CN100336722C - One-dimensional ring shaped Nano silicon material and preparation - Google Patents
One-dimensional ring shaped Nano silicon material and preparation Download PDFInfo
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- CN100336722C CN100336722C CNB2005100658159A CN200510065815A CN100336722C CN 100336722 C CN100336722 C CN 100336722C CN B2005100658159 A CNB2005100658159 A CN B2005100658159A CN 200510065815 A CN200510065815 A CN 200510065815A CN 100336722 C CN100336722 C CN 100336722C
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Abstract
The present invention relates to a silicon nanometer material in a one-dimensional bamboo joint shape and a preparation method. The material has a structure in a one-dimensional line shape, the outside diameter of the material is from 50 to 200 nm, and the inner part has a hollow structure in a bamboo joint shape. The preparation method comprises the following steps: a porous alumina template is prepared by an anodic oxidation method; gold is deposited at the bottom of the hole of the template by an alternating current deposition method; the template is dissolved by a NaOH solution, nanometer stage gold particles are left, and the gold particles are pumped, filtered and washed by distilled water; the gold particles are transferred to absolute alcohol to form a gold monodisperse solution used as the disperser of the absolute alcohol; a porcelain boat loading gold catalyst is used as a substrate for growing silicon and is put into the center of a tubular furnace, the mixed gas of SiH4 and H2 is led into the tubular furnace, a yellowy silicon nanometer material in a one-dimensional bamboo joint shape is formed on the inner wall of the porcelain boat, SiH4 gas is closed, the heating is stopped, and the material naturally cools to be at indoor temperature; the reaction process is over.
Description
Technical field
The present invention relates to a kind of silicon nano material, especially relate to a kind of one-dimensional ring shaped Nano silicon material and preparation method thereof.
Background technology
Since S.Iijima (S.Iijima in 1991, Nature 1991,354,56.) synthesized since the carbon nanotube, because potential application prospect aspect nanoelectronics, monodimension nanometer material, the especially preparation research of one dimension semiconductor nano material have become a hot fields of current nanosecond science and technology.Because silicon (Si) is most widely used material in semi-conductor industry and the microelectronics, simultaneously, the emission on the scene of the monodimension nanometer material of silicon, aspect such as luminous have shown some unique good character, so the study on the synthesis of the one dimension Nano structure of relevant silicon enjoys scientist's concern always.
People such as the Lieber of Harvard University (A.M.Morales, C.M.Lieber, Science 1998,279,208.) utilize the method for laser auxiliary catalysis growth (Laser-assisted Catalytic Growth), prepare silicon nanowires (SiNWs) with single crystal structure.Its method is earlier silica flour to be mixed with a spot of catalyzer (as iron, gold etc.) and be pressed into target, under certain density reducing atmosphere, ablates with laser.The prepared silicon nanowires diameter that goes out is 6～20nm, and length is greater than 1 μ m.In initial nucleation and propagation process owing to will follow the principle of minimum interfacial free energy, therefore the direction of growth of the silicon nanowires for preparing of this method be basically＜111.Simultaneously, (the Y.Cui of this research group, L.J.Lauhon, M.S.Gudiksen, J.Wang, C.M.Lieber, Appl.Phys.Lett.2001,78,2214.) also adopt the method for metal catalytic chemical vapour deposition (Metal-catalyzed Chemical Vapor Deposition) to prepare silicon nanowires.As the silicon source, the monodispersed gold nano grain for preparing in advance reacts under certain vacuum tightness and temperature (450～600 ℃) as catalyzer with silane.This method has demonstrated selectivity and controllability preferably, can control the size of silicon nanowires diameter by the size of regulating granules of catalyst.More than the foundation of two kinds of methods, basically be based on gas-liquid-solid growth (Vapor-Liquid-SolidGrowth) model, referring to (R.S.Wagner, W. C.Ellis, Appl.Phys.Lett.1964,4,89.), at first, the silicon source exists with the gasiform form under the condition of laser radiation or pyrolytic decomposition, when gaseous atom runs into catalyzer, with the liquid minimum eutectic of catalyzer formation specified proportion; Then, because silicon source sustainable supply, silicon is just constantly separated out from