CN104889410A - A manufacture method for controllable metal nanoparticles - Google Patents
A manufacture method for controllable metal nanoparticles Download PDFInfo
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- CN104889410A CN104889410A CN201510136274.8A CN201510136274A CN104889410A CN 104889410 A CN104889410 A CN 104889410A CN 201510136274 A CN201510136274 A CN 201510136274A CN 104889410 A CN104889410 A CN 104889410A
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Abstract
The invention provides a manufacture method for controllable metal nanoparticles. The method comprises the steps of first providing a substrate comprising a base body and a top insulating layer; depositing a metal nano-film on the top of the top insulating layer; obtaining a micron metal pattern by using a photoetching method and an etching method; and finally using the method of focused ion beam irradiation to obtain dimension-controllable metal nanoparticles during metal etching. The method is simple in process and high in efficiency; the positions and the dimensions of the metal nanoparticles are controllable; the metal nanoparticles are compatible with a CMOS technology, so that the metal nanoparticles have better extensibility; the metal nanoparticles have a wider using prospect in the field of catalysts, micro-electronics and biochemical detection.
Description
Technical field
The present invention relates to a kind of preparation method of controllable metal nano particle.Belong to nano material preparation and application technical field.
Background technology
Because the size of metal nanoparticle is little, specific area is large, makes it obtain in fields such as optics, chemical catalysis, biochemistry detection and uses widely.Wherein, because of metal has good electrology characteristic and excellent heat transfer performance, makes metal in the concern be subject to especially of microelectronic.Infusive is that Nanometer Copper can the growth of catalysis silicon nanowires at 400 DEG C, easily with CMOS technology compatibility.(Vincent T.Renard, Michael Jublot waits " Catalyst preparation for CMOS-compatible silicon nanowire synthesis " Naturte nanotechnology, 4 (2009), 654-657.In literary composition, the thick copper of 20nm is oxidized under the condition of hypoxemia, obtain cuprous oxide, cuprous oxide and silane reaction produce Cu-Si compound, this compound can under lower temperature conditions with silane reaction grow silicon nanowires) this novel silicon nanometer preparation method compatible with CMOS technology, bring very valuable inspiration to the making of micro-nano sensor, have great importance.
At present, the Traditional Method manufacturing various metal nanoparticle has that mechanical milling method, spray-on process, sol-gel are sent out, electro-deposition and micro emulsion method.These conventional methods exist that nanoparticle size is wayward, cost is high or the defect such as manufacturing process is complicated.Along with the development of technology, some new production methods propose gradually, improve the controllability of making nano particle, reduce cost of manufacture.As Samsung Electro-Mechanics Co., Ltd mixed copper forerunner (nitric acid metal, acetic acid metal, ethylenediamine metal etc.) and amines, react under heating condition, obtain nano copper particle (Chinese patent 200710145582.2) through alcoholic solvent precipitation.What propose as Zhang Tong etc. prepares the method for gold nano grain (see Chinese Patent Application No.: 201210270560.X by golden film annealing, application publication number CN 102806354 A), sputtering or evaporation one deck gold thin film, then anneal 30 ~ 120 minutes at 350 ~ 600 DEG C, prepare gold nano grain.The feature of nano particle prepared by this method is, pattern is relatively better, nanosphere size distribution is more even.But the graphical of gold nano grain can not be realized.After Korean Patent (patent No. 10-2005-35606) proposes to use cvd precursor designing technique to design copper precursors, copper nano particles is prepared with pyrolysis technique, the method can produce copper nano particles under lower than the condition of 200 DEG C, and than adopting, the physical method of annealed metal nano thin-film is superior.But the method needs to design precursor, and cost is high.The people such as the Zhou Youfu of Fujian Inst. of Matter Structure, Chinese Academy of Sciences are mineralizer with sodium halide, take glucose as reducing agent, and monovalent metallic ion under hydrothermal conditions reduction reaction generates copper nano particles.(see Chinese Patent Application No.: 201110257946.2 publication numbers: CN 102962468 A).For another example the woods of East China Normal University and spring and Chu Junhao, adopt the synthetic method of semi-solid phase, divalent metal salt, reducing agent, stabilizing agent and water are mixed to get uniform mixture, adopt the method for microwave thermal, Fast back-projection algorithm obtains copper nano particles (see Chinese Patent Application No.: 201110355856. publication numbers: CN 102407343 A).
