CN101798058B - Method for modifying surface heterogeneous medium of silica-based nanowire - Google Patents

Method for modifying surface heterogeneous medium of silica-based nanowire Download PDF

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CN101798058B
CN101798058B CN 201010126626 CN201010126626A CN101798058B CN 101798058 B CN101798058 B CN 101798058B CN 201010126626 CN201010126626 CN 201010126626 CN 201010126626 A CN201010126626 A CN 201010126626A CN 101798058 B CN101798058 B CN 101798058B
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nanowire
nano wire
silica
irradiation
tem
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CN101798058A (en
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朱贤方
苏江滨
李论雄
吴燕
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Xiamen University
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Xiamen University
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Abstract

The invention discloses a method for modifying a surface heterogeneous medium of a silica-based nanowire, relating to a method for modifying the surface of a nanowire. The method comprises the steps of the following steps of: putting a TEM (transmission electron microscopy) sample into a sample seat; pushing the sample into a sample room; vacuumizing the TEM; observing and screening the nanowire in the TEM sample; primarily screening the nanowire under the low-power observing mode of the TEM, wherein the screened nanowire is positioned in a micro grid hole; further screening the primarily-screened nanowire under the higher-power observing mode of the TEM, so that the surface of the nanowire is smooth and does not absorb with other solid impurities; shooting the topography of the unmodified screened nanowire segment with a CDC of an electric mirror; performing purpose irradiation to the nanowire according to the requirement of the modification; and recording the surface-modifying effect of the nanowire after irradiation in a shooting way. The method not only can easily control each irradiation parameter and have high controllability, but also can realize good contact and conglutination between the silica-based nanowire and each non-crystalline carbon nanometer structure.

Description

A kind of method for modifying surface heterogeneous medium of silica-based nanowire
Technical field
The present invention relates to a kind of surface modification method of nano wire, especially relate to a kind of method for modifying surface heterogeneous medium of silica-based nanowire.
Background technology
Modify in processing technology at present nano wire, in the transmission electron microscope of field, the high-energy focusing electron beam irradiation is a kind of means that are in daily use, it not only can realize cutting, punching, the welding of nano wire, and the change of the pattern such as length, diameter, flexibility, but also can be in the nanostructured (modifying surface heterogeneous medium) of other element of nanowire surface induction and deposition.for the former, existing document existing than systematic research (referring to document: 1. Su Jiang shore, master thesis, 2008, Xiamen: Xiamen University, 2.Xu S Y, Tian M L, Wang J G et al, Small, 2005,1 (12): 1221, 3. permitted victory brave, electron microscopic journal, 2007,26:563, 4.Remeika M, Bezryadin A, Nanotech., 2005,16:1172, 5.Kondo Y, Takayanagi K, Phys.Rev.Lett., 1997,79:3455), for the latter, bibliographical information also seldom at present, only find that Wang Ming give birth to wait that (referring to document: 6. Wang Ming gives birth to, Wang Jingyun, Chen Qing, Peng practices lance, the electron microscopic journal, 2005, 24:11) method by manual electron beam motion has deposited the carbon nano dot respectively on little grid carbon film and many walls carbon pipe, carbon nanocoils, at the ZnO nano-wire surface deposition one deck amorphous carbon film (nano wire modification), and Wang Y G etc. is (referring to document: 7.Wang Y G, Zuo B S, Wang T H etal, J.Phys.Chem.C, 2008, 112:7572) utilize accurate focused beam (beam spot diameter, 200nm) to deposit one deck hydrocarbon film in the ZnSe nanowire surface.Yet, although Wang Mingsheng etc. utilize the method for manually controlling the electron beam motion simple, but in practical operation, the stability of electron beam moving direction and bundle spot were difficult to accurately control in the time of staying of each point, cause that the general thickness of the carbon nanocoils that grows out is uneven, axial bending and surface irregularity, the film thickness uniformity of the amorphous carbon film that the ZnO nano-wire surface deposits also is difficult to control, thereby may bring uncertainty or stay hidden danger in the practical application of nano-device.And, above-mentioned Wang Ming gives birth to wait and utilizes method that method that manual focused beam moves along nanowire surface and Wang Y G etc. utilize large beam spot electronic beam irradiation nano wire respectively at the relative film uniformly of nanowire surface deposition a layer thickness, but they are all had no idea at the controlled amorphous carbon-film of nanowire surface deposition one deck thickness local.In addition, the heterogeneous modification of above-mentioned only nanowire surface is not as modifying object with silica-based nanowire.
