CN114180577A - Silicon nanowire array and preparation method thereof - Google Patents
Silicon nanowire array and preparation method thereof Download PDFInfo
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- CN114180577A CN114180577A CN202111453274.2A CN202111453274A CN114180577A CN 114180577 A CN114180577 A CN 114180577A CN 202111453274 A CN202111453274 A CN 202111453274A CN 114180577 A CN114180577 A CN 114180577A
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Abstract
The invention provides a silicon nanowire array and a preparation method thereof, belonging to the field of synthesis of micro-nano materials. Taking industrial grade diatomite with low cost as a silicon source, mixing the industrial grade diatomite with graphite and sodium alginate after pretreatment, grinding and pulping, packaging with a polyimide film and a metal lithium sheet after drying, and charging and discharging for several times to prepare the silicon nanowire array. The invention has the advantages of easily obtained raw materials, simple process, lower cost and wide application prospect. The prepared silicon nanowires have bright appearance and characteristic, the diameter of the silicon nanowires is about 50nm, the silicon nanowires are integrally arranged in a regular array shape, and the silicon nanowires have a wide application prospect in the aspects of nano electronic devices, optoelectronic devices, new energy sources and the like.
Description
Technical Field
The invention belongs to the field of micro-nano material synthesis, and particularly relates to a silicon nanowire array and a preparation method thereof.
Background
Silicon nanowires are a typical representation of one-dimensional nanomaterials and have good semiconductor-specific properties, such asThe concentration of the intrinsic carriers is 1.5 multiplied by 1010/cm3Intrinsic resistivity of 1.5 × 1010 Ω · cm, electron mobility of 1350cm2V.s) hole mobility of 480cm2V · s. In addition, the silicon nanowire also shows physical properties such as field emission, thermal conductivity, visible photoluminescence and the like which are different from bulk silicon materials, and has huge application prospects in the aspects of nano electronic devices, optoelectronic devices, new energy resources and the like. More importantly, the silicon nanowire has excellent compatibility with the existing silicon technology, and further has great market application potential. Therefore, the silicon nanowire is a new material with great application potential in the field of one-dimensional nanomaterials.
Guo and Qi et al reported a method for real-time electrical monitoring of single label-free single molecule ATPase hydrolysis by using high gain silicon nanowire-based field effect transistor circuits, indicating that nanowires have good applications in the kinetic process of bioactivity for direct detection of single molecules or single event sensitivity (ACS Nano 2017,11,12, 12789-. Park, Kim and Cahoon et al report the light absorption properties of a silicon nanowire photovoltaic device with dielectric and metal grating structures, where the one-dimensional dielectric or metal grating is fabricated by a lossless, precisely aligned polymer assisted transfer method, and the Si3N4 grating combined with the silicon nanowire effectively enhances the photocurrent of the transverse electric polarized light (Nano lett, 2017,17,12, 7731-. Patolsky and Yaish et al report a spectrally gated field effect transistor detector with a subminiature red-green-blue-violet filter. These photodetectors are based on silicone nanowire hybrid field effect transistor devices, capable of detecting specific visible wavelength spectra below the half-peak 100 nm. These highly compact, spectrally controlled nanodevices are likely to be used in a variety of new optoelectronic devices in the future (Nano Lett.2018,18,1, 190-.
Chinese patent CN201510194017.X prepares silicon nanowire with surface modified with 4-amino-1, 8-naphthamide fluorophore, and further reacts with sodium nitrite and sodium azide to nitridize amino groups, so as to obtain the silicon nanowire-based hydrogen sulfide fluorescence chemical sensor. Chinese patent CN201910579528.1 obtains a silicon nanowire chip with a tip by carrying out metal-assisted etching and alkali etching on a monocrystalline silicon wafer after surface washing pretreatment. Chinese patent cn201010618787.x deposits a first silicon dioxide layer, a second silicon dioxide layer and a silicon nitride layer on a single crystal silicon substrate, respectively, and forms silicon nanowires after etching respectively. The preparation method of the silicon nanowire disclosed above mainly focuses on a laser ablation method, a chemical vapor deposition combined chemical etching method, a metal assisted etching method and the like, and the used raw materials and equipment are expensive and the preparation process is complicated. Therefore, there is still a need to continuously explore the development of novel methods for preparing silicon nanowires.