Manufacture field at nano-probe, the appearance of nano wire probe solves the difficult problem that traditional handicraft is difficult to prepare the high nano-probe of sharpness.But also encounter new difficulty, i.e. the catalyst position of aided nano line growth and size need to control.The GM section of the people from International Business Machine Corporation (IBM) such as to hold high, and to propose a kind of monolithic high aspect ratio nano-size scanning probe microscope by nanowire growth (SPM) most advanced and sophisticated.The method manufacturing process is loaded down with trivial details, and the number of nanowires simultaneously grown is more, needs specially treated could finally realize nano wire probe.Therefore, realize the controlled metal nanoparticle of position, size to be prepared in nano wire probe and to manufacture field and have great importance.
The metal nanoparticle adopting the method for chemical reaction or physical method to obtain exists with the form of liquid suspension or powder, limits metal nanoparticle as the use of catalyst in fixed point, controllable nano Material growth field.Adopt the method for annealing also can not realize simultaneously.Therefore, realize metal nanoparticle as the application of catalyst in fixed point controllable nano Material growth field, need the manufacture difficult problem that size is controlled, position is controlled solving metal nanoparticle.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of controllable metal nano particle compatible mutually with CMOS technology, for solving the problem that prior art cannot realize at the controlled metal nanoparticle of ad-hoc location manufactured size.
For achieving the above object and other relevant objects, the invention provides a kind of preparation method of controllable metal nano particle, described preparation method at least comprises step:
1) provide one to comprise matrix and push up the substrate of insulating barrier;
2) at top insulating barrier disposed thereon metal nanometer thin film;
3) method of photoetching and etching is adopted to obtain micron metal figure;
4) adopt the method for FIB irradiation, while etching metal, obtain position and all controlled metal nanoparticle of size.
Alternatively, described step 1) in matrix material be silicon, germanium or germanium silicon, the material of top insulating barrier is silica, silicon nitride, aluminium oxide or hafnium oxide.
Alternatively, the thickness range of described top insulating barrier is 50 ~ 800nm.
Alternatively, described step 2) the middle method of magnetron sputtering or evaporation that adopts is at top insulating barrier disposed thereon one deck or multiple layer metal nano thin-film, and the thickness range of metal nanometer thin film is 10 ~ 600nm.Metallic film material can be copper, aluminium, gold, platinum, chromium, titanium, nickel or the composite nanometer film be made up of these metals, and the metal nanometer thin film of compound.The metal nanometer thin film number of plies is not limit, as long as gross thickness is in 10 ~ 600nm scope.
Alternatively, described step 2) in adopt the method for photoetching and etching to make metal micro dimension of picture scope be (0.1 ~ 200 μm) * (0.1 ~ 200 μm).Can be isometrical size, also can be do not wait through size, in described scope.
Alternatively, described step 3) operating voltage that adopts ion beam irradiation is 30keV, gas current scope is 1.1pA ~ 7nA, and exposure time is 10s ~ 200s.
Alternatively, described step 3) in the metal nanoparticle size range that obtains of ion beam irradiation be: 10nm ~ 200nm.
As mentioned above, the preparation method of controllable metal nano particle of the present invention, comprises step: first provide one to comprise matrix and push up the substrate of insulating barrier; Then at top insulating barrier disposed thereon metal nanometer thin film; Then the method for photoetching and etching is adopted to obtain micron metal figure; Finally adopt the method for FIB irradiation, while etching metal, obtain the controlled metal nanoparticle of size.