minimum eutectic; The final silicon nano material that forms with one dimension linear structure.People such as the Li Shutang of City University of Hong Kong (R.Q.Zhang, Y.Lifshitz, S.T.Lee, Adv.Mater, 2003,7-8,635) adopt oxide compound assisting growth method (Oxide Assisted Growth, OAG) preparation silicon nanowires.This group is mixed high-purity silicon or its oxide powder by a certain percentage with metal catalyst powder, under 1100～1400 ℃ temperature, carry out thermal evaporation, 900～1100 ℃ of temperature ranges, discovery has the silicon nanowires of a large amount of crystalline state to generate, and the product of gained has the diameter of comparison homogeneous.In addition, people such as Zhang Lide (X.Y.Zhang, L.D, Zhang, Adv.Mater, 2001,13,16,1328.) utilize porous anodic aluminium oxide as template, as catalyzer, successfully prepare the silicon nanowire array of high-sequential with gold.People such as Zhu (J.Luo, L.Zhang, Y.J.Zhang, J.Zhu, AdvMater.2002,14,1413.) utilize the corrosion of hydrofluoric acid to silicon chip, prepare silicon nanowires, and this method is simple, but controllability is relatively poor, and the diameter of nano wire is bigger.Because Siliciumatom becomes the key characteristic to determine it to tend to sp3 hydridization, be difficult point so have the silicon nano material of hollow structure synthetic always.People such as Yang (J.Sha, J.Niu, X.Ma, J.Xu, X.Zhang, Q.Yang, D.Yang, Adv.Mater, 2002,14,1219.) prepare the crystalline silicon nanotube (Silicon nanotubes) with consistent size first with alumina formwork.People such as Lee (W.Shi, H.Peng, N.Wang, C.P.Li, L.Xu, C.S.Lee, R.Kalish, S.T.Lee, J.Am.Chem.Soc.2001,123,11095-11096.) then utilize OAG successfully to prepare along the silicon nano belt (Silicon nanoribbons) of＜110〉direction growths.
Summary of the invention
The present invention aims to provide hollow silicon nano material of a kind of one dimension ring shape and preparation method thereof.
The said one-dimensional ring shaped Nano silicon material of the present invention is the material with one dimension linear structure, and outside diameter is 50～200nm.Inside is hollow structure, and the boring structure is a bamboo knot shaped structure, and said bamboo knot shaped structure internal diameter is 10～150nm, is shaped as pyrometric cone or trapezoidal tapers or and the cavity of analogue and axis ordered arrangement along the line.
Preparation method's concrete steps of the said one-dimensional ring shaped Nano silicon material of the present invention are as follows: 1) adopt anode oxidation method to prepare porous alumina formwork; 2) use the alternating-current deposition method, at the hole bottom deposit layer of metal gold of porous alumina formwork; 3) with NaOH solution template is dissolved fully, stay and have nano level gold grain, and the distilled water suction filtration cleans, gold grain is transferred in the dehydrated alcohol, form dehydrated alcohol and make the monodisperse liquor of the gold of dispersion agent, keep this solution and make the catalyzer of grown silicon nano material; 4) substrate of the porcelain boat of the said Au catalyst of step 3) as grown silicon will be housed, put it into tube furnace central authorities, feed the mixed gas of SiH4, H2, on the porcelain boat inwall, form the hollow silicon nano material of flaxen one dimension ring shape, close SiH4 gas, stop heating, naturally cool to room temperature, reaction process finishes.
Said employing anode oxidation method is prepared porous alumina formwork, can be the 0.3M oxalic acid solution in concentration, under 10 ℃ temperature, with the aluminium foil is anodal, with the platinized platinum is negative pole, adds the volts DS of 40V, forms the thick aluminum oxide (Al2O3) of 20～30 μ m at aluminium foil surface after 2～3 hours.
Said alternating-current deposition technique method is at the hole bottom deposit layer of metal gold of porous alumina formwork, be that the aluminium foil of aluminum oxide and platinized platinum are arranged is the two poles of the earth for surface attachment with the gained of step 1), electrolytic solution is hydrochloro-auric acid (HAuCl4) solution, concentration is 10-3M, voltage is 8～10V, frequency is 50Hz, and the time of galvanic deposit is 10～15 minutes.
The concentration of said NaOH solution is 0.1M.
In step 4), the temperature of tube furnace is 470 ℃, and pressure is 1050torr.The ratio of SiH4 and H2 mixed gas is SiH4: H2=2 by volume: 1, and total gas couette is controlled at 15～30sccm.The said entire reaction time that forms the hollow silicon nano material of flaxen one dimension ring shape on the porcelain boat inwall is 2～3 hours.
