CN103745917B - A kind of electric field controls prepares the method for nanostructure on monocrystalline silicon substrate surface - Google Patents
A kind of electric field controls prepares the method for nanostructure on monocrystalline silicon substrate surface Download PDFInfo
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- 239000000758 substrate Substances 0.000 title claims abstract description 119
- 229910021421 monocrystalline silicon Inorganic materials 0.000 title claims abstract description 117
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- 238000000034 method Methods 0.000 title claims abstract description 20
- 229910052751 metal Inorganic materials 0.000 claims abstract description 32
- 239000002184 metal Substances 0.000 claims abstract description 32
- 238000001451 molecular beam epitaxy Methods 0.000 claims abstract description 21
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 20
- 239000010703 silicon Substances 0.000 claims abstract description 20
- 238000000151 deposition Methods 0.000 claims abstract description 15
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 11
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 10
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- 229910052738 indium Inorganic materials 0.000 description 32
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
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- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
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Abstract
一种电场控制在单晶硅基片表面制备纳米结构的方法,属于纳米材料技术领域,按以下步骤进行:(1)选用n型Si(111)硅圆晶片,切割制成长方形的单晶硅基片;(2)固定于分子束外延室的真空室样品台上;在真空条件下加热清洁其表面;(3)向表面沉积Au原子,获得具有不同重构的表面结构;(4)将In沉积到单晶硅基片中心,获得矩形薄膜片层;(5)施加直流电场驱动电迁移,控制电迁移扩散,获得准二维金属纳米结构。本发明通过预先沉积在硅表面的异质金属膜层将在电场作用下发生定向的迁移扩散,扩散的结果是原始膜层均匀展宽而表面形貌不被破坏,有效地消除某些结构缺陷,如使薄膜表面普遍存在的三维岛状结构趋于平整化,实现原子级表面加工。
A method for preparing a nanostructure on the surface of a single crystal silicon substrate under electric field control, which belongs to the technical field of nanomaterials, and is carried out according to the following steps: (1) Select an n-type Si (111) silicon wafer and cut it into a rectangular single crystal silicon substrate; (2) fixed on the vacuum chamber sample stage of the molecular beam epitaxy chamber; heating and cleaning its surface under vacuum conditions; (3) depositing Au atoms on the surface to obtain surface structures with different reconstructions; (4) In is deposited on the center of the single crystal silicon substrate to obtain a rectangular thin film layer; (5) applying a DC electric field to drive electromigration, controlling electromigration diffusion, and obtaining a quasi-two-dimensional metal nanostructure. In the present invention, the heterogeneous metal film layer deposited on the silicon surface in advance will undergo directional migration and diffusion under the action of an electric field. As a result of the diffusion, the original film layer will be uniformly widened without destroying the surface morphology, effectively eliminating some structural defects. For example, the ubiquitous three-dimensional island structure on the surface of the film tends to be flattened to achieve atomic-level surface processing.
Description
技术领域technical field
本发明属于纳米材料技术领域,特别涉及一种电场控制在单晶硅基片表面制备纳米结构的方法。The invention belongs to the technical field of nanomaterials, in particular to a method for preparing nanostructures on the surface of a single crystal silicon substrate under electric field control.
背景技术Background technique
外场作用下固体表面原子的迁移运动是一个具有广泛应用背景的基础问题。半导体硅基底上施加一个平行于基底表面的直流电场时,其表面上发生的一系列电迁移扩散现象就是一个典型的例子,具有非常重要的物理意义。众所周知,作为半导体工业中最重要的材料,硅和各种硅基微/纳结构器件构成了现代电子与信息产业的基石;而各种纳米结构的器件化和实用化都需要建立在纳米材料的控制生长和相关物理效应的澄清的基础之上。因此,深入探索外场作用下材料表面纳米尺度形貌和结构特征的变化规律,进而通过宏观的外力作用实现对纳米结构的操纵已经成为许多纳米技术应用中的关键。以扫描隧道显微镜(STM)为工具,对表面原子或原子团簇施加纵向电场进行操纵移动以形成各种微小的纳米结构是一项颇具代表性的成熟技术,但它在构建包含更多原子(如104~106个原子)的较大尺寸纳米结构时并不适用;而同样广为人知的自组装生长技术虽然适于制备包含大量原子的纳米结构,但却难以实现其局部结构的精细调控。The migration of atoms on a solid surface under the action of an external field is a basic problem with a wide range of applications. When a DC electric field parallel to the surface of the substrate is applied on the semiconductor silicon substrate, a series of electromigration and diffusion phenomena occurring on the surface is a typical example, which has very important physical significance. As we all know, as the most important material in the semiconductor industry, silicon and various silicon-based micro/nanostructure devices constitute the cornerstone of the modern electronics and information industry; and the deviceization and practical application of various nanostructures need to be based on the basis of nanomaterials. Based on the clarification of controlled growth and associated physical effects. Therefore, it has become the key to many nanotechnology applications to deeply explore the change rules of the nanoscale morphology and structural characteristics of the surface of materials under the action of external fields, and then realize the manipulation of nanostructures through macroscopic external forces. Using scanning tunneling microscopy (STM) as a tool, applying a longitudinal electric field to surface atoms or atomic clusters to manipulate and move them to form various tiny nanostructures is a representative and mature technology, but it is in the construction of more atoms (such as 10 4 to 10 6 atoms) is not suitable for large-scale nanostructures; and the self-assembly growth technology, which is also well known, is suitable for preparing nanostructures containing a large number of atoms, but it is difficult to achieve fine regulation of its local structure.