The present invention has following beneficial effect:
1, the position of metal nanoparticle is precisely controlled.Adopt FIB irradiation micron metal figure in the present invention, obtain metal nanoparticle.FIB irradiation position is by controlling micron metal figure, and the focal position of FIB just realizes accurate control.Micron metal figure provides coarse alignment, and the focal position of FIB then can realize the accurate aligning at Nano grade, and therefore, in the present invention, the position of metal nanoparticle can be precisely controlled.In addition, FIB irradiation range is that enlargement ratio when can be worked by FIB is regulated.
2, the size of metal nanoparticle is precisely controlled.By regulating micron metal thickness, focused ion size of current, FIB bundle spot size, accepting the time of FIB irradiation in the present invention, and substrate temperature five parameters control the size of metal nanoparticle.Therefore, the size of metal nanoparticle can be precisely controlled.
3, the present invention and CMOS technology compatibility, manufacturing cycle is short, efficiency is high.Adopt CMOS technology to produce micron metal figure, adopt FIB irradiation micron metal figure, whole process time is short, and efficiency is high simultaneously.
Accompanying drawing explanation
Fig. 1 is shown as the process chart of the preparation method of controllable metal nano particle of the present invention.
Fig. 2 is shown as the step 1 of the preparation method of controllable metal nano particle of the present invention) before the structural representation of matrix.
Fig. 3 is shown as the preparation method step 1 of controllable metal nano particle of the present invention) in the structural representation that presents.
The preparation method step 2 of Fig. 4 ~ be shown as controllable metal nano particle of the present invention) in the structural representation that presents
Fig. 5 is shown as the preparation method step 3 of controllable metal nano particle of the present invention) in the structural representation that presents.
Fig. 6 is shown as the preparation method step 4 of controllable metal nano particle of the present invention) in the structural representation that presents.
Fig. 7 is shown as the controllable metal nano particle electron microscope picture that the embodiment of the present invention is produced.
Element numbers explanation
S1 ~ S4 step
1 substrate
10 matrixes
11 top insulating barriers
2 metal nanometer thin films
21 micron metal figures
22 metal nanoparticles
Detailed description of the invention
Below by way of specific instantiation, embodiments of the present invention are described, those skilled in the art the content disclosed by this description can understand other advantages of the present invention and effect easily.The present invention can also be implemented or be applied by detailed description of the invention different in addition, and the every details in this description also can based on different viewpoints and application, carries out various modification or change not deviating under spirit of the present invention.
Refer to accompanying drawing 1 to Fig. 7.It should be noted that, the diagram provided in the present embodiment only illustrates basic conception of the present invention in a schematic way, then only the assembly relevant with the present invention is shown in graphic but not component count, shape and size when implementing according to reality is drawn, it is actual when implementing, and the kenel of each assembly, quantity and ratio can be a kind of change arbitrarily, and its assembly layout kenel also may be more complicated.
As shown in Figure 1, the preparation method of a kind of controllable metal nano particle provided by the invention, at least comprises the following steps:
S1, provides one to comprise matrix and pushes up the substrate of insulating barrier;
S2, at top insulating barrier disposed thereon metal nanometer thin film;
S3, makes micron metal figure by the method for photoetching, etching;
S4, is utilizing FIB irradiation metal micro figure, obtains position and the controlled nano-metal particle of size;
Be described in detail below in conjunction with the preparation method of concrete accompanying drawing to controllable metal nano particle of the present invention.
First perform step S1, provide one to comprise matrix 10 and push up the substrate 1 of insulating barrier 11.
Refer to accompanying drawing 2 ~ Fig. 3, described matrix 1 comprises the top insulating barrier 11 be positioned on described matrix 1 and matrix 10.That is, described substrate 1 entirety is made up of matrix 10 and the top insulating barrier 11 be positioned on described matrix 10.
Described matrix 10 can be silicon, germanium or germanium silicon, does not limit at this.In the present embodiment, described matrix 10 is monocrystalline silicon.The material of top insulating barrier is silica, silicon nitride, aluminium oxide or hafnium oxide.Exemplarily, described top insulating barrier 11 is silica.The thickness of described top insulating barrier 11 can within the scope of 50 ~ 800nm, in the present embodiment, the thickness of described top insulating barrier 11 elects 300nm as temporarily, certainly, in other embodiments, the thickness of described top insulating barrier 11 and end insulating barrier 12 can also be 50nm, 200nm, 500nm or 800nm etc.