According to the prepared silicon nano material that goes out of the present invention, on form, show space one dimension form (outer appearnce is similar to wire), the diameter of this one-dimentional structure is 20～100nm, length can reach the hundreds of micron, but at upwards distributing the in an orderly manner cavity of tens nanoscale size of inner shaft, this cavity mostly is trilateral or half-oval shaped, or between between the two.The wide 50nm in cavity base, high about 70nm, and oriented unanimity, overall shape is similar to bamboo.Because the hole diameter of porous alumina formwork can be regulated and control according to the difference of synthesis condition in advance, just the size of catalyzer can change, so the diameter of this one dimension silicon nano material can be regulated and control to a certain extent artificially.Simultaneously, it is long more that mixed gas feeds the time, just the reaction times long more, then the length of this one-dimensional material is long more.
Up to now, also on all kinds of reference, find to have the monodimension nanometer material of the silicon of this form.And, the prepared material structure homogeneous that comes out, distribution of sizes is narrower, and productive rate is higher, does not contain other impurity substantially.Not hard to imagine, this unidimensional silicon nano material, the same with silicon nanowires and nano-tube, will certainly the potential application prospect be arranged in that nanoelectronic is technical.In addition, this method is comparatively simple, and plant and instrument is less demanding, is easy to grasp and control.
Description of drawings
Fig. 1 is the scanning electron microscope image of the said one-dimensional ring shaped Nano silicon material of the present invention.In Fig. 1, scale (a) is 2 μ m, and scale (b) is 200nm, and scale (c) is 100nm.
Fig. 2 is scanning transmission electron microscope (STEM) picture of the said one-dimensional ring shaped Nano silicon material of the present invention.In Fig. 2, arrow is depicted as the track of energy-spectrum scanning, and scale is 100nm.
Fig. 3 is the element distribution energy-spectrum scanning curve of the said one-dimensional ring shaped Nano silicon material of the present invention.In Fig. 3, the position (position) of electron beam process during X-coordinate representative scanning, unit is nm, ordinate zou is the signal relative intensity (intensity) that obtains.
Fig. 4 is under normal operation, the transmission electron microscope image of the said one-dimensional ring shaped Nano silicon material of the present invention.1., scale 2. is 20nm in Fig. 4,, scale 3. is 200nm.
Fig. 5 is under the condition that the SiH4 gas flow reduces, the transmission electron microscope image of the said one-dimensional ring shaped Nano silicon material of the present invention.In Fig. 5, scale 1. is 100nm, and scale 2. is 20nm, and scale 3. is 50nm.
Fig. 6 is in the reaction generating process, under the SiH4 gas flow situation from large to small, and the transmission electron microscope image of the said one-dimensional ring shaped Nano silicon material of the present invention.In Fig. 6, scale 1. is 0.5 μ m, and scale 2. is 100nm, and scale 3. is 5nm.
Fig. 7 is under the SiH4 flow condition that further change is big, the transmission electron microscope image of the said one-dimensional ring shaped Nano silicon material of the present invention.In Fig. 7, scale is 100nm.
Fig. 8 is when using less catalyzer, the transmission electron microscope image of prepared material.Scale is 50nm.
Fig. 9 is when using bigger catalyzer, the transmission electron microscope image of prepared material.Scale is 200nm.
Embodiment
Embodiment 1 adopts two step anonizings to prepare the alumina formwork of porous array structure.(thickness is 0.2mm with the aluminium foil cut out in advance, purity is 99.99%) in the mixing solutions of ethanol, trichloromethane and acetone (volume ratio is 1: 2: 1) carry out ultrasonic cleaning, in NaOH solution (concentration is 0.5M), soaked 10 minutes then, with distilled water that surface cleaning is clean.After above pre-treatment step finishes, aluminium foil is carried out electrochemical etching.Polishing is to carry out under the volts DS of 10V and 70 ℃ of water-baths, and polishing fluid is the mixed solution (volume ratio is 1: 1) of phosphoric acid and glycerine, and platinized platinum is a counter electrode, respectively at aluminium foil two towards right, the two sides of aluminium foil can be polished uniformly like this.Polishing time is generally at 10～15 minutes.Polished aluminium foil is put into 15 ℃ 0.3M oxalic acid solution, carries out anodic oxidation: be the centre that is placed on platinized platinum that aluminium foil is parallel equally, oxidation voltage is 40V, and oxidization time is about 2 hours.At this moment, the aluminium foil two sides forms uniformly, arranges orderly porous alumina membrane.
At room temperature carry out the alternating-current deposited gold with the alumina formwork that has just prepared, its device is identical with above-mentioned electrolytic cell device, and electrolytic solution is hydrochloro-auric acid (HAuCl4) solution, concentration is 10-3M, voltage is 8～10V, and frequency is 50Hz, and the time of galvanic deposit is 10～15 minutes.Then, the template of having plated gold is immersed in the NaOH solution of 0.1M, dissolves fully until template, stay mauve gold nano grain, suction filtration cleans several times, disperses with ethanol at last.
