CN100434353C - Gas phase synthesis process of nanometer particle array with one-dimensional diameter and number density gradient - Google Patents
Gas phase synthesis process of nanometer particle array with one-dimensional diameter and number density gradient Download PDFInfo
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- CN100434353C CN100434353C CNB2006100379687A CN200610037968A CN100434353C CN 100434353 C CN100434353 C CN 100434353C CN B2006100379687 A CNB2006100379687 A CN B2006100379687A CN 200610037968 A CN200610037968 A CN 200610037968A CN 100434353 C CN100434353 C CN 100434353C
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Abstract
The present invention adopts a gas phase aggregation method for clustering a beam current source (1) for generating nanometer particles. A nanometer particle beam current (5) is obtained by adiabatic expansion and enters a sediment chamber (6) with high vacuum through a collimator (4), so a nanometer particle beam current with directional height is formed. A substrate seat is rotated so that a substrate (7) and the nanometer particle beam current (5) form an incidence angle of 10 DEG, and the substrate (7) and a block mask (11) are maintained to be positioned in an exposure shoot area of the nanometer particle beam current (5). After the nanometer particle beam current (5) is controlled to deposit the substrate (7) for 30 seconds, a nanometer particle array with a one-dimensional gradient of diameters and density can be obtained on the surface of the substrate (7). The method has the characteristics of high efficiency, low cost, simple manufacture technology, etc. The present invention can complete the deposition of the nanometer particle gradient array in scores of seconds under common nanometer particle source technological parameters.
Description
One, technical field
The gas phase that the present invention relates to a kind of nano material is synthetic, specifically relates to a kind of gas-phase synthesizing method with nano particles array of diameter and number density one dimension gradient.
Two, background technology
So far synthetic technology, for from the number nanometers still can not better controlled to the nano particle of tens nanometer size range.Though for specific material, the method that obtains the uniform nano particles array of size by specific technical process is unrare, but in the size range of number nanometer order of magnitude of such leap, carry out the careful selection and the controlled arrangement of nano particle, remain a challenge technically to tens nanometer.More existing based on the nanostructured technology of preparing of exposure with etching, for example electron beam exposure or focused-ion-beam lithography etc. can reach this purpose in theory, but cost are high, efficient is very low, and it still is doubt whether can reaching commercial Application.And the self assembly by atom and nano particle, obtain nano particle dot array, be a kind of method of high efficiency, low cost, at present aspect the preparation of the even lattice structure of nano particle near the level of practicability, but can not realize that the spatial selectivity of different size nano particle arranges.About having the preparation of the nano particles array that population density distributes, still be in the laboratory exploratory stage in the world.(the R.B.Bhat such as Rajendra R.Bhat of the upright university of North Carolina, USA, D.A.Fischer, J.Genzer, Langmuir, 18,5643 (2002)) once reported by silane vapor diffusion technology and prepared substrate, again substrate had been immersed in the gold colloid, obtained having the golden nanometer particle array that the one dimension concentration gradient distributes with amino molecule one dimension concentration gradient.(the S.T.Plummer such as Plummer of Illinois, US university, P.W.Bohn, Langmuir, 18,4142 (2002)) self assembled monolayer that then adopts electrochemical method to have CONCENTRATION DISTRIBUTION in the substrate surface preparation distributes in order to produce the number density gradient as the template-directed polystyrene nanoparticle.The population density one dimension gradient that these methods obtain be distributed in the spatial dimension of mm-scale, and at the yardstick of micron to sub-micron, it is uniform that the distribution of nano particle still can be considered.In addition, can not obtain the gradient distribution of diameter of nano particles.Therefore, for having the scale preparation of the nano particles array of size and the distribution of concentration one dimension gradient to submicron-scale, do not form the universal method of high efficiency, low cost at present as yet at micron.
