CN101798058A - Method for modifying surface heterogeneous medium of silica-based nanowire - Google Patents
Method for modifying surface heterogeneous medium of silica-based nanowire Download PDFInfo
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- CN101798058A CN101798058A CN201010126626A CN201010126626A CN101798058A CN 101798058 A CN101798058 A CN 101798058A CN 201010126626 A CN201010126626 A CN 201010126626A CN 201010126626 A CN201010126626 A CN 201010126626A CN 101798058 A CN101798058 A CN 101798058A
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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
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 the processing technology at present nano wire, the high-energy focusing electron beam irradiation is a kind of means that are in daily use in the transmission electron microscope of field, it not only can realize cutting, punching, the welding of nano wire, and the change of 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 to win bravely 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, 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, deposited one deck amorphous carbon film (nano wire modification) in the ZnO nanowire surface, 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, though Wang Mingsheng etc. utilize the method for manually control electron beam motion simple, but in practical operation, the stability of electron beam moving direction and bundle spot all are difficult to accurately control in the time of staying of each point, cause the general thickness inequality of carbon nanocoils, axial bending and the surface irregularity that grow out, the film thickness uniformity of the amorphous carbon film that the ZnO nanowire surface is deposited 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 manual focused beam moves along nanowire surface and Wang Y G etc. to utilize the method for large beam spot electronic beam irradiation nano wire to deposit the relative film uniformly of a layer thickness in nanowire surface respectively, 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 to be presoma with organic gas molecule residual in the transmission electron microscope, utilize transmission electron microscope fixed point irradiation and automatic orientation line to sweep function, in the amorphous carbon nanostructured of silica-based nanowire surface various patterns of arbitrary assigned address controllable deposition and size, thus the method for the realization 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: under TEM low power observing pattern, nano wire is carried out primary election earlier, selected nano wire is arranged in little grid hole, under higher multiple observing pattern, just selected nano wire is done further screening then, make nanowire surface smooth and be not adsorbed with other solid impurity;
3) modification of nano wire: take the pattern of modifying preceding selected nano wire fragment with the subsidiary CCD of Electronic Speculum earlier, 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 finished then.
In step 1), 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, under ultrasonic vibration, corrode earlier with hydrofluoric acid, remove the oxide layer on surface, under ultrasonic vibration, disperse then with organic solvent, treat that aggregate fully disperses and when forming 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 promptly get the TEM sample; Described organic solvent can be selected absolute ethyl alcohol or acetone etc. for use.
In step 2) in, described TEM low power observing pattern can select 6000 for use * about, described primary election can be according to the needs of finishing, and preferably selecting pattern is that two ends are fixed and axially straight and be of a size of the nano wire of 10~100nm; Described higher multiple observing pattern can select 20000 *~150000 for use *.
In step 3), the multiplication factor of described Electronic Speculum can be 20000 *~150000 *; Described irradiation can adopt following method: 1. under the focused beam fixed point irradiation of beam spot size less than nanowire diameter, come the deposit carbon nano particle by control 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 parameters such as control beam spot size, irradiation position and exposure times, realize 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 the irradiation zone, and along with the increase of exposure time, the organic gas molecule of nanowire surface is not only decomposed gradually fully in the irradiation zone, under the driving of concentration gradient, the organic gas molecule of nanowire surface will constantly be diffused within the bundle spot irradiation zone along nanowire surface near the irradiation zone, and decompose under focused beam irradiation and further deposition.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 the pattern and the size of the amorphous carbon nanostructured that deposited.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 parameters such as control beam spot size, radiation mode, exposure time and irradiation positions, thereby realize the controlled heterogeneous modification of nanowire surface.In addition, the present invention adopts in the 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 that silica-based nanowire contacts and adhesion with the good of amorphous carbon nanostructured, this is to weigh another important indicator that nanowire surface is modified quality except that controllability.
Description of drawings
Fig. 1 be among the embodiment 1 the amorphous carbon nano particle to amorphous SiO
xThe heterogeneous modification of the controlled surface of nano wire.
Fig. 2 be among the embodiment 2 the amorphous carbon nanometer rods to amorphous SiO
xThe heterogeneous modification of the controlled surface of nano wire.
Fig. 3 be among the 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 in conjunction with the accompanying drawings below by embodiment.
Embodiment 1:
1) preparation of TEM sample:
Earlier scrape a little SiO from silicon chip substrate with blade
xThe nano wire powder (<<1mg), (power=150W, frequency=42kHz) disperse 10min with absolute ethyl alcohol (mass fraction 〉=99.7%) down will contain SiO with liquid-transfering gun again in ultrasonic vibration then
xThe ethanolic solution of nano wire drips 2 and drips to on the copper mesh of little grid carbon film, leaves standstill and promptly gets the TEM sample after 15min dries.
2) dress sample:
Earlier 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 with tweezers
-5Pa.
3) screening of nano wire:
The amorphous SiO that present embodiment is selected
xThe nano wire two ends all are fixed on the carbon film, smooth surface, and even thickness radially, axially straight and be arranged in little grid hole.