Summary of the invention
Purpose of the present invention aims to provide a kind of method for modifying surface heterogeneous medium of silica-based nanowire.
Technical scheme of the present invention is that organic gas molecule residual in the transmission electron microscope is as presoma, utilize transmission electron microscope fixed point irradiation and automatic orientation line to sweep function, in the amorphous carbon nanostructured of the silica-based nanowire surface various patterns of arbitrary assigned address controllable deposition and size, thereby realize the method for the silica-based nanowire controlled heterogeneous modification in surface.
The present invention includes following steps:
1) dress sample: the TEM sample is put into specimen holder, then specimen holder is pushed in the sample room, and transmission electron microscope is vacuumized, the nano wire in the TEM sample is observed screening;
2) screening of nano wire: first under TEM low power observing pattern, nano wire is carried out primary election, selected nano wire is arranged in little grid holes, then under higher multiple observing pattern, just selected nano wire is done further screening, make nanowire surface smooth and absorption other solid impurity is arranged;
3) modification of nano wire: first take with the subsidiary CCD of Electronic Speculum the pattern of modifying front selected nano wire fragment, then according to the needs of modifying, nano wire is carried out purposive irradiation, the finishing effect of Taking Pictures recording nano wire after irradiation is completed.
In step 1) in, describedly vacuumize that can to control vacuum be 10 -4~10 -5Pa; It is the Tecnai F30 field transmission electron microscope of 300kV that described transmission electron microscope can adopt accelerating potential; Described TEM sample can scrape the silica-based nanowire powder from silicon chip substrate, and described silica-based nanowire can be Si nano wire or SiO xNano wire etc.; If described silica-based nanowire Si nano wire, described TEM sample can scrape the silica-based nanowire powder from silicon chip substrate, first corrode with hydrofluoric acid under ultrasonic vibration, remove the oxide layer on surface, then disperse with organic solvent under ultrasonic vibration, when aggregate fully disperseed and form the uniform suspension of color, the organic solution that will contain nano wire dripped to on the copper mesh of little grid carbon film, dry or dry after namely get the TEM sample; Described organic solvent can be selected absolute ethyl alcohol or acetone etc.
In step 2) in, described TEM low power observing pattern can be selected 6000 * left and right, and described primary election can be according to the needs of finishing, and preferably selecting pattern is that two ends are fixed and axial straight nano wire with being of a size of 10~100nm; Described higher multiple observing pattern can select 20000 *~150000 *.
In step 3) in, the multiplication factor of described Electronic Speculum can be 20000 *~150000 *; Described irradiation can adopt following methods: 1. under the focused beam fixed point irradiation of beam spot size less than nanowire diameter, come the deposit carbon nano particle by controlling beam spot size and exposure time, realize that carbon nano-particle is to the heterogeneous modification of the controlled surface of silica-based nanowire; 2. less than the focused beam of nanowire diameter, nano wire is carried out direct line when sweeping when beam spot size, sweep parameter (as beam spot size by control line, the direction that line is swept, speed and length etc.) deposit the carbon nano rod of various patterns, realize that carbon nano rod is to the heterogeneous modification of the controlled surface of silica-based nanowire; 3. under the focused beam fixed point irradiation of beam spot size greater than nanowire diameter, deposit the controlled amorphous carbon-film of thickness local and form coaxial configuration by controlling the parameters such as beam spot size, irradiation position and exposure time, realizing that amorphous carbon-film is to the heterogeneous modification of the controlled surface of silica-based nanowire.
