CN102230179B - Method for preparing metal nano stripes - Google Patents
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- CN102230179B CN102230179B CN 201110168949 CN201110168949A CN102230179B CN 102230179 B CN102230179 B CN 102230179B CN 201110168949 CN201110168949 CN 201110168949 CN 201110168949 A CN201110168949 A CN 201110168949A CN 102230179 B CN102230179 B CN 102230179B
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Abstract
The invention discloses a method for preparing metal nano stripes. The method comprises the following steps that a target material is disposed in a way that a target surface of the target material and a surface of a horizontal substrate form an angle theta; the surface of the horizontal substrate is bombarded vertically by ion beams from an ion beam gun in at least one inert gas as working gas; the target material is bombarded by ion beams from ion beam gun in a way that the ion beams and the normal of the target surface of the target material form an angle theta; the substrate is bombarded by ion beams reflected by the target surface in a way that the reflected ion beams and the normal of the substrate form an angle of 180 degree to 2-theta and simultaneously, the substrate moves horizontally; and when the previous step is finished, metal nano stripes are obtained, wherein the target material has a rectangular structure and surfaces of the target material are smooth. The method for preparing self-assembled metal micro-nano stripes has the advantages of low cost, good controllability and feasibility of industrialization, and can be utilized for the fields of productions of metal grating polarizers, nonlinear optical devices, plasma photonic chips, LED luminous efficiency reinforced metal gratings and micro-nano magnetic structures.
Description
Technical field
The invention belongs to field of new, relate to a kind of method for preparing metal nano stripes.
Background technology
Ion beam bombardment inductive substance surface self-organization nanostructure has caused the very big interest of science and industry member in recent years.From 1999, the people such as Facsko were since " Science " report adopts ion beam bombardment GaSb crystal to obtain the self-assembled nanometer dot matrix.People adopt ion beam bombardment self-assembly on Si, Ge semi-conductor, glass, metal blocks material to go out orderly nano-dot matrix or nanometer striped in succession.In patent of invention CN 101748374A, the method that adopts the ion beam sputtering technology growing high density and fine self-assembled Ge quantum dot is disclosed.Report all is to adopt ion beam bombardment to prepare nanostructure at homogeneity monocrystalline, polycrystalline or amorphous block at present.In heterogeneous substrate, adopt ionic fluid directly to bombard preparation elemental metals nanometer striated structure and but have no report, reason is that the elemental metals film can not form non-crystal structure in heterogeneous substrate, because the diffusion anisotropic of surface atom causes being difficult to form expected structure.Sputter procedure needs accurately control in addition, in order to avoid metal level is by sputter or sputter amount cause metal Nano structure to fail to be separated from each other not fully.Therefore prepare the nano metal striped, often adopt comparatively complicated technical process, such as photoetching technique, electron beam lithography etc.
On the other hand, low energy ion beamwidth bombardment inductive substance surface nano-structure is the self-assembling technique of a kind of low cost, high production, has stronger competitive edge.Nano metal striped on the foreign substrate is with a wide range of applications at aspects such as metal grating, surface plasma conduction, the luminous enhancing of LED, the preparations of magnetic Nano structure.
Therefore, if can directly adopt ion beam bombardment to grow metal nano stripes in heterogeneous substrate, can overcome current technical bottleneck, this technology will be applied to wider field.Correlation technique has no bibliographical information.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing metal nano stripes.
The method for preparing metal nano stripes provided by the invention, after comprising the steps: the target surface of target is the θ angle to be parallel to substrate surface angle placed, take rare gas element as working gas, vertically bombard substrate surface with ion beam gun, the ionic fluid that described ion beam gun is sent bombards described target to be the θ angle with described target material surface normal, ionic fluid via the target surface reflection bombards described substrate to be 180 ° of-2 θ angles with described substrate normal direction, simultaneously described substrate is moved horizontally, bombard the complete described metal nano stripes that obtains; Wherein, the structure of described target is the rectangular configuration of surfacing.