Disclosure of Invention
The present invention is directed to overcoming the above-mentioned disadvantages of the prior art and providing a silicon nanowire array and a method for fabricating the same.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
a preparation method of a silicon nanowire array comprises the following steps:
1) mixing diatomite and sodium alginate, adding water, and grinding to obtain precursor slurry;
2) uniformly coating the precursor on a copper foil, and drying;
3) sequentially stacking the dried copper foil, the polyimide film and the metal lithium sheet, packaging in an argon or nitrogen atmosphere, and injecting a carbonate mixed liquid;
4) and (3) charging and discharging the packaged product for a plurality of times, then taking out the copper foil, washing the copper foil for a plurality of times by using ethylene carbonate and deionized water in sequence, and removing the copper foil after drying to obtain the silicon nanowire array.
Further, in the step 1), the diatomite is pretreated by the following steps: mixing and grinding an industrial grade diatomite raw material, sodium chloride and magnesium powder according to the mass ratio of 1 (1-3) to 1-3, calcining for 1-3 hours at 500-700 ℃ in an argon atmosphere, and then pickling, washing and vacuum drying.
Further, in the step 1), the mass ratio of the diatomite to the sodium alginate is 9 (0.5-1), and the grinding time is 10-30 minutes.
Further, in the step 1), the amount of deionized water added per 100mg of diatomite is 1-3 mL.
Further, in the step 2), the thickness of the copper foil is 10-15 μm.
Further, in the step 3), the carbonate mixed liquid includes ethylene carbonate containing lithium bistrifluoromethylsulfonyl imide, diethyl carbonate and a mixed solution thereof.
Further, in the step 3), every 2cm2The addition amount of the copper foil corresponding to the carbonate mixed liquid is 0.5-1 mL.
Further, in the step 4), the voltage range during charging and discharging is 1-3V, the charging and discharging times are 20-40 times, and the vacuum drying time is 6-8 hours.
Further, in the step 2), the drying conditions are as follows:
pre-drying at 60 ℃ for 20-40 minutes, and then vacuum drying at 60-80 ℃ for 10-12 hours.
Compared with the prior art, the silicon nanowire array prepared by the preparation method provided by the invention has the following beneficial effects:
the preparation method of the silicon nanowire array has the advantages that the used raw materials are common and easily-obtained industrial products, the equipment is simple, the preparation process is simple and convenient, the repeatability is high, the problems that the raw materials and the equipment of the conventional preparation method are expensive, the preparation process is complex and the like are solved, and the preparation method is a brand-new preparation method of the silicon nanowire.
The silicon nanowire array has the advantages of distinct appearance characteristics, diameter of about 50nm, and regular array arrangement of the whole silicon nanowire array, and has a wide application prospect in the aspects of nano electronic devices, optoelectronic devices, new energy and the like.
Drawings
FIG. 1 is an XRD pattern of a silicon nanowire array of example 1;
FIG. 2 is a scanning electron micrograph of a silicon nanowire array of example 1.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the accompanying drawings:
example 1
Mixing 90mg of pretreated diatomite and 10mg of sodium alginate, adding 1mL of deionized water, grinding for 20 minutes to obtain precursor slurry, uniformly coating the precursor slurry on a copper foil with the thickness of 15 mu m, pre-drying for 40 minutes at 60 ℃, and then drying for 10 hours in vacuum at 80 ℃. And then, sequentially stacking a copper foil, a polyimide film and a metal lithium sheet, packaging in an argon atmosphere, injecting 0.5mL of a mixed solution containing ethylene carbonate and diethyl carbonate of lithium bis (trifluoromethyl) sulfonyl imide according to a volume ratio of 1:1, charging and discharging the packaged product for 40 times under the voltage range of 1-3V, taking out the copper foil containing the silicon substance, sequentially washing the copper foil with ethylene carbonate and deionized water for several times, carrying out vacuum drying at 60 ℃ for 8 hours, and removing the copper foil to obtain the product. The diatomite is pretreated by the following steps: mixing and grinding industrial grade diatomite raw material, sodium chloride and magnesium powder according to the mass ratio of 1:1:1, calcining for 3 hours at 500 ℃ in an argon atmosphere, and then pickling, washing and vacuum drying.