发明内容Contents of the invention
针对现有电场控制制备纳米结构在技术上存在的上述问题,本发明提供一种电场控制在单晶硅基片表面制备纳米结构的方法,通过水平方向上直流电场的作用使单晶硅基片的膜层均匀扩展来形成纳米有序结构。Aiming at the above-mentioned problems existing in the technology of preparing nanostructures by electric field control, the present invention provides a method for preparing nanostructures on the surface of a single crystal silicon substrate by electric field control, which makes the single crystal silicon substrate The film layer is uniformly expanded to form a nano-ordered structure.
本发明的一种电场控制在单晶硅基片表面制备纳米结构的方法按以下步骤进行:A kind of electric field control of the present invention prepares the method for nanostructure on the surface of monocrystalline silicon substrate to carry out according to the following steps:
1、选用镜面抛光的电阻率为50~100Ω·cm的n型Si(111)硅圆晶片,沿长边平行于〈1-10〉方向进行切割,制成长方形的单晶硅基片;1. Select an n-type Si (111) silicon wafer with a mirror-polished resistivity of 50-100Ω·cm, cut along the long side parallel to the <1-10> direction, and make a rectangular single-crystal silicon substrate;
2、将单晶硅基片固定于分子束外延室的真空室样品台上;在真空室压强≤2×10-8Pa的超高真空条件下,将单晶硅基片加热至1473±10K并保持2~6s,清洁其表面;2. Fix the monocrystalline silicon substrate on the vacuum chamber sample stage of the molecular beam epitaxy chamber; under the ultra-high vacuum condition of the vacuum chamber pressure ≤ 2×10 -8 Pa, heat the monocrystalline silicon substrate to 1473±10K And keep it for 2-6s to clean the surface;
3、通过蒸发源向表面经过清洁的单晶硅基片表面沉积0.1~1层Au原子,在单晶硅基片表面获得具有不同重构的金吸附单晶硅表面结构;沉积时控制真空室气压≤1×10-7Pa,单晶硅基片温度为873±10K;所述的不同重构的金吸附单晶硅表面结构是指7×7、(7×7+5×2)、5×2、(5×2+α-√3×√3)、α-√3×√3或β-√3×√3表面结构;3. Deposit 0.1 to 1 layer of Au atoms on the surface of the cleaned single crystal silicon substrate through the evaporation source, and obtain gold-adsorbed single crystal silicon surface structures with different reconstructions on the surface of the single crystal silicon substrate; control the vacuum chamber during deposition Air pressure ≤ 1×10 -7 Pa, temperature of monocrystalline silicon substrate is 873±10K; the surface structure of different reconstructed gold-adsorbed monocrystalline silicon refers to 7×7, (7×7+5×2), 5×2, (5×2+α-√3×√3), α-√3×√3 or β-√3×√3 surface structure;
4、将金属In在室温下通过分子束外延室内的掩模上的狭缝窗口蒸发沉积到单晶硅基片中心位置,在单晶硅基片上获得矩形薄膜片层,矩形薄膜片层的厚度为2.0±0.2ML;4. Evaporate and deposit metal In at room temperature through the slit window on the mask in the molecular beam epitaxy chamber to the center of the single crystal silicon substrate, and obtain a rectangular thin film layer on the single crystal silicon substrate. The thickness of the rectangular thin film layer is 2.0±0.2ML;
5、沿着〈1-10〉方向对单晶硅基片上的矩形薄膜片层施加直流电场开始驱动电迁移,控制矩形薄膜片层的电迁移扩散,电流强度为0.1~0.5A,施加电流的时间为1~60min,施加电场时单晶硅基片的温度为630~763K,在单晶硅基片表面获得准二维金属纳米结构。5. Apply a direct current electric field to the rectangular thin film layer on the single crystal silicon substrate along the <1-10> direction to start driving electromigration, and control the electromigration diffusion of the rectangular thin film layer. The current intensity is 0.1-0.5A, and the applied current The time is 1-60 minutes, the temperature of the single-crystal silicon substrate is 630-763K when the electric field is applied, and a quasi-two-dimensional metal nanostructure is obtained on the surface of the single-crystal silicon substrate.
上述方法中,掩模的窗口为长方形或狭缝式,宽度在50~200μm,掩模材质选用金属钽。In the above method, the window of the mask is rectangular or slit, with a width of 50-200 μm, and the material of the mask is metal tantalum.
上述方法中,沉积金属的单原子层(monolayer,ML)数表示金属的覆盖度,一个单原子层(ML)对应于表面上每平方厘米包含7.8×1014个原子。In the above method, the number of monoatomic layers (monolayer, ML) of the deposited metal represents the coverage of the metal, and one monoatomic layer (ML) corresponds to 7.8×10 14 atoms per square centimeter on the surface.