It should be noted that, described substrate 1 to have completed SiO at upper surface
2the matrix 10 of insulating barrier, directly provides and just can be utilized by the present invention.
Then step S2 is performed, at described top insulating barrier 11 disposed thereon metal nanometer thin film 2.
Adopt the method for magnetron sputtering or evaporation at top insulating barrier disposed thereon one deck or multiple layer metal nano thin-film, the thickness range of metal nanometer thin film is 10 ~ 600nm.Certainly, other suitable techniques also can be adopted to form metal nanometer thin film 2 on described top insulating barrier 11 surface, do not limit at this.Metallic film material can be copper, aluminium, gold, platinum, chromium, titanium, nickel or the composite nanometer film be made up of these metals, and the metal nanometer thin film of compound.In the present embodiment, magnetron sputtering deposition thickness is adopted to be the copper of 200nm, as shown in Figure 4.Certainly, in other embodiments, the composite nanometer film that the material of metal nanometer thin film 2 can be chosen as aluminium, gold, platinum, chromium, titanium, nickel or be made up of these metals, and the metal of compound, thickness can also be made as any one of 10nm, 100nm, 300nm, 400nm, 500nm or 600nm kind.
Then perform step S3, make micron metal figure 21.
Obtained the micron metal figure 21 of regular shape by graphical treatment and etching technics after described top insulating barrier 11 disposed thereon metal nanometer thin film 2.In the present embodiment, adopt photoetching and plasma etching (Ion beam etching, RIE) technique, detailed process is: on described metal nanometer thin film 2, apply photoresist, opening is formed afterwards by photoetching or the graphical described photoresist of beamwriter lithography, metal nanometer thin film 2 below opening described in recycling plasma etching forms micron metal figure 21, as shown in Figure 5.
The size range of the micron metal figure 21 formed is (0.1 ~ 200 μm) × (0.1 ~ 200 μm).In the present embodiment, described micron metal figure 21 is of a size of 5 μm × 5 μm.
It should be noted that, in other embodiments, also can pass through stripping technology realization formation micron metal figure 21 structure that photoetching, sputtering or evaporation process form.Particularly, after the insulating barrier 11 surface application photoresist of described top, obtain without photoresist array pattern by uv-exposure, development, cleaning and drying; Metal nanometer thin film 2 is made at photoresist with without photoresist region again by sputtering or evaporation process, finally whole substrate is placed in acetone soln to soak, photoresist is separated with substrate with the nanometer metallic film 2 on photoresist surface, and the nanometer metallic film 2 leaving part forms micron metal figure 21.
Perform step S4 afterwards, refer to accompanying drawing 6, carry out FIB irradiation, described micron metal figure 21 is etched away in FIB irradiation process, obtains described metal nanoparticle 22 in described micron metal figure 21 position simultaneously.
Particularly, the structure that step S3 obtains is placed in Focused Ion Beam (FIB) cavity, then vacuumizes.When the pressure in cavity is less than 10
-5when pa, first by micron copper image hotpoint coarse alignment, find target zone region.Open ion beam, and carry out focusing on and selecting suitable enlargement ratio under ion beam, obtain required irradiation range.Finally carry out FIB irradiation.Preferably, the operating voltage of ion beam irradiation is 30keV, and gas current scope is 1.1pA ~ 7nA, and exposure time is 10s ~ 200s.The metal nanoparticle size range obtained is in 10nm ~ 200nm.
In the present embodiment, in micron metal figure 21 process described in FIB irradiation, the operating voltage of ion beam irradiation is 30keV, and gas current scope is 4.3nA, and exposure time is 60s.And in irradiation process, described micron metal figure 21 is etched, obtain described metal nanoparticle 22 in described micron metal figure 21 position simultaneously.Be illustrated in figure 7 described metal nanoparticle 22 size that obtains in this example within the scope of 10nm ~ 30nm.