Fig. 1 is an XRD pattern of the silicon nanowire array prepared in example 1, where XRD diffraction peaks at 28 °, 47 °, and 56 ° 2 θ correspond to cubic phase silicon, and the remaining XRD diffraction peaks marked with asterisks correspond to glass slides.
Referring to fig. 2, fig. 2 is a scanning electron microscope image of the product of example 1, and the prepared nanowires have distinct morphology and characteristics, have a diameter of about 50nm, and are arranged in a regular array as a whole.
Example 2
Mixing 90mg of pretreated diatomite and 5mg of sodium alginate, adding 3mL of deionized water, grinding for 10 minutes to obtain precursor slurry, uniformly coating the precursor slurry on a copper foil with the thickness of 10 mu m, pre-drying for 20 minutes at 60 ℃, and then drying for 12 hours in vacuum at 60 ℃. And then sequentially stacking the copper foil, the polyimide film and the metal lithium sheet, packaging in a nitrogen atmosphere, injecting 1mL of ethylene carbonate solution containing lithium bis (trifluoromethyl) sulfonyl imide, charging and discharging the packaged product for 20 times under the voltage range of 1-3V, taking out the copper foil containing the silicon substance, sequentially washing the copper foil with ethylene carbonate and deionized water for several times, drying in vacuum at 80 ℃ for 6 hours, and removing the copper foil to obtain the product. The diatomite is pretreated by the following steps: mixing and grinding industrial grade diatomite raw material, sodium chloride and magnesium powder according to the mass ratio of 1:3:3, calcining for 1 hour at 700 ℃ under argon atmosphere, and then pickling, washing and vacuum drying.
Example 3
Mixing 90mg of pretreated diatomite and 8mg of sodium alginate, adding 2mL of deionized water, grinding for 30 minutes to obtain precursor slurry, uniformly coating the precursor slurry on a copper foil with the thickness of 14 mu m, pre-drying for 30 minutes at 60 ℃, and then drying for 11 hours in vacuum at 70 ℃. And then, sequentially stacking a copper foil, a polyimide film and a metal lithium sheet, packaging in an argon atmosphere, injecting 0.8mL of diethyl carbonate solution containing lithium bis (trifluoromethyl) sulfonyl imide, charging and discharging the packaged product for 30 times under the voltage range of 1-3V, taking out the copper foil containing the silicon substance, sequentially washing the copper foil with ethylene carbonate and deionized water for several times, carrying out vacuum drying at 70 ℃ for 7 hours, and removing the copper foil to obtain the product. The diatomite is pretreated by the following steps: mixing and grinding industrial grade diatomite raw material, sodium chloride and magnesium powder according to the mass ratio of 1:2:1, calcining for 1 hour at 600 ℃ under the argon atmosphere, and then pickling, washing and vacuum drying.
Example 4
Mixing 90mg of pretreated diatomite and 6mg of sodium alginate, adding 1mL of deionized water, grinding for 30 minutes to obtain precursor slurry, uniformly coating the precursor slurry on a copper foil with the thickness of 15 mu m, pre-drying for 40 minutes at 60 ℃, and then drying for 10 hours in vacuum at 80 ℃. And then, sequentially stacking a copper foil, a polyimide film and a metal lithium sheet, packaging in an argon atmosphere, injecting 0.6mL of a mixed solution containing ethylene carbonate and diethyl carbonate of lithium bis (trifluoromethyl) sulfonyl imide according to a volume ratio of 1:1, charging and discharging the packaged product for 40 times under a voltage range of 1-3V, taking out the copper foil containing the silicon substance, sequentially washing the copper foil with ethylene carbonate and deionized water for several times, drying the copper foil in vacuum at 80 ℃ for 6 hours, and removing the copper foil to obtain the product. The diatomite is pretreated by the following steps: mixing and grinding industrial grade diatomite raw material, sodium chloride and magnesium powder according to the mass ratio of 1:1:1, calcining for 1 hour at 600 ℃ under the argon atmosphere, and then pickling, washing and vacuum drying.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (10)
1. A preparation method of a silicon nanowire array is characterized by comprising the following steps:
1) mixing diatomite and sodium alginate, adding water, and grinding to obtain precursor slurry;
2) uniformly coating the precursor on a copper foil, and drying;
3) sequentially stacking the dried copper foil, the polyimide film and the metal lithium sheet, packaging in an argon or nitrogen atmosphere, and injecting a carbonate mixed liquid;
4) and (3) charging and discharging the packaged product for a plurality of times, then taking out the copper foil, washing the copper foil for a plurality of times by using ethylene carbonate and deionized water in sequence, and removing the copper foil after drying to obtain the silicon nanowire array.
