide process carbon electrode to replace Graphite Electrodes.Reaction conditions is identical, obtains nano-wire array and is designated as NW-N.
Embodiment 14
With embodiment 1, just in step (c), adopt 0.2mol% salt acid elution to replace water washing.The nano-wire array obtaining is designated as NW-O.
With embodiment 1, just in step (c), adopt dimethyl sulfoxide (DMSO) washing to replace water washing.The nano-wire array obtaining is designated as NW-P.
Embodiment 16
With embodiment 1, just, in step (b), adopt 1100 ° of C temperature to replace 850 ° of C.The nano-wire array obtaining is designated as NW-Q.
Embodiment 17
With embodiment 1, just, in step (b), adopt 600 ° of C temperature to replace 850 ° of C.Meanwhile, with the CaCl containing 20%KCl and 20%NaCl
2replaced pure CaCl
2.The nano-wire array obtaining is designated as NW-R.
Embodiment 18
With embodiment 1, just, in step (b), adopt 2.3V voltage to replace 1.9V voltage, the nano-wire array obtaining is designated as NM-S.
Embodiment 19
With embodiment 1, just, in step (b), adopt 1.7V voltage to replace 1.9V voltage, the nano-wire array obtaining is designated as NM-T.
The appearance and size structured data of the nano-wire array obtaining, lists in table 1.Pattern adopts scanning electronic microscope (SEM) to detect, and what with annex energy dispersion X-ray spectrum (EDX) confirmation in SEM, obtain is elemental silicon material.
The structural information of several nano-wire arrays of table 1.
Note: D4L20 represents the right cylinder of diameter 4mm length 20mm, and F8L20 represents the cylindrical tube of diameter 8mm length 20mm
Claims (8)
1. a preparation method for self-holding silicon nanowire array, is characterized in that: described method is carried out as follows
(1) silicon-containing solid A is raw material, by metal M 2, wire netting M1 is contacted with A and fix, and wire netting M1 is fixed on silicon-containing solid A surface, makes the working electrode B that wire netting covers A part surface or all surfaces;
(2) prepare melting salt X as electrolytic solution, under inert atmosphere protection or vacuum state, make it to melt in crucible and keep within the scope of 600-1100 ° of C of saline solution constant temperature;
(3) part that working electrode B wire netting is covered is submerged in fused salt as negative electrode; Carbon-containing electrode C is anode.Between two electrodes, apply the voltage of 1.7-2.3V, the period is to make to have reacted for 0.5-10 hour;
(4), after having reacted, working electrode B is cooling rear taking-up in inert atmosphere or vacuum; Adopt solvent D washing, remove salt, peel wire netting M1 and wire M2 off, obtain the nano-wire array product of silicon.
2. the preparation method of silicon nanowire array as claimed in claim 1, it is characterized in that, described silicon-containing solid A is transparent or opaque silica glass, the quartz glass tube that the sheet that its thickness is not limit at 0.1mm-4mm length and width area or the length with 0.1mm-4mm diameter are not limit or quartz glass bar and other any regular or irregularly shaped.
3. the preparation method of the silicon nanowire array as described in claim 1 and 2, is characterized in that, made working electrode B form is sheet or cylinder or is block or other arbitrary shapes; Wire netting must wrap up at least one face that closely covers electrode material silicon-containing solid A.
4. the preparation method of silicon nanowire array as claimed in claim 1, is characterized in that, wire netting M1 used and metal M 2 can be single kind of refractory metal Ni, Mo, W, Ti, Cr, Mn or Co;
Or the metal of several high-temperature corrosion resistances or metal alloy, it is stainless steel, nickelalloy or Kantal alloy; M1 and M2 are same metal or metal alloy or metal not of the same race or metal alloy; The order number of wire netting is not limit, and form is not limit;
The structure of metal M 2 is used for fixedly M1 and A, and metal M 2 is wire, metal holder or metal bolts, and corresponding can be that wire is wound around, metal holder clamping or metal threaded fixing.
5. the preparation method of silicon nanowire array as claimed in claim 1, is characterized in that, melting salt X bath composition is one or two or more kinds mixture of alkaline earth metal halide salt, and ratio is not limit;
Or the mixture of the alkaline earth metal oxide that contains 0.01-15wt% alkaline earth metal oxide and halide salts, become the mixture of the above materials of 2 kinds or 3 kinds;
Or the mixture of alkaline earth metal halide salt and alkali halide salts, wherein the amount of alkali halide salts is 0.01-50wt%, becomes the mixture of 2 kinds or 3 kinds above materials;
Or containing 0.01-15wt% alkaline earth metal oxide, 0.01-50wt% alkali halide salts, the mixture of alkali halide salts, alkaline earth metal oxide and alkaline earth metal halide salt, becomes the mixture of the above materials of 3 kinds or 4 kinds.
6. the preparation method of silicon nanowire array as claimed in claim 5, is characterized in that,
Alkaline earth metal halide salt is CaCl
2, BaCl
2or CaF
2; Alkaline earth metal oxide is CaO;
Alkali halide salts is NaCl or KCl.
7. silicon nanowire array preparation method as claimed in claim 1, is characterized in that, anode carbon-containing electrode C is Graphite Electrodes or carbon electrode.
8. according to the silicon nanowire array preparation method described in claim 1 and 5, it is characterized in that,
Corresponding one or two or more kinds the salt of mixture of alkaline earth metal halide salt that uses, cleaning solvent D is water or 0.01-1mol% hydrochloric acid or organic solvent dimethyl sulfoxide (DMSO), propylene carbonate or the ethanol that can dissolve alkaline earth metal halide salt;
The corresponding alkaline earth metal oxide and the mixture of halide salts that contains 0.01-15wt% alkaline earth metal oxide that use, becomes 2 kinds or the 3 kinds mixture of materials above, and cleaning solvent D is 0.01-1mol% hydrochloric acid;
The mixture of corresponding alkaline earth metal halide salt and alkali halide salts, wherein the amount of alkali halide salts is 0.01-50wt%, the mixture that becomes 2 kinds or 3 kinds above materials, cleaning solvent D is water or 0.01-1mol% hydrochloric acid or can dissolves organic solvent dimethyl sulfoxide (DMSO), propylene carbonate or the ethanol of alkaline earth metal halide salt and alkali halide salts;
Correspondence contains 0.01-15wt% alkaline earth metal oxide, 0.01-50wt% alkali halide salts, the mixture of alkali halide salts, alkaline earth metal oxide and alkaline earth metal halide salt, the mixture that becomes 3 kinds or 4 kinds above materials, cleaning solvent D is 0.01-1mol% hydrochloric acid.
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| CN107799427A (en) * | 2016-09-05 | 2018-03-13 | 达兴材料股份有限公司 | Method for producing photovoltaic element |
| CN110512223A (en) * | 2019-08-07 | 2019-11-29 | 武汉大学 | No template prepares the melten salt electriochemistry method of nano-tube |
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| CN107799427A (en) * | 2016-09-05 | 2018-03-13 | 达兴材料股份有限公司 | Method for producing photovoltaic element |
| CN110512223A (en) * | 2019-08-07 | 2019-11-29 | 武汉大学 | No template prepares the melten salt electriochemistry method of nano-tube |
| CN110512223B (en) * | 2019-08-07 | 2020-12-01 | 武汉大学 | Fused salt electrochemical method for preparing silicon nanotube without template |
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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 |