传统电迁移制备纳米间隙结构是利用其破坏性,而本发明提供的方法属于半导体表面异质电迁移,是通过水平方向上直流电场的作用使膜层均匀扩展来形成纳米有序结构。不同于发生在集成电路微小互联引线中导致金属或合金薄膜材料破坏失效的传统电迁移,半导体表面电迁移是一类独特的物质输运现象,它起因于表面原子的定向移动,对表面形貌具有重要的影响作用。按照迁移物的特点,又可以将其分为两类:其一,对于清洁的硅邻晶表面,即表面只存在同质的硅吸附原子时,直流电场和电流依作用方向的不同会形成复杂的表面形貌(包括规则台阶结构、台阶束和台阶蜿蜒结构);自从A.V.Latyshev等首次报道在邻晶Si(111)面上直流电所导致的台阶结构不稳定性以来,国际上大量的工作主要集中在对此现象的唯象研究和理论建模上,其目的是寻找这些表面台阶结构的控制因素,期望这些特定尺度、有序排列的台阶可以作为薄膜材料外延生长时的优先成核中心或作为合成纳米结构的模板;曾有人利用这一特性进行了在邻晶面上生长量子线和量子点的实验,但是由于单原子台阶形状很不规则,很难得到有序排列的量子线和量子点;其二是表面异质电迁移,它指的是当对清洁的半导体硅基底施加水平方向直流电场时,预先沉积在硅表面的异质金属膜层将在电场作用下发生定向的迁移扩散,扩散的结果是原始膜层均匀展宽而表面形貌不被破坏,并且通过原子在表面的迁移运动,还能有效地消除某些结构缺陷,如使薄膜表面普遍存在的三维岛状结构趋于平整化,实现原子级表面加工。Traditional electromigration is used to prepare nano-gap structures by using its destructiveness, while the method provided by the present invention belongs to semiconductor surface heterogeneous electromigration, which is to form a nano-ordered structure by uniformly expanding the film layer through the action of a direct current electric field in the horizontal direction. Different from the traditional electromigration that occurs in the tiny interconnection wires of integrated circuits and leads to the destruction and failure of metal or alloy thin film materials, electromigration on the surface of semiconductors is a unique type of material transport phenomenon, which is caused by the directional movement of surface atoms and has a significant impact on surface morphology. have an important influence. According to the characteristics of the migratory substances, they can be divided into two categories: first, for the clean silicon adjacent crystal surface, that is, when there are only homogeneous silicon adatoms on the surface, the DC electric field and current will form complex transitions depending on the direction of action. The surface morphology (including regular step structure, step bundle and step meander structure); since A.V.Latyshev first reported the step structure instability caused by direct current on the adjacent crystal Si(111) surface, a lot of work in the world Mainly focus on the phenomenological research and theoretical modeling of this phenomenon, the purpose of which is to find the controlling factors of these surface step structures, expecting that these specific scale and orderly arranged steps can be used as the preferential nucleation center during the epitaxial growth of thin film materials Or as a template for synthesizing nanostructures; some people have used this characteristic to grow quantum wires and quantum dots on adjacent crystal planes. However, due to the irregular shape of single-atom steps, it is difficult to obtain ordered quantum wires and quantum dots. Quantum dots; the second is surface heterogeneous electromigration, which means that when a horizontal DC electric field is applied to a clean semiconductor silicon substrate, the heterogeneous metal film layer deposited on the silicon surface in advance will undergo directional migration under the action of the electric field Diffusion, the result of diffusion is that the original film layer is uniformly expanded without destroying the surface morphology, and through the migration of atoms on the surface, it can also effectively eliminate some structural defects, such as the tendency of the three-dimensional island structure that commonly exists on the surface of the film. In planarization, to achieve atomic level surface processing.
本发明的电场控制在单晶硅基片表面制备纳米结构的方法可以直接在清洁的单晶硅基片上透过掩模沉积薄膜,也可以先在整个单晶硅基片表面沉积某一种金属(如金、银或铜),然后再利用掩模沉积形成叠层薄膜,The method for preparing nanostructures on the surface of a single crystal silicon substrate by controlling the electric field of the present invention can directly deposit a thin film through a mask on a clean single crystal silicon substrate, or deposit a certain metal on the entire surface of a single crystal silicon substrate (such as gold, silver or copper), and then use mask deposition to form a laminated film,
通过硅基片两端用钽金属夹具(同时也作为电极)固定,硅基底上用于驱动电迁移扩散而施加的直流电场是沿着水平方向的,这使得原先沉积成规则形状的膜片能够按要求演变成不同尺寸、形貌和表面结构;通过电迁移参数的调控也可以获得具有一定成分的单金属、合金或硅化物纳米结构。By fixing both ends of the silicon substrate with tantalum metal clamps (also used as electrodes), the DC electric field applied on the silicon substrate to drive the electromigration diffusion is along the horizontal direction, which makes the film deposited in a regular shape possible. It evolves into different sizes, shapes and surface structures as required; through the regulation of electromigration parameters, single metal, alloy or silicide nanostructures with a certain composition can also be obtained.