2. The method for preparing silicon nanowire arrays as claimed in claim 1, wherein in step 1), diatomaceous earth is pretreated by: mixing and grinding an industrial grade diatomite raw material, sodium chloride and magnesium powder according to the mass ratio of 1 (1-3) to 1-3, calcining for 1-3 hours at 500-700 ℃ in an argon atmosphere, and then pickling, washing and vacuum drying.
3. The method for preparing the silicon nanowire array according to claim 1, wherein in the step 1), the mass ratio of the diatomite to the sodium alginate is 9 (0.5-1), and the grinding time is 10-30 minutes.
4. The method for preparing silicon nanowire array as claimed in claim 3, wherein the amount of deionized water added per 100mg of diatomaceous earth in step 1) is 1-3 mL.
5. The method for preparing a silicon nanowire array as claimed in claim 1, wherein in the step 2), the thickness of the copper foil is 10-15 μm.
6. The method for preparing a silicon nanowire array as claimed in claim 1, wherein the carbonate-based mixed liquid in step 3) comprises ethylene carbonate containing lithium bistrifluoromethylsulfonimide, diethyl carbonate and a mixed solution thereof.
7. The method for preparing silicon nanowire array as claimed in claim 1, wherein the step 3) is performed every 2cm2The addition amount of the copper foil corresponding to the carbonate mixed liquid is 0.5-1 mL.
8. The method for preparing a silicon nanowire array as claimed in claim 1, wherein in the step 4), the voltage range during charging and discharging is 1-3V, the number of charging and discharging times is 20-40, and the vacuum drying time is 6-8 hours.
9. The method for preparing a silicon nanowire array as claimed in claim 1, wherein in the step 2), the drying conditions are as follows:
pre-drying at 60 ℃ for 20-40 minutes, and then vacuum drying at 60-80 ℃ for 10-12 hours.
10. A silicon nanowire array produced by the production method according to any one of claims 1 to 9.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115010397A (en) * | 2022-06-24 | 2022-09-06 | 陕西科技大学 | Diatomite foaming agent and preparation method thereof |
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| CN106025242A (en) * | 2016-07-29 | 2016-10-12 | 成都新柯力化工科技有限公司 | Silicon alloy nano-wire compound negative electrode material for lithium-ion battery and preparation method thereof |
| CN106941153A (en) * | 2017-01-19 | 2017-07-11 | 江永斌 | Flocculence elemental silicon nanowire cluster/carbon compound cathode materials and preparation method and purposes |
| CN111106391A (en) * | 2019-12-11 | 2020-05-05 | 西安交通大学 | Preparation method and application of high-strength solid electrolyte membrane |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20130220821A1 (en) * | 2012-02-27 | 2013-08-29 | Los Alamos National Security, Llc | Article comprising silicon nanowires on a metal substrate |
| US20130252101A1 (en) * | 2012-03-21 | 2013-09-26 | University Of Southern California | Nanoporous silicon and lithium ion battery anodes formed therefrom |
| US20140154564A1 (en) * | 2012-11-30 | 2014-06-05 | Lg Chem, Ltd. | Anode active material for lithium secondary battery, preparation method thereof, and lithium secondary battery comprising the same |
| CN106025242A (en) * | 2016-07-29 | 2016-10-12 | 成都新柯力化工科技有限公司 | Silicon alloy nano-wire compound negative electrode material for lithium-ion battery and preparation method thereof |
| CN106941153A (en) * | 2017-01-19 | 2017-07-11 | 江永斌 | Flocculence elemental silicon nanowire cluster/carbon compound cathode materials and preparation method and purposes |
| CN111106391A (en) * | 2019-12-11 | 2020-05-05 | 西安交通大学 | Preparation method and application of high-strength solid electrolyte membrane |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115010397A (en) * | 2022-06-24 | 2022-09-06 | 陕西科技大学 | Diatomite foaming agent and preparation method thereof |
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