the present invention adopts focused beam induced carbon deposition to realize the silica-based nanowire controlled heterogeneous modification in surface, under the high-energy focusing electron beam irradiation, the organic gas molecular breakdown of nanowire surface is amorphous carbon and is deposited on nanowire surface and is subjected to the irradiation position in irradiation zone, and along with the increase of exposure time, in irradiation zone, the organic gas molecule of nanowire surface is not only decomposed gradually fully, under the driving of concentration gradient, within near irradiation zone, the organic gas molecule of nanowire surface will constantly be diffused into bundle spot irradiation zone along nanowire surface, and decompose under focused beam irradiation and further deposit.The parameters such as the beam spot size of focused beam, radiation mode (fixed point irradiation or direct line sweep etc.) and exposure time will comprehensively determine pattern and the size of the amorphous carbon nanostructured that deposits.Therefore can deposit the amorphous carbon nanostructured (comprising the amorphous carbon-film of carbon nano-particle, carbon nano rod, local projection etc.) of various patterns, size at the arbitrary assigned address of nanowire surface by controlling the parameters such as beam spot size, radiation mode, exposure time and irradiation position, thereby realize the controlled heterogeneous modification of nanowire surface.in addition, the present invention adopts in a transmission Electronic Speculum high-energy focusing electron beam irradiation as the modification means, it not only can high-resolution home position observation nano wire the finishing effect, but also can induce particularly non-crystalline silicon base nano-wire of silica-based nanowire, and the amorphous carbon nanostructured surface shows very strong surface plasticity rheology or moistening effect (referring to document: 1. Su Jiang shore, master thesis, 2008, Xiamen: Xiamen University), thereby realize good contact and the adhesion of silica-based nanowire and amorphous carbon nanostructured, this is to weigh another important indicator that nanowire surface is modified quality except controllability.
Description of drawings
Fig. 1 be in embodiment 1 the amorphous carbon nano particle to amorphous SiO xThe heterogeneous modification of the controlled surface of nano wire.
Fig. 2 be in embodiment 2 the amorphous carbon nanometer rods to amorphous SiO xThe heterogeneous modification of the controlled surface of nano wire.
Fig. 3 be in embodiment 3 at the amorphous carbon-film of irradiation position local projection to the heterogeneous modification of the controlled surface of single crystalline Si nano wire.
The specific embodiment
The invention will be further described by reference to the accompanying drawings below by embodiment.
Embodiment 1:
1) preparation of TEM sample:
First scrape a little SiO with blade from silicon chip substrate xThe nano wire powder (<<1mg), then (power=150W, frequency=42kHz) the lower absolute ethyl alcohol (mass fraction 〉=99.7%) of using disperses 10min, then will contain SiO with liquid-transfering gun in ultrasonic vibration xThe ethanolic solution of nano wire drips 2 and drips to on the copper mesh of little grid carbon film, namely gets the TEM sample after standing 15min dries.
2) dress sample:
First with tweezers, the ready TEM sample of step 1 is put into specimen holder and fix, then specimen holder progressively is pushed in the sample room, and transmission electron microscope is evacuated to 10 -5Pa.
3) screening of nano wire:
The amorphous SiO that the present embodiment is selected xThe nano wire two ends all are fixed on carbon film, smooth surface, and even thickness radially, axially straight and be arranged in little grid holes.
4) modification of nano wire:
As Fig. 1 (a) with (b), be about respectively at beam spot size under the focused beam fixed point irradiation of 15nm and 35nm, by changing exposure time (t 1: t 2: t 3=10s:15s:30s, t 4: t 5: t 6=60s:110s:160s), at the amorphous SiO of diameter 40nm xNanowire surface is subjected to the irradiation position amorphous carbon nano particle of all having distinguished controllable deposition.Specifically, when exposure time more in short-term, carbon nano-particle just forms, the size of its size and bundle spot is very near (as particle 1, approximately 17nm), beam spot size has directly determined the size of carbon nano-particle at the beginning of forming.But along with the increase of exposure time, particle can further be grown up (from particle 1 to particle 3, or from particle 4 to particle 6), and its size even surpasses the diameter (as particle 6, approximately 65nm) of nano wire.Therefore, under the focused beam fixed point irradiation of beam spot size less than nanowire diameter, can deposit easily the amorphous carbon nano particle of suitable dimension by controlling beam spot size and exposure time, realize that carbon nano-particle is to the controlled surface modification of nano wire.In Fig. 1, scale is 20nm.