在已知衬底材料和镀膜材料的性质条件下,精确控制施加表面直流电场的电流大小、取向和时间,利用电迁移扩散的特点,达到按需移动的目的;事先沉积0.1~1单层的金原子,构成不同的表面移动平台,在此之上沉积的其它金属的迁移扩散速率可以被精确控制。Under the condition of knowing the properties of the substrate material and coating material, precisely control the current magnitude, orientation and time of the applied surface DC electric field, and use the characteristics of electromigration and diffusion to achieve the purpose of moving on demand; deposit 0.1 to 1 monolayer in advance The gold atoms constitute different surface mobile platforms on which the migration and diffusion rates of other metals deposited can be precisely controlled.
本发明利用与分子束外延设备集成在一起的场发射扫描电子显微镜和反射高能电子衍射装置,在通电驱动电迁移扩散的同时,可连续观察测量样品表面形貌和表面结构的变化,并进行记录。纳米结构形成以后,依据所配备电子能谱仪情况,可对该纳米结构进行原位或非原位的化学成份、价态和电子结构的分析表征。The present invention utilizes a field emission scanning electron microscope and a reflection high-energy electron diffraction device integrated with molecular beam epitaxy equipment to continuously observe and measure changes in the surface morphology and surface structure of samples while electrifying and driving electromigration diffusion, and record them . After the nanostructure is formed, in-situ or ex-situ chemical composition, valence state and electronic structure analysis and characterization of the nanostructure can be performed according to the equipped electron spectrometer.
附图说明Description of drawings
图1为Au原子覆盖度与温度(不同重构表面结构)关系曲线图;Figure 1 is a graph showing the relationship between Au atomic coverage and temperature (different reconstructed surface structures);
图2为本发明实施例中的电场控制在单晶硅基片表面制备纳米结构装置结构示意图;2 is a schematic diagram of the structure of a nanostructure device prepared on the surface of a single crystal silicon substrate by electric field control in an embodiment of the present invention;
图中,1、真空室,2、电子枪系统,3、单晶硅基片,4、二次电子探测器,5、线性运动操纵机构,6、挡板,7、蒸发源,8、观察、控制和记录系统,9、光纤,10、衍射电子束,11、掩模;In the figure, 1. Vacuum chamber, 2. Electron gun system, 3. Monocrystalline silicon substrate, 4. Secondary electron detector, 5. Linear motion control mechanism, 6. Baffle plate, 7. Evaporation source, 8. Observation, Control and recording system, 9. Optical fiber, 10. Diffraction electron beam, 11. Mask;
图3为本发明实施例中的单晶硅基片与电极布置示意图;Fig. 3 is a schematic diagram of a monocrystalline silicon substrate and electrode layout in an embodiment of the present invention;
图中,3、单晶硅基片,12、掩模窗口,13、钽电极;In the figure, 3, single crystal silicon substrate, 12, mask window, 13, tantalum electrode;
图4为本发明实施例1中两个单原子层厚度(2.0ML)的金属铟(In)在清洁的Si(111)硅表面由直流电场驱动的结构演变过程扫描电镜观察图;图中,(a)初始薄膜,(b)施加0.1A电流作用1min,衬底温度630K,(c)施加0.1A电流作用10min,(d)施加0.1A电流作用30min,(e)施加0.3A电流作用3min,衬底温度763K,(f)施加0.3A电流作用10min,(g)施加0.3A电流作用20min;Fig. 4 is a scanning electron microscope observation diagram of the structure evolution process of metal indium (In) with two monoatomic layer thicknesses (2.0ML) on a clean Si(111) silicon surface driven by a DC electric field in Example 1 of the present invention; in the figure, (a) initial film, (b) apply 0.1A current for 1min, substrate temperature 630K, (c) apply 0.1A current for 10min, (d) apply 0.1A current for 30min, (e) apply 0.3A current for 3min , substrate temperature 763K, (f) apply 0.3A current for 10min, (g) apply 0.3A current for 20min;
图5为本发明实施例2中的两个单原子层(2.0ML)厚度的金属铟(In)在预先沉积覆盖了1.0单原子层金(Au)的Si(111)-β-√3×√3-Au表面由直流电场驱动的结构演变过程电子显微图;初始薄膜的制备方法与实施例1中的(a)图完全相同,(m)施加0.1A电流作用1min,衬底温度630K,(n)施加0.1A电流作用4min。Fig. 5 is the Si(111)-β-√3× √ Electron micrograph of the structural evolution process of the 3-Au surface driven by a DC electric field; the preparation method of the initial film is exactly the same as that in Example 1 (a), (m) apply a 0.1A current for 1min, and the substrate temperature is 630K , (n) Apply a 0.1A current for 4min.