In the present invention, except the position of metal nanoparticle can be controlled, the present invention can by micron metal thickness, focused ion size of current, FIB bundle spot size, accept time of FIB irradiation, and substrate temperature five parameters control the size of metal nanoparticle.
In sum, the preparation method of a kind of controllable metal nano particle provided by the invention, solves the position that cannot realize metal nanoparticle in conventional method and the controlled manufacture difficult problem of size.Achieve metal nanoparticle controlled manufacture at an arbitrary position.The present invention simultaneously adopts FIB irradiation micron metal figure, and whole process time is short, and efficiency is high.In addition, the complete compatibility of the present invention and CMOS technology makes it have good autgmentability and the wider scope of application.So the present invention effectively overcomes various shortcoming of the prior art and tool high industrial utilization.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.
Claims (10)
1. a preparation method for controllable metal nano particle, is characterized in that, described preparation method at least comprises:
1) provide one to comprise matrix and push up the substrate of insulating barrier;
2) at top insulating barrier disposed thereon metal nanometer thin film;
3) method of photoetching and etching is adopted to obtain micron metal figure;
4) adopt the method for FIB irradiation, while etching metal, obtain position and all controlled metal nanoparticle of size.
2. method according to claim 1, is characterized in that described step 1) in matrix material be silicon, germanium or germanium silicon, top insulating barrier material be silica, silicon nitride, aluminium oxide or hafnium oxide.
3. method according to claim 1, is characterized in that in described step 2) in:
1. adopt the method for magnetron sputtering or evaporation at top insulating barrier disposed thereon one deck or multiple layer metal nano thin-film, the thickness range of metal nanometer thin film is 10 ~ 600nm;
2. metal nanometer thin film material be copper, aluminium, gold, platinum, chromium, titanium, nickel or the composite nanometer film that is made up of these metals, and the metal nanometer thin film of compound;
3. the thickness range of described top insulating barrier is 50 ~ 800nm.
4. method according to claim 3, is characterized in that the metal nanometer thin film number of plies is not limit, and just thickness is in 10 ~ 600nm scope.
5. the method according to claim 3 or 4, it is characterized in that described metal nanometer thin film material is Cu, thickness is 200nm.
6. method according to claim 1, it is characterized in that described step 3) in adopt the method for photoetching and etching to make metal micro dimension of picture scope be (0.1 ~ 200 μm) × (0.1 ~ 200 μm), described metal micro metallic pattern size differs and is decided to be isometrical size.
7. method according to claim 1, is characterized in that described step 4) operating voltage that adopts FIB irradiation is 30keV, gas current scope is 1.1pA ~ 7nA, and exposure time is 10s ~ 200s.
8. the method according to claim 6 or 7, is characterized in that step 3) the micron metal figure that obtains provides coarse alignment, step 4) realize the accurate aligning of Nano grade.
9. method according to claim 1, is characterized in that described step 4) in the metal nanoparticle size range that obtains of ion beam irradiation be 10nm ~ 200nm.
10. method according to claim 6, is characterized in that:
A) photoetching described in comprises beamwriter lithography;
B) etching described in comprises plasma etching industrial;
C) the micron metal dimension of picture described in is 5 μm × 5 μm.
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| CN201510136274.8A CN104889410B (en) | 2015-03-26 | A kind of preparation method of controllable metal nano particle |
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| CN201510136274.8A CN104889410B (en) | 2015-03-26 | A kind of preparation method of controllable metal nano particle |
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| CN104889410B CN104889410B (en) | 2018-02-09 |
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| CN107140600A (en) * | 2017-05-16 | 2017-09-08 | 广东工业大学 | A kind of controllable manufacture method of metal aperture |
| CN109807345A (en) * | 2019-01-31 | 2019-05-28 | 江南大学 | A kind of preparation and application of photothermal conversion dot-matrix array chip |
| CN109825562A (en) * | 2019-01-18 | 2019-05-31 | 广东工业大学 | A kind of nano-pore manufacturing method being plastically deformed based on ion beam bombardment nano thin-film |
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