Quantum size effect is the key property of nano particle.The character of nano particle and its size and arrangement mode are closely related.Specific character often only comes across specific size range, perhaps in specific size range particular outer is excited the generation resonance response.For with the device of nano particle as structure and functional unit, the exploitation size of the method, particularly nano particle of growth nano-particle and control method of Pareto diagram under particular chemical environment and structural environment are very important.Acquisition with nano particles array of size gradient distribution then is the size relevant nature of research and applying nano particle, realizes that best performanceization provides the very big free degree.Have the nano particles array that size and population density gradient distribute, also have important use at aspects such as high-density optical storage, micro photo electric device and senser elements and be worth.
Three, summary of the invention
1. goal of the invention
The object of the present invention is to provide a kind of preparation to have the gas-phase synthesizing method of the nano particles array of diameter and number density one dimension gradient.The method can be applicable in preparation technology's flow process of nano-device, has that low cost, technology are simple, high efficiency, is easy to characteristics such as scale.
2. technical scheme
The present invention has provided a kind of vacuum moulding machine of the nanometer particle beam by directed movement, is implemented in the universal method that micron has the metal nano particles array that size and population density one dimension gradient distribute to the submicron-scale.This method can realize the meticulous control to nano-particles size and CONCENTRATION DISTRIBUTION gradient and distribution.And be applicable at macroscopical area (mm
2More than) to obtain concurrently by this gradient distributed architecture be that the nano structural material that constitutes is periodically continuously arranged in the unit.This method is based on vacuum deposition process, with the device preparation technology of current main-stream very big compatibility is arranged.
The operation principle of this method is: make the orientation nanoparticle line of uniform-dimension be deposited on substrate surface to plunder the form of penetrating under vacuum state, by on the line operating path, introducing the mask that stops perpendicular to substrate of micron height, make substrate surface the shadow region of particle beams deposition (expose to the sun and penetrate) occur.Nano particle interparticle fusion growth to a certain degree can occur after depositing to substrate surface, particle size is grown up.Border in the shadow region, nano particle can cause producing on these both sides, border the inhomogeneities of particle density and extent of growth along the slip of incident direction and to the reciprocal diffusion motion of incident, and finally obtain the one dimension gradient distribution of particle size and number density.
A kind of gas-phase synthesizing method with nano particles array of diameter and number density one dimension gradient, its synthesis step is as follows:
(a) mask 11 that stops that will be provided with transmission window vertically is close to the surface of substrate 7, and substrate 7 is fixed on the rotatable block substrate, then block substrate is positioned in the high vacuum settling chamber 6 of sealing;
(b) adopt gas phase aggregation method cluster beam source 1 to produce the vapor phase metal nano particle, in condensation chamber 2, produce the high desnity metal atom by atomizer 8 in argon gas atmosphere, metallic atom is grown in argon gas and is formed metal nanoparticle;
(c) obtain nanometer particle beam by adiabatic expansion, adopt first order difference vacuum system 9 that the nano particle in the condensation chamber 2 is ejected in the vacuum chamber by aerodynamics nozzle 3 with argon gas, form the metal nanoparticle line;
(d) collimating aperture by collimater 4 obtains directed metal nanoparticle line, by second level difference vacuum system 10 the metal nanoparticle line is entered in the vacuum deposition chamber 6 through collimater 4, forms the metal nanoparticle line of high orientation;
(e) block substrate in the rotation high vacuum settling chamber 6 makes the incidence angle of 5 one-tenth 10 ° of substrate 7 and nanometer particle beams, and keeps substrate 7 and stop that mask is positioned at exposing to the sun of nanometer particle beam 5 and penetrates the district;
(f) 5 pairs of substrates of control nanometer particle beam, 7 depositions stopped deposition after 30 seconds; Promptly obtain nano particles array with diameter and number density one dimension gradient on substrate 7 surface.
Stop that mask is is that the stainless steel of 1-10 micron or copper or splitting are made with thickness described in the above-mentioned steps a, this stops that mask is divided into and is used to prepare stopping mask and being used to prepare that the nano particle of alternately repeated size and density gradient distribution displays stops two kinds of masks of nano particle display that single size and density gradient distribute.