图6为本发明实施例3中的两个单原子层(2.0ML)厚度的金属铟(In)在预先沉积覆盖了0.5单原子层金(Au)的Si(111)-5×2-Au表面由直流电场驱动的结构演变过程电子显微图;初始薄膜的制备方法与实施例1中的(a)图完全相同,(x)施加0.1A电流作用1min,衬底温度630K,(y)施加0.1A电流作用10min,630K,(z)继续施加0.2A电流持续10min,衬底温度763K。Figure 6 shows the Si(111)-5×2-Au covered with 0.5 monoatomic layer gold (Au) covered with two monoatomic layers (2.0ML) of metal indium (In) in Example 3 of the present invention. Electron micrograph of the surface structure evolution process driven by a DC electric field; the preparation method of the initial film is exactly the same as that in Example 1 (a), (x) 0.1A current is applied for 1 min, and the substrate temperature is 630K, (y) Apply 0.1A current for 10min, 630K, (z) continue to apply 0.2A current for 10min, substrate temperature 763K.
图7为本发明实施例4中的两个单原子层(2.0ML)厚度的金属铟(In)在预先沉积覆盖了0.7单原子层金(Au)的Si(111)-(5×2+α-√3×√3)-Au表面由直流电场驱动的结构演变过程电子显微图;初始薄膜的制备方法与实施例1中的(a)图完全相同,(u)施加0.1A电流作用5min,衬底温度630K,(v)施加0.1A电流作用10min,630K,(w)施加0.1A电流持续至30min,630K。Fig. 7 is the Si(111)-(5×2+ Electron micrograph of the structure evolution process of the α-√3×√3)-Au surface driven by a DC electric field; the preparation method of the initial film is exactly the same as that in (a) in Example 1, (u) applying a 0.1A current 5min, substrate temperature 630K, (v) apply 0.1A current for 10min, 630K, (w) apply 0.1A current for 30min, 630K.
具体实施方式detailed description
本发明实施例中采用的分子束外延室为日本真空(ULVAC)制造的分子束外延室。The molecular beam epitaxy chamber used in the embodiment of the present invention is a molecular beam epitaxy chamber manufactured by Japan Vacuum (ULVAC).
本发明实施例中采用的观测设备为日立S–4200型场发射扫描电子显微镜(FE–SEM)和微探针型反射高能电子衍射(μ-probeRHEED)装置。The observation equipment used in the embodiment of the present invention is a Hitachi S-4200 field emission scanning electron microscope (FE-SEM) and a microprobe reflection high-energy electron diffraction (μ-probeRHEED) device.
本发明实施例中采用的线形运动操纵机构为ULVAC制造的分子束外延室配套使用的的线形运动操纵机构。The linear motion control mechanism used in the embodiment of the present invention is a linear motion control mechanism used in conjunction with the molecular beam epitaxy chamber manufactured by ULVAC.
本发明实施例中采用的金属In蒸发源的重量纯度99.9999%。The weight purity of the metal In evaporation source used in the embodiment of the present invention is 99.9999%.
本发明实施例中采用的Au蒸发源的重量纯度99.9999%。The weight purity of the Au evaporation source used in the embodiment of the present invention is 99.9999%.
本发明实施例中金属钽的重量纯度99.9999%。The weight purity of metal tantalum in the embodiment of the present invention is 99.9999%.
实施例1Example 1
本发明实施例中的电场控制在单晶硅基片表面制备纳米结构装置如图2所示,包括真空室1,电子枪系统2,二次电子探测器4,线性运动操纵机构5,挡板6,蒸发源7,观察、控制和记录系统8,光纤9,衍射电子束10,掩模11;The electric field control in the embodiment of the present invention prepares a nanostructure device on the surface of a single crystal silicon substrate as shown in Figure 2, including a vacuum chamber 1, an electron gun system 2, a secondary electron detector 4, a linear motion manipulation mechanism 5, and a baffle 6 , evaporation source 7, observation, control and recording system 8, optical fiber 9, diffracted electron beam 10, mask 11;
选用镜面抛光的电阻率为50~100Ω·cm的n型Si(111)硅圆晶片,沿长边平行于〈1-10〉方向进行切割制成长方形的单晶硅基片;Choose mirror-polished n-type Si (111) silicon wafers with a resistivity of 50-100Ω·cm, and cut along the long side parallel to the <1-10> direction to make rectangular single-crystal silicon substrates;
将单晶硅基片固定于分子束外延室的真空室样品台上,在真空室压强≤2×10-8Pa条件下,将单晶硅基片加热至1473±10K并保持2s,清洁其表面;此时获得清洁的Si(111)7×7表面;Fix the single crystal silicon substrate on the vacuum chamber sample stage of the molecular beam epitaxy chamber, under the condition of vacuum chamber pressure ≤ 2×10 -8 Pa, heat the single crystal silicon substrate to 1473±10K and keep it for 2s, clean it surface; at this point a clean Si(111)7×7 surface is obtained;
将金属In在室温下通过分子束外延室内的掩模上的狭缝窗口蒸发沉积到单晶硅基片中心位置,在单晶硅基片上获得矩形薄膜片层,矩形薄膜片层的厚度为2.0±0.2ML;掩模的窗口为长方形或狭缝式,宽度在150μm,掩模材质选用钽;在蒸发镀铟膜时,用反射式高能电子衍射装置随时监测衍射斑点花样,当出现√3×√3表面重构的衍射花样时就表明铟的覆盖度刚好为1/3ML(三分之一单原子层),并记录这个时间;根据蒸镀铟的速率和时间就能准确控制沉积铟薄膜的覆盖度大小,当蒸发速率相同,蒸发时间为覆盖度1/3ML的时间的6倍时,既得到覆盖度为2.0ML的铟膜;Metal In is evaporated and deposited on the center of the single crystal silicon substrate through the slit window on the mask in the molecular beam epitaxy chamber at room temperature, and a rectangular thin film layer is obtained on the single crystal silicon substrate. The thickness of the rectangular thin film layer is 2.0 ±0.2ML; the window of the mask is rectangular or slit, the width is 150μm, and the mask material is tantalum; when evaporating indium film, use the reflective high-energy electron diffraction device to monitor the diffraction spot pattern at any time, when √3× √3 The surface reconstructed diffraction pattern shows that the coverage of indium is just 1/3ML (one-third monoatomic layer), and this time is recorded; the deposition of indium film can be accurately controlled according to the rate and time of evaporation indium When the evaporation rate is the same and the evaporation time is 6 times that of the coverage of 1/3ML, an indium film with a coverage of 2.0ML is obtained;