Embodiment 2:
1) preparation of TEM sample:
With embodiment 1.
2) dress sample:
With embodiment 1.
3) screening of nano wire:
With embodiment 1.
4) modification of nano wire:
As shown in Fig. 2 (a), when beam spot size approximately the focused beam of 30nm along the amorphous SiO of diameter 40nm xThe radial direction of nano wire carries out from nano wire one side direction opposite side that when line is swept, (line is swept approximately 40nm of length, line is swept approximately 10nm/min of speed), nanowire surface is subjected to the irradiation position to deposit a diameter and restraints the much bigger amorphous carbon nanometer rods of spot (approximately 45nm, see Fig. 2 (b)).And sweep length when increasing to 100nm (line is swept approximately 20nm/min of speed) when beam spot size is reduced to 20nm, line, and as shown in Fig. 2 (c), the amorphous SiO of diameter 46nm xThe surface of nano wire and side are swept direction along the line and are grown a diameter and restraint the bigger amorphous carbon nanometer rods of spot (approximately 24nm, see Fig. 2 (d)).It should be noted that as shown in Fig. 2 (d), far away apart from the side surface of nano wire, carbon nano rod is just thinner, and the carbon deposition just more is not easy in other words.Therefore, when beam spot size carries out direct line when sweeping less than the focused beam of nanowire diameter to nano wire, can sweep parameter (as beam spot size by control line easily, the direction that line is swept, speed and length etc.) deposit the amorphous carbon nanometer rods of various patterns, realize that carbon nano rod modifies the controlled surface of nano wire.In Fig. 2, scale is 20nm.
Embodiment 3:
1) preparation of TEM sample:
First with blade from silicon chip substrate scrape a little single crystalline Si nano wire powder (<<1mg), then at ultrasonic vibration (power=150W, frequency=42kHz) lower to 5% hydrofluoric acid corrosion 10min, again at ultrasonic vibration (power=150W, frequency=42kHz) lower to absolute ethyl alcohol (mass fraction 〉=99.7%) dispersion 10, the ethanolic solution that will contain the Si nano wire with liquid-transfering gun at last drips 2 and drips to on the copper mesh of little grid carbon film, namely gets the TEM sample after standing 15min dries.
2) dress sample:
With embodiment 1.
3) screening of nano wire:
The selected single crystalline Si nano wire two ends of the present embodiment all are fixed on carbon film, smooth surface, and even thickness radially, axially straight and be arranged in little grid holes.
4) modification of nano wire:
As shown in Fig. 3 (a), when beam spot size approximately the Electron Beam Focusing of 90nm when irradiation is fixed a point at the center of the single crystalline Si nano wire of diameter 63nm, the nano wire periphery has deposited one deck at the amorphous carbon-film that is subjected to irradiation position local projection, thereby forms the coaxial configuration of local enlargement.And be reduced to 70nm when beam spot size, as shown in Fig. 3 (b), successively when irradiation is fixed a point in the position 1 of the single crystalline Si nano wire of diameter 55nm and position 2, similarly, obtained two and be in the coaxial configuration that is subjected to irradiation position local enlargement.Further, a series of continuous TEM photos (not providing) show, exposure time is longer, and the amorphous carbon surface film is thicker.Therefore, under the focused beam fixed point irradiation of beam spot size greater than nanowire diameter, can deposit the controlled amorphous carbon-film of various thickness locals and form coaxial configuration by controlling the parameters such as beam spot size, irradiation position and exposure time easily, realize that amorphous carbon-film is to the controlled surface modification of nano wire.In Fig. 3, (a) scale is 20nm, and (b) scale is 50nm.