In the aforesaid method, the material that consists of described target is selected from least a among Al, Ag, Au, Cr, Cu, Co, Fe, Mo, Mn, Nb, Nd, Ni, Pt, Ti, W, Zn and the Zr, preferred Ti, Cr, Fe, Co, Ni, Cu or Zn; The material that consists of described substrate is selected from silicon single crystal, glass, silica glass, sapphire, AlN, ZnO, SiC, LiNbO
3, LiTaO
3At least a with in the amorphous metal material, wherein, the preferred CoZrNb amorphous of described amorphous metal material; The resistance of described substrate has no special requirements, if insulating substrate, for avoiding ion beam bombardment process charge accumulated, can apply in the thermoelectron and electric current according to ordinary method, wherein, in used and the intensity of electric current be 1.2～2 times of ion beam current intensity, the surfaceness of this substrate is 0.1nm～10nm, preferred 0.1nm～1.0nm.The angle that is the θ angle for the target surface of realizing target to be parallel to substrate surface is placed, the back side of this metal targets can be fixed on the adjustable rotating mechanism of angle, make target surface and the angle on sample driving water plane that is placed with substrate at 45 °～90 °, preferred 50 °～85 °, adjustable between more preferably 55 °～80 °, and this rotating mechanism links to each other with baffle plate.
In the described implant steps, intensifying ring voltage is 100V～500V, preferred 120V～200V, more preferably 120V～150V; Plate voltage is 0.5kV～10.0kV, preferred 0.6kV～6.0kV, more preferably 0.6kV～3.0kV; Ion beam current density is 1.0 * 10
14Cm
-2S
-1～1.0 * 10
16Cm
-2S
-1, preferred 0.5-5.0 * 10
15Cm
-2S
-1, more preferably 1.0 * 10
15Cm
-2S
-1This implant steps is carried out under vacuum condition; Described rare gas element is selected from least a among Ar, Kr and the Xe; In the described vacuum condition, base vacuum is not less than 5 * 10
-4Pa, preferred 2 * 10
-4Pa; Operating air pressure is 1 * 10
-2Pa～1 * 10
-1Pa, preferred 2 * 10
-2Pa.Described substrate temperature is 0 ℃～800 ℃, preferred 20 ℃～700 ℃, and more preferably 25-700 ℃; The speed that moves horizontally of described substrate is not less than 0.01cm/min, preferred 0.02cm/min～0.20cm/min, and more preferably 0.02cm/min～0.05cm/min, the speed that moves horizontally of this substrate can be adjustable continuously in above-mentioned scope.Vertical range between the lower-most point of described target and the described substrate horizontal surface is 0mm～20mm, preferred 1mm～10mm, more preferably 1mm.
Preferably, in the method, used ion beam gun is Kaufman molded breadth beam ion rifle, and is corresponding, and used bombardment system is Kaufman molded breadth beam ion source bombardment system, comprises the thermoelectron neutrodyne circuit in this ion source bombardment system.
In addition, in actually operating, before described implant steps, can first substrate be distinguished ultrasonic cleaning certain hour (as can be 15min) to remove organism and inorganic impurity with acetone, dehydrated alcohol, deionized water in advance.
The metal nano stripes for preparing according to the method described above also belongs to protection scope of the present invention.Be 100nm～1000nm the eigenperiod of this metal nano stripes, preferred 100nm～800nm, more preferably 150-800nm; Live width is 10nm～100nm, preferred 20nm～80nm, more preferably 30-80nm.
The invention provides a kind of preparation method who utilizes the micro-nano metal stripe of ion beam bombardment self-assembly, compare with existing photoetching method or electron beam lithography method, possess following advantage: the method has widely substrate material adaptability, contains semi-conductor, isolator, amorphous metal material; Have widely metal targets adaptability, metal targets comprises the most metals except the low melting point active metals such as Li, Na, K; Technological process is simple, and single stage method just can realize the self-assembly preparation of metal nano stripes; Controlled between the cycle 100nm to 1000nm of metal micro-nano striped, wavelength region contains deep ultraviolet and visible light wave range, can overcome the technological limit of existing photoetching, optics prepare aspect very advantageous; Cost is low, quantum of output is large, efficient is high, is easy to realize scale industrialization production.
Description of drawings
Fig. 1 is the ion beam bombardment device synoptic diagram of preparation metal nano stripes provided by the invention.Among the figure: 1, Kaufman molded breadth beam ion rifle; 2, metal targets; 3, the target fixed mechanism that angle is adjustable; 4, the adjustable for height baffle plate of vertical direction; 5, substrate base; 6, the sample worktable; 7, the travel direction of worktable in the bombardment process.
Fig. 2 is the SEM detected result figure of the embodiment of the invention 1 gained sample.
Embodiment
The present invention is further elaborated below in conjunction with specific embodiment, but the present invention is not limited to following examples.Described method is ordinary method if no special instructions.Described material all can get from open commercial sources if no special instructions.