Substrate described in the above-mentioned steps a is monocrystalline silicon piece or quartz glass or graphite monocrystalline or an agraphitic carbon film production of selecting atomically flating for use.
Gas phase aggregation method cluster beam source described in the above-mentioned steps b is magnetic controlled plasma gas phase aggregate source or high temperature evaporation type gas phase aggregate source, described atomizer is magnetron sputtering or high temperature evaporation, condensation chamber 2 is used cooled with liquid nitrogen, ar pressure is 100-200Pa, the nano particle that grows into, its diameter are the 3-30 nanometer.
First order difference vacuum system 9 can obtain to drop to from 100Pa the difference vacuum of 0.1Pa among the above-mentioned steps c, and 2 millimeters of the diameters of aerodynamics nozzle 3, the air pressure of nozzle exit end vacuum chamber are 0.1Pa.
Second level difference vacuum system 10 described in the above-mentioned steps d can obtain to drop to 10 from 0.1Pa
-4The difference vacuum of Pa, the collimating aperture diameter 2mm on the collimater 4, the vacuum of high vacuum settling chamber 6 is 10
-4Pa;
The nano particles array that obtains among the above-mentioned steps f, wherein diameter of nano particles varies continuously to 30nm along the incident direction of nano particle by 3nm, and population density has the variation of twice, and this gradient distributes and has crossed over long 1～3 micron zone.
3. beneficial effect
The present invention has used metal nanoparticle can merge between little nano particle before substrate surface has the higher migration rate and the diameter that reaching capacity and the characteristic of growing up.Deposit by the angle of plunderring of orientation nanoparticle line under high vacuum environment of original dimension less than saturated diameter, and introduce the suitable mask that stops, can obtain to distribute along the continually varying gradient that one dimension direction diameter of nano particles is crossed over an order of magnitude by the number nanometer to tens nanometer, the gradient that can also have population density simultaneously distributes.This gradient may reside in hundreds of nanometers in several microns interval, and siding-to-siding block length can be controlled by the incident angle that changes the nano particle bundle.This method is currently uniquely a kind ofly can realize the universal method that nano-particles size and population density gradient distribute to the submicron-scale at micron by vapour deposition.This Promethean scheme has efficiently, low-cost, technology characteristic of simple.Under the technological parameter of the nanoparticle sources of routine, just can finish the deposition of nano particle gradient array common tens of seconds.And manufacturing process can be monitored in real time by various rigorous analysis technology, has good compatibility with the modern device manufacture craft technically.
Four description of drawings
Fig. 1: the generation and the precipitation equipment that are used to realize the nanometer particle beam of this method.1. gas phase aggregation method cluster beam source; 2. the condensation chamber of growth nano-particle; 3. aerodynamics nozzle; 4. collimater; 5. nanometer particle beam; 6. high vacuum settling chamber; 7. substrate; 8. atomizer (magnetron sputtering, high temperature evaporation etc.); 9. first order difference vacuum system; 10. second level difference vacuum system.
Fig. 2 (a): the basic structure that stops mask that is used to obtain single size and density gradient distribution.Among the figure, the shadow region is a barrier structure, and the clear area is the transmission window of nano particle, and D is the width of transmission window.
Fig. 2 (b): the structure that stops mask that is used to obtain alternately repeated size and density gradient distribution.Among the figure, the shadow region is a barrier structure, and the clear area is the transmission window of nano particle, and D is the width of transmission window, and G is the repetition period of transmission window.
Fig. 3: stop that mask is positioned over the allocation plan of substrate surface.(11) for stopping mask, (7) are substrate.Stop that mask (11) is close to substrate (7) surface and vertically places.