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 the about 40nm of diameter
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, about 17nm), beam spot size has directly determined the size at the beginning of the carbon nano-particle formation.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), its size even surpass the diameter (as particle 6, about 65nm) of nano wire.Therefore, under the focused beam fixed point irradiation of beam spot size, can deposit the amorphous carbon nano particle of suitable dimension easily by control beam spot size and exposure time, realize the controlled surface modification of carbon nano-particle nano wire less than nanowire diameter.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:
Shown in Fig. 2 (a), as the focused beam of the about 30nm of beam spot size amorphous SiO along the about 40nm of diameter
xThe radial direction of nano wire carries out from nano wire one side direction opposite side that (line was swept the about 40nm of length when line was swept, line is swept the about 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 (about 45nm sees Fig. 2 (b)).And sweep length when increasing to 100nm (line is swept the about 20nm/min of speed) when beam spot size is reduced to 20nm, line, and shown in Fig. 2 (c), the amorphous SiO of the about 46nm of diameter
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 (about 24nm sees Fig. 2 (d)).It should be noted that shown in Fig. 2 (d) far away more apart from the side surface of nano wire, carbon nano rod is just thin more, the carbon deposition just is not easy more 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:
Earlier with blade from silicon chip substrate scrape a little single crystalline Si nano wire powder (<<1mg), then at ultrasonic vibration (power=150W, frequency=42kHz) down with 5% hydrofluoric acid corrosion 10min, again at ultrasonic vibration (power=150W, frequency=42kHz) disperse 10 with absolute ethyl alcohol (mass fraction 〉=99.7%) down, the ethanolic solution that will contain the Si nano wire with liquid-transfering gun drips 2 and drips to on the copper mesh of little grid carbon film at last, leaves standstill and promptly gets the TEM sample after 15min dries.
2) dress sample:
With embodiment 1.
3) screening of nano wire:
The selected single crystalline Si nano wire two ends of present embodiment all are fixed on the carbon film, smooth surface, and even thickness radially, axially straight and be arranged in little grid hole.
4) modification of nano wire:
Shown in Fig. 3 (a), when irradiation is fixed a point at the center that the electron beam of the about 90nm of beam spot size focuses on the single crystalline Si nano wire of the about 63nm of diameter, 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, shown in Fig. 3 (b), successively when irradiation is fixed a point in the position 1 of the single crystalline Si nano wire of the about 55nm of diameter and position 2, similarly, obtained two and be in the coaxial configuration that is subjected to the local enlargement of irradiation position.Further, a series of continuous TEM photos (not providing) show that exposure time is long more, and the amorphous carbon surface film is thick more.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 parameters such as control beam spot size, irradiation position and exposure times easily, realize the controlled surface modification of amorphous carbon-film nano wire.In Fig. 3, (a) scale is 20nm, and (b) scale is 50nm.
In above-mentioned 3 embodiment, find also behind the 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 the experiment,, avoid the uncontrollable deposition of unirradiated position amorphous carbon-film as far as possible as size that enlarges bundle spot under the observing pattern or the time that shortens electron microscopic observation etc.; But from another angle, 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.
Claims (10)
1. the method for modifying surface heterogeneous medium of a silica-based nanowire is characterized in that may further comprise the 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: under TEM low power observing pattern, nano wire is carried out primary election earlier, selected nano wire is arranged in little grid hole, under higher multiple observing pattern, just selected nano wire is done further screening then, make nanowire surface smooth and be not adsorbed with other solid impurity;
3) modification of nano wire: take the pattern of modifying preceding selected nano wire fragment with the subsidiary CCD of Electronic Speculum earlier, 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 finished then.
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), and 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), and 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), and described TEM sample is to scrape the silica-based nanowire powder from silicon chip substrate.
5. the method for modifying surface heterogeneous medium of a kind of silica-based nanowire as claimed in claim 4 is characterized in that described silica-based nanowire is Si nano wire or SiO
xNano wire.
6. the method for modifying surface heterogeneous medium of a kind of silica-based nanowire as claimed in claim 5, it is characterized in that described silica-based nanowire is the Si nano wire, described TEM sample is to scrape the silica-based nanowire powder from silicon chip substrate, under ultrasonic vibration, corrode earlier with hydrofluoric acid, remove the oxide layer on surface, under ultrasonic vibration, disperse then with organic solvent, treat that aggregate fully disperses and when forming 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 promptly get the TEM sample.
7. the method for modifying surface heterogeneous medium of a kind of silica-based nanowire as claimed in claim 6 is characterized in that described organic solvent selects absolute ethyl alcohol or acetone for use.
8. the method for modifying surface heterogeneous medium of a kind of silica-based nanowire as claimed in claim 1, it is characterized in that in step 2) in, described TEM low power observing pattern selects 6000 for use * about, described primary election is the needs according to finishing, and selecting pattern is that two ends are fixed and axially straight and be of a size of the nano wire of 10~100nm; Described higher multiple observing pattern selects 20000 *~150000 for use *.
9. 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 3), the multiplication factor of described Electronic Speculum is 20000 *~150000 *.
10. the method for modifying surface heterogeneous medium of a kind of silica-based nanowire as claimed in claim 1, it is characterized in that in step 3), described irradiation adopts following method: 1. under the focused beam fixed point irradiation of beam spot size less than nanowire diameter, come the deposit carbon nano particle by control 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 parameters such as control beam spot size, irradiation position and exposure times, realize that amorphous carbon-film is to the heterogeneous modification of the controlled surface of silica-based nanowire.
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