Adopt chemical vapour deposition technique to prepare one-dimensional ring shaped Nano silicon material.The clean porcelain boat that is attached with gold nano grain is put into the vitrified pipe central authorities of tube furnace.This system is a closed system, an end air inlet, and the other end and mechanical pump are to being connected.(SiH4: Ar=5: 95) as the silicon source, hydrogen is as the reaction carrier gas for silane gas.In order to guarantee the existence of system's no oxygen and other assorted gas, at first total system is vacuumized several times repeatedly before the reaction, heat up under hydrogen atmosphere according to pre-set program then, hydrogen flowing quantity is 30sccm, temperature rise rate is 4 ℃/min, rise to 650 ℃ and kept 2 hours, to guarantee the abundant activation of catalyzer.Afterwards, lower the temperature and remain on 470 ℃, begin to feed silane gas.This moment, silane flow rate was 10sccm, hydrogen flowing quantity 5sccm, and metering pin valve makes system pressure remain on 1050torr, and the reaction times is 2 hours.
Fig. 1 is scanning electronic microscope (SEM) picture of this material, and material presents the one dimension form as can be seen, and surface topography is smooth smooth, no any structure defective.Transmission electron microscope (TEM) picture by this material is cavity of periodic intervals arrangement in its inside as can be seen.Simultaneously, we find that the difference of granules of catalyst is determining the shape of cavity to a great extent, that is to say, can regulate and control the shape of cavity by the change to catalyst shape.Can determine that by the electronic energy spectrum (EDX) of this material the composition of material is an elemental silicon.The crystalline structure that can be drawn material by the regional image K-M (SAED) of this material is a non-crystalline state.Fig. 2,3 is respectively scanning transmission electron microscope (STEM) picture and the element distribution energy-spectrum scanning (Element Mapping) of this material, further specifies the specific form that is had of this material.
Under all constant situation of the condition (temperature, pressure) of embodiment 2 in embodiment 1, when beginning to react for 470 ℃, with the flow set of SiH4 is 5sccm, as shown in Figure 5, this moment, the product form changed, with the front form (as shown in Figure 4, the flow of SiH4 is 10sccm) internal cavities of comparing arranges tightr, textural defect appears in the interlayer between the cavity, even is interconnected, and is the tubulose of complete hollow.
Under all constant situation of the condition (temperature, pressure) of embodiment 4 in embodiment 1, when beginning to react for 470 ℃, with the flow set of SiH4 is 50sccm, as shown in Figure 7, at this moment, can not get the material of cavity structure, products therefrom becomes the silicon nanowires with complete solid construction by one-dimensional ring shaped Nano silicon material prepared among the embodiment 1 fully.
Embodiment 5 as previously mentioned, the diameter of this nano material can change by the change to the catalyzer size.In embodiment 1, when anodised voltage is transferred to 30V, other conditions are all identical in embodiment 1, the aperture of porous alumina diminishes, in subsequent step, the particle diameter of formed gold grain is decreased to 50nm, and as shown in Figure 8, this moment, the prepared material diameter that goes out became 40～50nm by 70～80nm among the embodiment 1.
It is in 6% phosphoric acid (H3PO4) solution that the aluminium foil of the surface attachment porous alumina membrane that embodiment 6 will prepare is immersed in concentration, time is about 30 minutes, by the aperture of tart corrosion expansion aluminum oxide hole, other experiment conditions are all identical in embodiment 1.As shown in Figure 9, this moment, prepared material diameter became 180～200nm by 70～80nm among the embodiment 1.
Claims (10)
1, one-dimensional ring shaped Nano silicon material is characterized in that outside diameter is 50～200nm in order to have the material of one dimension linear structure, and inside is hollow structure, and the boring structure is a bamboo knot shaped structure.
2, one-dimensional ring shaped Nano silicon material as claimed in claim 1 is characterized in that said bamboo knot shaped structure internal diameter is 10～150nm.
3, one-dimensional ring shaped Nano silicon material as claimed in claim 1 or 2, it is characterized in that said ring shape be shaped as pyrometric cone or trapezoidal tapers or and analogue, and the cavity of axis ordered arrangement along the line.