Fig. 4: nanometer particle beam sees through and stops the schematic diagram that mask (11) deposits substrate (7).α is the incidence angle of nanometer particle beam.Owing to stop the effect of mask, near the substrate surface of mask, be the shadow region of nano particle deposition on the mask right side, the right-hand member in the shadow region, the gradient that nano-particles size and number density occur distributes.
Fig. 5 (a) has the schematic diagram of the nano particles array of single size and the distribution of number density gradient.
Fig. 5 (b) has the schematic diagram of the nano particles array of alternately repeated size and the distribution of number density gradient.
Five, the specific embodiment
Below with the be deposited as example of metallic tin nano particle at the agraphitic carbon substrate surface, the basic procedure of this method is described:
(1) adopt the splitting be about 1 micron thickness to stop mask (11) by the structure fabrication of Fig. 2 (a), the wide 20mm of mask, high 20mm, the transmission window width is 3 microns, apart from the mask bottom 3 microns, mask (11) is close to amorphous carbon film substrate (7) surface by the configuration of Fig. 3 vertically places, and be fixed on the rotatable block substrate, then block substrate is sealed on the appropriate location of high vacuum settling chamber (6);
(2) adopt magnetic controlled plasma gas phase aggregate source to produce the sijna rice corpuscles, in the condensation chamber (2) of cooled with liquid nitrogen, produce the high density tin atom by magnetron sputtering (8) under the ar pressure of 200Pa, tin atom is grown to serve as nano particle in argon gas, and its diameter is 3 nanometers;
(3) obtain nanometer particle beam by adiabatic expansion, adopt first order difference vacuum system (9), sijna rice corpuscles in the condensation chamber (2) is ejected in the vacuum chamber that air pressure is 0.1Pa with the aerodynamics nozzle (3) of argon gas by 2 mm dias, forms sijna rice corpuscles line;
(4) obtain the orientation nanoparticle line by collimater (4), by second level difference vacuum system (10), it is 10 that the collimater (4) that makes sijna rice corpuscles line pass through the 2mm diameter enters vacuum
-4In the high vacuum settling chamber (6) of Pa, form the nanometer particle beam (5) of high orientation, the angle of divergence of line is 3 °;
(5) block substrate in the rotation high vacuum settling chamber (6) makes substrate (7) surface become 10 ° incidence angle with nanometer particle beam, and keeps the lining body and stop that mask is positioned at exposing to the sun of nanometer particle beam and penetrates the district;
(6) control nanometer particle beam (5) after 30 seconds, stops deposition to lining body deposition; Obtain to be similar to the sijna rice corpuscles array shown in Fig. 5 (a) at substrate surface; Wherein, the diameter of nano particle varies continuously to 18nm along the incident direction of nano particle by 3nm, and population density has the variation of twice approximately, and this gradient distributes and crossed over long 3 microns zone;
(1) adopt the stainless steel thin slice be about 2 micron thickness to stop mask (11) by the structure fabrication of Fig. 2 (b), the wide 20mm of mask, high 20mm, each transmission window width is 3 microns, 3 microns of the transmission windows of lower side apart from the mask bottom, the repetition period of transmission window is 5 microns, and substrate (7) surface that mask (11) is close to monocrystalline silicon piece by the configuration of Fig. 3 is vertically placed, and be fixed on the rotatable block substrate, then block substrate is sealed on the appropriate location of high vacuum settling chamber (6);
Step (2), (3), (4), (5) are with embodiment 1;
(6) control nanometer particle beam (5) after 30 seconds, stops deposition to lining body deposition; Obtain to be similar to the sijna rice corpuscles array shown in Fig. 5 (b) at substrate surface; The gradient distributed areas that alternately occur diameter of nano particles and number density at substrate surface; In each dull gradient distributed area, the diameter of nano particle varies continuously to 18nm along the incident direction of nano particle by 3nm, and population density has the variation of twice approximately, and the zone that this gradient distributes alternately occurred at substrate surface by 3 microns cycle.