沿着〈1-10〉方向对单晶硅基片上的矩形薄膜片层施加直流电场开始驱动电迁移,控制矩形薄膜片层的电迁移扩散,电流强度为0.1~0.3A,施加电流的时间为1~20min,施加电场时单晶硅基片的温度为630K~763K,在单晶硅基片表面获得准二维金属纳米结构;由直流电场驱动的结构演变过程如图4所示。Apply a DC electric field to the rectangular thin film layer on the single crystal silicon substrate along the <1-10> direction to start driving electromigration, control the electromigration and diffusion of the rectangular thin film layer, the current intensity is 0.1-0.3A, and the time for applying the current is 1 to 20 minutes, when the electric field is applied, the temperature of the single crystal silicon substrate is 630K to 763K, and a quasi-two-dimensional metal nanostructure is obtained on the surface of the single crystal silicon substrate; the structure evolution process driven by the DC electric field is shown in Figure 4.
实施例2Example 2
电场控制在单晶硅基片表面制备纳米结构装置同实施例1;The nanostructure device prepared on the surface of a single crystal silicon substrate by electric field control is the same as that in Example 1;
选用镜面抛光的电阻率为50~100Ω·cm的n型Si(111)硅圆晶片,沿长边平行于〈1-10〉方向进行切割制成长方形的单晶硅基片;Choose mirror-polished n-type Si (111) silicon wafers with a resistivity of 50-100Ω·cm, and cut along the long side parallel to the <1-10> direction to make rectangular single-crystal silicon substrates;
将单晶硅基片固定于分子束外延室的真空室样品台上,在真空室压强≤2×10-8Pa条件下,将单晶硅基片加热至1473±10K并保持2s,清洁其表面;此时获得清洁的Si(111)7×7表面;Fix the single crystal silicon substrate on the vacuum chamber sample stage of the molecular beam epitaxy chamber, under the condition of vacuum chamber pressure ≤ 2×10 -8 Pa, heat the single crystal silicon substrate to 1473±10K and keep it for 2s, clean it surface; at this point a clean Si(111)7×7 surface is obtained;
通过蒸发源向表面经过清洁的单晶硅基片表面沉积1.0层Au原子,在单晶硅基片表面获得β-√3×√3金吸附单晶硅表面结构;沉积时控制真空室气压≤1×10-7Pa,单晶硅基片温度为873±10K;Deposit 1.0 layer of Au atoms on the surface of the cleaned single crystal silicon substrate through the evaporation source, and obtain a β-√3×√3 gold adsorption single crystal silicon surface structure on the surface of the single crystal silicon substrate; control the vacuum chamber pressure ≤ during deposition 1×10 -7 Pa, the temperature of single crystal silicon substrate is 873±10K;
将金属In在室温下通过分子束外延室内的掩模上的狭缝窗口蒸发沉积到单晶硅基片中心位置,在单晶硅基片上获得矩形薄膜片层,矩形薄膜片层的厚度为2.0±0.2ML;掩模的窗口为长方形或狭缝式,宽度在150μm,掩模材质选用钽;在蒸发镀铟膜时,用反射式高能电子衍射装置随时监测衍射斑点花样,当出现√3×√3表面重构的衍射花样时就表明铟的覆盖度刚好为1/3ML(三分之一单原子层),并记录这个时间;根据蒸镀铟的速率和时间就能准确控制沉积铟薄膜的覆盖度大小,当蒸发速率相同,蒸发时间为覆盖度1/3ML的时间的6倍时,既得到覆盖度为2.0ML的铟膜;Metal In is evaporated and deposited on the center of the single crystal silicon substrate through the slit window on the mask in the molecular beam epitaxy chamber at room temperature, and a rectangular thin film layer is obtained on the single crystal silicon substrate. The thickness of the rectangular thin film layer is 2.0 ±0.2ML; the window of the mask is rectangular or slit, the width is 150μm, and the mask material is tantalum; when evaporating indium film, use the reflective high-energy electron diffraction device to monitor the diffraction spot pattern at any time, when √3× √3 The surface reconstructed diffraction pattern shows that the coverage of indium is just 1/3ML (one-third monoatomic layer), and this time is recorded; the deposition of indium film can be accurately controlled according to the rate and time of evaporation indium When the evaporation rate is the same and the evaporation time is 6 times that of the coverage of 1/3ML, an indium film with a coverage of 2.0ML is obtained;
沿着〈1-10〉方向对单晶硅基片上的矩形薄膜片层施加直流电场开始驱动电迁移,控制矩形薄膜片层的电迁移扩散,电流强度为0.1A,施加电流的时间为1~4min,施加电场时单晶硅基片的温度为630K,在单晶硅基片表面获得准二维金属纳米结构;由直流电场驱动的结构演变过程如图5所示。Apply a DC electric field to the rectangular thin film layer on the single crystal silicon substrate along the <1-10> direction to start driving electromigration, control the electromigration and diffusion of the rectangular thin film layer, the current intensity is 0.1A, and the time of applying the current is 1~ For 4 minutes, the temperature of the single crystal silicon substrate was 630K when the electric field was applied, and a quasi-two-dimensional metal nanostructure was obtained on the surface of the single crystal silicon substrate; the structure evolution process driven by the DC electric field is shown in Figure 5.