In above-mentioned 3 embodiment, find also after irradiation that nanowire surface also more or less all deposits amorphous carbon-film and (sees Fig. 1 (a) and (b) in the unirradiated position, Fig. 2 (b) and (d), Fig. 3 (a) and (b)), it is an interference or injury that this controlled surface to nano wire is modified, can take some effective measures in experiment, as enlarge under observing pattern the size of bundle spot or shorten time etc. of electron microscopic observation, avoid the uncontrollable deposition of unirradiated position amorphous carbon-film as far as possible; The existence of nanowire surface amorphous carbon-film makes nano wire form a kind of " nano wire---amorphous carbon-film " nucleocapsid structure or coaxial configuration, thereby may have physics, the chemical property that more is better than common nano wire but from another perspective.

Claims (4)

1. the method for modifying surface heterogeneous medium of a silica-based nanowire is characterized in that comprising the following steps:
1) dress sample: the TEM sample is put into specimen holder, then specimen holder is pushed in the sample room, and transmission electron microscope is vacuumized, the nano wire in the TEM sample is observed screening; Described silica-based nanowire is Si nano wire or SiO xNano wire; Described TEM sample is to scrape the silica-based nanowire powder from silicon chip substrate, first corrode with hydrofluoric acid under ultrasonic vibration, remove the oxide layer on surface, then disperse with organic solvent under ultrasonic vibration, when aggregate fully disperses and form the uniform suspension of color, the organic solution that will contain nano wire drips to on the copper mesh of little grid carbon film, dry or dry after namely get the TEM sample;
2) screening of nano wire: first under TEM low power observing pattern, nano wire is carried out primary election, selected nano wire is arranged in little grid holes, then under higher multiple observing pattern, just selected nano wire is done further screening, make nanowire surface smooth and absorption other solid impurity is arranged; Described TEM low power observing pattern is selected 6000 * left and right, and described primary election is the needs according to finishing, and selecting pattern is that two ends are fixed and axial straight nano wire with being of a size of 10~100nm; Described higher multiple observing pattern selects 20000 *~150000 *;
3) modification of nano wire: first take with the subsidiary CCD of Electronic Speculum the pattern of modifying front selected nano wire fragment, then according to the needs of modifying, nano wire is carried out purposive irradiation, the finishing effect of Taking Pictures recording nano wire after irradiation is completed; Described irradiation adopts following methods: 1. under the focused beam fixed point irradiation of beam spot size less than nanowire diameter, come the deposit carbon nano particle by controlling beam spot size and exposure time, realize that carbon nano-particle is to the heterogeneous modification of the controlled surface of silica-based nanowire; 2. less than the focused beam of nanowire diameter, nano wire is carried out direct line when sweeping when beam spot size, sweep the parameter beam spot size by control line, the direction that line is swept, speed and length deposit the carbon nano rod of various patterns, realize that carbon nano rod is to the heterogeneous modification of the controlled surface of silica-based nanowire; 3. under the focused beam fixed point irradiation of beam spot size greater than nanowire diameter, deposit the controlled amorphous carbon-film of thickness local and form coaxial configuration by controlling beam spot size, irradiation position and exposure time, realizing that amorphous carbon-film is to the heterogeneous modification of the controlled surface of silica-based nanowire.
2. the method for modifying surface heterogeneous medium of a kind of silica-based nanowire as claimed in claim 1, is characterized in that in step 1) in, described vacuumizing is that control vacuum is 10 -4~10 -5Pa.
3. the method for modifying surface heterogeneous medium of a kind of silica-based nanowire as claimed in claim 1, is characterized in that in step 1) in, it is the Tecnai F30 field transmission electron microscope of 300kV that described transmission electron microscope adopts accelerating potential.
4. the method for modifying surface heterogeneous medium of a kind of silica-based nanowire as claimed in claim 1, is characterized in that in step 1) in, described organic solvent is selected absolute ethyl alcohol or acetone.
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