The preparation principle of preparation metal nano stripes method provided by the invention is described: above near substrate 5, place rectangular metal target 2 below in conjunction with Figure of description 1, metal targets is the θ angle with parallel substrate surface direction, this angle can be adjusted with selection mechanism 3, adopt inert gas ion beam rifle 1 (Kaufman molded breadth bundle) vertically to bombard substrate surface, ionic fluid is to be θ angle bombardment target with the metal targets surface normal, ionic fluid via the target surface reflection bombards substrate to be 180 ° of-2 θ angles with the substrate base normal direction, forms orderly nanometer striated structure at substrate surface.Simultaneously the atoms metal that pounded of target deposits at substrate surface, and preferential deposition is at the crest location of nanometer striated structure, and the atoms metal that is in wave trough position is then fallen by ion beam sputtering, thereby forms stable metal nano stripes structure.The nanostructure of self-assembly has kept the identical cycle on this metal Nano structure and the substrate.In the zone near the target edge; the stroke of atoms metal is short, deposition effect strong (deposition effect of atoms metal also can be controlled by vertical range and the θ angle of regulating substrate and target); otherwise more more weak away from deposition effect; the continuous production that (travel direction is as shown in arrow 7, bombards the protection that complete part is in baffle plate 4) just can realize large-area metal nano stripes that moves horizontally by sample worktable 6.
Adopt Kaufman molded breadth beam ion source bombardment system, the ion beam spot diameter is 50mm, and take high-purity Ar (99.999%) as working gas, base vacuum is 2 * 10
-4Pa, operating air pressure are 2 * 10
-2Pa.Substrate material adopts EPI polishing N-type single crystalline Si (100) substrate, and its resistance is 0.01 Ω cm～0.02 Ω cm, and surfaceness is 0.2nm.Substrate Si (100) substrate uses respectively acetone, dehydrated alcohol, deionized water difference ultrasonic cleaning 15min to remove organism and inorganic impurity in advance.Take high-purity Fe (99.995%) piece with flat surface rectangular configuration as metal targets, the angle that target material surface and substrate working platform level are set is 80 °, and the vertical height of position, the end of target and substrate Si (100) substrate is 1mm.Operating temperature is 25 ℃ of normal temperature, and the speed of moving horizontally is 0.05cm/min.Be 120V at acceleration voltage, plate voltage is 3.0kV, and ion beam current density is 1.0 * 10
15Cm
-2S
-1Bombarding conditions under, used substrate material is bombarded, bombard that complete to obtain eigenperiod provided by the invention be that 150nm, Fe metal strip live width are the metal nano stripes of 30nm, the SEM figure of detected result striated structure is (bright fringes represents Fe nanometer striped among the figure) as shown in Figure 2.
Adopt Kaufman molded breadth beam ion source bombardment system, the ion beam spot diameter is 50mm, and take high-purity Ar (99.999%) as working gas, base vacuum is 2 * 10
-4Pa, operating air pressure are 2 * 10
-2Pa.Substrate material adopts EPI polishing P type single crystalline Si (111) substrate, and its resistance is 5.6 Ω cm～10.4 Ω cm, and surfaceness is 0.2nm.Substrate Si (111) substrate uses respectively acetone, dehydrated alcohol, deionized water difference ultrasonic cleaning 15min to remove organism and inorganic impurity in advance.Take high-purity Co (99.995%) piece with flat surface rectangular configuration as metal targets, the angle that target material surface and substrate working platform level are set is 55 °, and the vertical height of position, the end of target and substrate Si (111) substrate is 1mm.Operating temperature remains 700 ℃, and the speed of moving horizontally is 0.02cm/min.Be 150V at acceleration voltage, plate voltage is 0.6kV, and ion beam current density is 1.0 * 10
15Cm
-2S
-1Bombarding conditions under, used substrate material is bombarded, bombard that complete to obtain eigenperiod provided by the invention be that 800nm, Co metal strip live width are the metal nano stripes of 80nm.