实施例3Example 3
电场控制在单晶硅基片表面制备纳米结构装置同实施例1;The preparation of nanostructure devices on the surface of a single crystal silicon substrate by electric field control is the same as in Example 1;
选用镜面抛光的电阻率为50~100Ω·cm的n型Si(111)硅圆晶片,沿长边平行于〈1-10〉方向进行切割制成长方形的单晶硅基片;Choose mirror-polished n-type Si (111) silicon wafers with a resistivity of 50-100Ω·cm, and cut along the long side parallel to the <1-10> direction to make rectangular single-crystal silicon substrates;
将单晶硅基片固定于分子束外延室的真空室样品台上,在真空室压强≤2×10-8Pa条件下,将单晶硅基片加热至1473±10K并保持2s,清洁其表面;此时获得清洁的Si(111)7×7表面;Fix the single crystal silicon substrate on the vacuum chamber sample stage of the molecular beam epitaxy chamber, under the condition of vacuum chamber pressure ≤ 2×10 -8 Pa, heat the single crystal silicon substrate to 1473±10K and keep it for 2s, clean it surface; at this point a clean Si(111)7×7 surface is obtained;
通过蒸发源向表面经过清洁的单晶硅基片表面沉积0.5层Au原子,在单晶硅基片表面获得5×2金吸附单晶硅表面结构;沉积时控制真空室气压≤1×10-7Pa,单晶硅基片温度为873±10K;Deposit 0.5 layers of Au atoms on the surface of the cleaned single crystal silicon substrate through the evaporation source, and obtain a 5×2 gold adsorption single crystal silicon surface structure on the surface of the single crystal silicon substrate; control the vacuum chamber pressure ≤ 1×10 - 7 Pa, the temperature of the single crystal silicon substrate is 873±10K;
将金属In在室温下通过分子束外延室内的掩模上的狭缝窗口蒸发沉积到单晶硅基片中心位置,在单晶硅基片上获得矩形薄膜片层,矩形薄膜片层的厚度为2.0±0.2ML;掩模的窗口为长方形或狭缝式,宽度在150μm,掩模材质选用钽;在蒸发镀铟膜时,用反射式高能电子衍射装置随时监测衍射斑点花样,当出现√3×√3表面重构的衍射花样时就表明铟的覆盖度刚好为1/3ML(三分之一单原子层),并记录这个时间;根据蒸镀铟的速率和时间就能准确控制沉积铟薄膜的覆盖度大小,当蒸发速率相同,蒸发时间为覆盖度1/3ML的时间的6倍时,既得到覆盖度为2.0ML的铟膜;Metal In is evaporated and deposited on the center of the single crystal silicon substrate through the slit window on the mask in the molecular beam epitaxy chamber at room temperature, and a rectangular thin film layer is obtained on the single crystal silicon substrate. The thickness of the rectangular thin film layer is 2.0 ±0.2ML; the window of the mask is rectangular or slit, the width is 150μm, and the mask material is tantalum; when evaporating indium film, use the reflective high-energy electron diffraction device to monitor the diffraction spot pattern at any time, when √3× √3 The surface reconstructed diffraction pattern shows that the coverage of indium is just 1/3ML (one-third monoatomic layer), and this time is recorded; the deposition of indium film can be accurately controlled according to the rate and time of evaporation indium When the evaporation rate is the same and the evaporation time is 6 times that of the coverage of 1/3ML, an indium film with a coverage of 2.0ML is obtained;
沿着〈1-10〉方向对单晶硅基片上的矩形薄膜片层施加直流电场开始驱动电迁移,控制矩形薄膜片层的电迁移扩散,电流强度为0.1~0.2A,施加电流的时间为1~10min,施加电场时单晶硅基片的温度为630K~763K,在单晶硅基片表面获得准二维金属纳米结构;由直流电场驱动的结构演变过程如图6所示。Apply a direct current electric field to the rectangular thin film layer on the single crystal silicon substrate along the <1-10> direction to start driving electromigration, control the electromigration and diffusion of the rectangular thin film layer, the current intensity is 0.1-0.2A, and the time for applying the current is 1 to 10 minutes, when the electric field is applied, the temperature of the single crystal silicon substrate is 630K to 763K, and a quasi-two-dimensional metal nanostructure is obtained on the surface of the single crystal silicon substrate; the structure evolution process driven by the DC electric field is shown in Figure 6.