Claims (7)
1. gas-phase synthesizing method with nano particles array of diameter and number density one dimension gradient, its synthesis step is as follows:
(a) mask (11) that stops that will be provided with transmission window vertically is close to the surface of substrate (7), and substrate (7) is fixed on the rotatable block substrate, then block substrate is positioned in the high vacuum settling chamber (6) of sealing;
(b) adopt gas phase aggregation method cluster beam source (1) to produce the vapor phase metal nano particle, in condensation chamber (2), produce the high desnity metal atom by atomizer (8) in argon gas atmosphere, metallic atom is grown in argon gas and is formed metal nanoparticle;
(c) obtain nanometer particle beam by adiabatic expansion, adopt first order difference vacuum system (9) that the nano particle in the condensation chamber (2) is ejected in the vacuum chamber by aerodynamics nozzle (3) with argon gas, form the metal nanoparticle line;
(d) collimating aperture by collimater (4) obtains directed metal nanoparticle line, by second level difference vacuum system (10) the metal nanoparticle line is entered in the vacuum deposition chamber (6) through collimater (4), form the metal nanoparticle line of high orientation;
(e) block substrate in the rotation high vacuum settling chamber (6) makes substrate (7) become 10 ° incidence angle with nanometer particle beam (5), and keeps substrate (7) and stop that mask (11) is positioned at exposing to the sun of nanometer particle beam (5) and penetrates the district;
(f) control nanometer particle beam (5) after 30 seconds, stops deposition to substrate (7) deposition, can obtain the nano particles array with diameter and number density one dimension gradient on substrate (7) surface.
2. gas-phase synthesizing method according to claim 1, it is characterized in that stopping that mask (11) is is that the stainless steel of 1-10 micron or copper or splitting are made with thickness described in the step a that this stops that mask is divided into and is used to prepare stopping mask and being used to prepare that the nano particle of alternately repeated size and density gradient distribution displays stops two kinds of masks of nano particle display that single size and density gradient distribute.
3. gas-phase synthesizing method according to claim 1 is characterized in that at the substrate (7) described in the step a be monocrystalline silicon piece or quartz glass or graphite monocrystalline or the agraphitic carbon film production of selecting atomically flating for use.
4. gas-phase synthesizing method according to claim 1, it is characterized in that being magnetic controlled plasma gas phase aggregate source or high temperature evaporation type gas phase aggregate source at the gas phase aggregation method cluster beam source (1) described in the step b, described atomizer (8) is magnetron sputtering or high temperature evaporation, condensation chamber (2) is used cooled with liquid nitrogen, ar pressure is 100-200Pa, the nano particle that grows into, its diameter are the 3-30 nanometer.
5. gas-phase synthesizing method according to claim 1, it is characterized in that in step c first order difference vacuum system (9) can obtain to drop to from 100Pa the difference vacuum of 0.1Pa, 2 millimeters of the diameters of aerodynamics nozzle (3), the air pressure of nozzle exit end vacuum chamber are 0.1Pa.
6. gas-phase synthesizing method according to claim 1 is characterized in that obtaining to drop to 10 from 0.1Pa in the second level difference vacuum system (10) described in the steps d
-4The difference vacuum of Pa, the collimating aperture diameter 2mm on the collimater (4), the vacuum of high vacuum settling chamber (6) is 10-4pa.
7. gas-phase synthesizing method according to claim 1, it is characterized in that the nano particles array that in step f, obtains, wherein diameter of nano particles varies continuously to 30nm along the incident direction of nano particle by 3nm, population density has the variation of twice, and this gradient distributes and crossed over long 1～3 micron zone.
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| GB2482897A (en) * | 2010-08-18 | 2012-02-22 | Mantis Deposition Ltd | An apparatus and method for the production of nanoparticles |
| CN102925863A (en) * | 2012-11-06 | 2013-02-13 | 苏州新锐博纳米科技有限公司 | Gas phase method for generating metastable phase nanometer particle beam and depositing nanometer film |
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