Claims (10)
1. method for preparing metal nano stripes, after comprising the steps: the target surface of target is the θ angle to be parallel to substrate surface angle placed, take rare gas element as working gas, vertically bombard substrate surface with ion beam gun, the ionic fluid that described ion beam gun is sent bombards described target to be the θ angle with described target material surface normal, ionic fluid via the target surface reflection bombards described substrate to be 180 ° of-2 θ angles with described substrate normal direction, simultaneously described substrate is moved horizontally, bombard the complete described metal nano stripes that obtains; Wherein, the structure of described target is the rectangular configuration of surfacing;
The material that consists of described target is selected from least a among Al, Ag, Au, Cr, Cu, Co, Fe, Mo, Mn, Nb, Nd, Ni, Pt, Ti, W, Zn and the Zr; The material that consists of described substrate is selected from silicon single crystal, glass, silica glass, sapphire, AlN, ZnO, SiC, LiNbO
3, LiTaO
3At least a with in the amorphous metal material; The surfaceness of described substrate is 0.1nm～10nm;
Described θ angle is 45 °～90 °; Vertical range between the lower-most point of described target and the described substrate horizontal surface is 0mm～20mm;
In the described implant steps, intensifying ring voltage is 100V～500V; Plate voltage is 0.5kV～10.0kV; Ion beam current density is 1.0 * 10
14Cm
-2S
-1～1.0 * 10
16Cm
-2S
-1
Described implant steps is carried out under vacuum condition; Described rare gas element is selected from least a among Ar, Kr and the Xe; In the described vacuum condition, base vacuum is not less than 5 * 10
-4Pa; Operating air pressure is 1 * 10
-2Pa～1 * 10
-1Pa;
Described substrate temperature is 0 ℃～800 ℃; The speed that moves horizontally of described substrate is not less than 0.01cm/min.
2. method according to claim 1 is characterized in that: the material that consists of described target is selected from least a among Ti, Cr, Fe, Co, Ni, Cu and the Zn; Described amorphous metal material is the CoZrNb amorphous; The surfaceness of described substrate is 0.1nm～1.0nm.
3. method according to claim 1, it is characterized in that: described θ angle is 50 °～85 °; Vertical range between the lower-most point of described target and the described substrate horizontal surface is 1mm～10mm.
4. method according to claim 1, it is characterized in that: in the described implant steps, intensifying ring voltage is 120V～200V; Plate voltage is 0.6kV～6.0kV; Ion beam current density is 0.5-5.0 * 10
15Cm
-2S
-1
5. method according to claim 1, it is characterized in that: in the described vacuum condition, base vacuum is not less than 2 * 10
-4Pa; Operating air pressure is 2 * 10
-2Pa.
6. method according to claim 1, it is characterized in that: described substrate temperature is 20 ℃～700 ℃; The speed that moves horizontally of described substrate is 0.02cm/min～0.20cm/min.
7. arbitrary described method according to claim 1-6 is characterized in that: described ion beam gun is Kaufman molded breadth beam ion rifle.
8. the metal nano stripes for preparing of the arbitrary described method of claim 1-7.
9. striped according to claim 8, it is characterized in that: be 100nm～1000nm the eigenperiod of described metal nano stripes; Live width is 10nm～100nm.
10. striped according to claim 9, it is characterized in that: be 100nm～800nm the eigenperiod of described metal nano stripes; Live width is 20nm～80nm.
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| DE102014107458B4 (en) * | 2014-05-27 | 2020-02-13 | Helmholtz-Zentrum Dresden - Rossendorf E.V. | patterning methods |
| CN105271107B (en) * | 2015-09-29 | 2017-03-29 | 中国人民解放军国防科学技术大学 | The large-area nano micro structure regulation and control preparation method of fused quartz optical surface |
Citations (3)
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|---|---|---|---|---|
| CN1516826A (en) * | 2001-04-19 | 2004-07-28 | 纳幕尔杜邦公司 | Ion-beam deposition process for mfg. attenuated phase shift photomask blanks |
| RU2347741C1 (en) * | 2007-08-27 | 2009-02-27 | Государственное образовательное учреждение высшего профессионального образования "Уральский государственный технический университет - УПИ имени первого Президента России Б.Н.Ельцина" | Method of producing nanocrystalline coats based on nanocrystals of lithium or sodium fluoride |
| CN101748374A (en) * | 2009-12-25 | 2010-06-23 | 云南大学 | Method for growing high density and fine self-assembled Ge quantum dot with ion beam sputtering technology |
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2011
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1516826A (en) * | 2001-04-19 | 2004-07-28 | 纳幕尔杜邦公司 | Ion-beam deposition process for mfg. attenuated phase shift photomask blanks |
| RU2347741C1 (en) * | 2007-08-27 | 2009-02-27 | Государственное образовательное учреждение высшего профессионального образования "Уральский государственный технический университет - УПИ имени первого Президента России Б.Н.Ельцина" | Method of producing nanocrystalline coats based on nanocrystals of lithium or sodium fluoride |
| CN101748374A (en) * | 2009-12-25 | 2010-06-23 | 云南大学 | Method for growing high density and fine self-assembled Ge quantum dot with ion beam sputtering technology |
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