4, the preparation method of one-dimensional ring shaped Nano silicon material as claimed in claim 1 is characterized in that the steps include: 1) adopt anode oxidation method to prepare porous alumina formwork; 2) use the alternating-current deposition method, at the hole bottom deposit layer of metal gold of porous alumina formwork; 3) with NaOH solution template is dissolved fully, stay and have nano level gold grain, and the distilled water suction filtration cleans, gold grain is transferred in the dehydrated alcohol, form dehydrated alcohol and make the monodisperse liquor of the gold of dispersion agent, keep this solution and make the catalyzer of grown silicon nano material; 4) substrate of the porcelain boat of the said Au catalyst of step 3) as grown silicon will be housed, put it into tube furnace central authorities, feed SiH
4, H
2Mixed gas, on the porcelain boat inwall, form the hollow silicon nano material of flaxen one dimension ring shape, close SiH
4Gas stops heating, naturally cools to room temperature, and reaction process finishes.
5, the preparation method of one-dimensional ring shaped Nano silicon material as claimed in claim 4, it is characterized in that said employing anode oxidation method prepares porous alumina formwork, be meant that in concentration be the 0.3M oxalic acid solution, under 10 ℃ temperature, with the aluminium foil is anodal, with the platinized platinum is negative pole, adds the volts DS of 40V, forms the thick aluminum oxide of 20～30 μ m at aluminium foil surface after 2～3 hours.
6, the preparation method of one-dimensional ring shaped Nano silicon material as claimed in claim 4, it is characterized in that the hole bottom deposit layer of metal gold of said alternating-current deposition technique method at porous alumina formwork, be that the aluminium foil of aluminum oxide and platinized platinum are arranged is the two poles of the earth for surface attachment with the gained of step 1), electrolytic solution is chlorauric acid solution, concentration is 10-3M, voltage is 8～10V, and frequency is 50Hz, and the time of galvanic deposit is 10～15 minutes.
7, the preparation method of one-dimensional ring shaped Nano silicon material as claimed in claim 4, the concentration that it is characterized in that said NaOH solution is 0.1M.
8, the preparation method of one-dimensional ring shaped Nano silicon material as claimed in claim 4 is characterized in that in step 4), and the temperature of tube furnace is 470 ℃, and pressure is 1050torr.
9, the preparation method of one-dimensional ring shaped Nano silicon material as claimed in claim 4 is characterized in that in step 4) SiH
4And H
2The ratio of mixed gas is SiH by volume
4: H
2=2: 1, total gas couette is controlled at 15～30sccm.
10, the preparation method of one-dimensional ring shaped Nano silicon material as claimed in claim 4 is characterized in that in step 4), and the said entire reaction time that forms the hollow silicon nano material of flaxen one dimension ring shape on the porcelain boat inwall is 2～3 hours.
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| US8647436B2 (en) | 2008-04-02 | 2014-02-11 | Raytheon Company | Carbon ion beam growth of isotopically-enriched graphene and isotope-junctions |
| US8252115B2 (en) * | 2008-04-02 | 2012-08-28 | Raytheon Company | System and method for growing nanotubes with a specified isotope composition via ion implantation using a catalytic transmembrane |
| CN102145890A (en) * | 2011-04-30 | 2011-08-10 | 南京大学 | Preparation method of hollow spherical silicon nanomaterial |
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| CN1382627A (en) * | 2002-03-05 | 2002-12-04 | 浙江大学 | Process for preparing nano carbon tube |
| US6723624B2 (en) * | 2002-07-31 | 2004-04-20 | Industrial Technology Research Institute | Method for fabricating n-type carbon nanotube device |
| CN1545486A (en) * | 2001-07-27 | 2004-11-10 | �Ϻ���ͨ��ѧ | Production of carbon nanotubes |
| CN1548589A (en) * | 2003-05-19 | 2004-11-24 | 中国科学院物理研究所 | Production process of alumina template with nano holes |
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| CN1545486A (en) * | 2001-07-27 | 2004-11-10 | �Ϻ���ͨ��ѧ | Production of carbon nanotubes |
| CN1382627A (en) * | 2002-03-05 | 2002-12-04 | 浙江大学 | Process for preparing nano carbon tube |
| US6723624B2 (en) * | 2002-07-31 | 2004-04-20 | Industrial Technology Research Institute | Method for fabricating n-type carbon nanotube device |
| CN1548589A (en) * | 2003-05-19 | 2004-11-24 | 中国科学院物理研究所 | Production process of alumina template with nano holes |
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| Growth characteristics of silicon nanowires synthesized byvapor-liquid-solid growth in nanoporous alumina templates Kok.Keong Lew et al,Journal of Crystal Growth,Vol.254 2003 * |
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