实施例4Example 4
电场控制在单晶硅基片表面制备纳米结构装置同实施例1;The nanostructure device prepared on the surface of a single crystal silicon substrate by electric field control is the same as that in Example 1;
选用镜面抛光的电阻率为50~100Ω·cm的n型Si(111)硅圆晶片,沿长边平行于〈1-10〉方向进行切割制成长方形的单晶硅基片;Choose mirror-polished n-type Si (111) silicon wafers with a resistivity of 50-100Ω·cm, and cut along the long side parallel to the <1-10> direction to make rectangular single-crystal silicon substrates;
将单晶硅基片固定于分子束外延室的真空室样品台上,在真空室压强≤2×10-8Pa条件下,将单晶硅基片加热至1473±10K并保持4s,清洁其表面;此时获得清洁的Si(111)7×7表面;Fix the single crystal silicon substrate on the vacuum chamber sample stage of the molecular beam epitaxy chamber, under the condition of the vacuum chamber pressure ≤ 2×10 -8 Pa, heat the single crystal silicon substrate to 1473±10K and keep it for 4s, clean it surface; at this point a clean Si(111)7×7 surface is obtained;
通过蒸发源向表面经过清洁的单晶硅基片表面沉积0.7层Au原子,在单晶硅基片表面获得(5X2+α-√3X√3)金吸附单晶硅表面结构;沉积时控制真空室气压≤1×10-7Pa,单晶硅基片温度为873±10K;Deposit 0.7 layers of Au atoms on the surface of the cleaned single crystal silicon substrate through the evaporation source, and obtain (5X2+α-√3X√3) gold adsorption single crystal silicon surface structure on the surface of the single crystal silicon substrate; vacuum is controlled during deposition Chamber pressure ≤1×10 -7 Pa, single crystal silicon substrate temperature 873±10K;
将金属In在室温下通过分子束外延室内的掩模上的狭缝窗口蒸发沉积到单晶硅基片中心位置,在单晶硅基片上获得矩形薄膜片层,矩形薄膜片层的厚度为2.0±0.2ML;掩模的窗口为长方形或狭缝式,宽度在150μm,掩模材质选用钽;在蒸发镀铟膜时,用反射式高能电子衍射装置随时监测衍射斑点花样,当出现√3×√3表面重构的衍射花样时就表明铟的覆盖度刚好为1/3ML(三分之一单原子层),并记录这个时间;根据蒸镀铟的速率和时间就能准确控制沉积铟薄膜的覆盖度大小,当蒸发速率相同,蒸发时间为覆盖度1/3ML的时间的6倍时,既得到覆盖度为2.0ML的铟膜;Metal In is evaporated and deposited on the center of the single crystal silicon substrate through the slit window on the mask in the molecular beam epitaxy chamber at room temperature, and a rectangular thin film layer is obtained on the single crystal silicon substrate. The thickness of the rectangular thin film layer is 2.0 ±0.2ML; the window of the mask is rectangular or slit, the width is 150μm, and the mask material is tantalum; when evaporating indium film, use the reflective high-energy electron diffraction device to monitor the diffraction spot pattern at any time, when √3× √3 The surface reconstructed diffraction pattern shows that the coverage of indium is just 1/3ML (one-third monoatomic layer), and this time is recorded; the deposition of indium film can be accurately controlled according to the rate and time of evaporation indium When the evaporation rate is the same and the evaporation time is 6 times that of the coverage of 1/3ML, an indium film with a coverage of 2.0ML is obtained;
沿着〈1-10〉方向对单晶硅基片上的矩形薄膜片层施加直流电场开始驱动电迁移,控制矩形薄膜片层的电迁移扩散,电流强度为0.1A,施加电流的时间为5~30min,施加电场时单晶硅基片的温度为630K,在单晶硅基片表面获得准二维金属纳米结构,由直流电场驱动的结构演变过程如图7所示。Apply a direct current electric field to the rectangular thin film layer on the single crystal silicon substrate along the <1-10> direction to start driving electromigration, control the electromigration and diffusion of the rectangular thin film layer, the current intensity is 0.1A, and the time of applying the current is 5~ After 30 minutes, the temperature of the single crystal silicon substrate was 630K when the electric field was applied, and a quasi-two-dimensional metal nanostructure was obtained on the surface of the single crystal silicon substrate. The structure evolution process driven by the DC electric field is shown in Figure 7.
实施例5Example 5
电场控制在单晶硅基片表面制备纳米结构装置同实施例1;The preparation of nanostructure devices on the surface of a single crystal silicon substrate by electric field control is the same as in Example 1;
选用镜面抛光的电阻率为50~100Ω·cm的n型Si(111)硅圆晶片,沿长边平行于〈1-10〉方向进行切割制成长方形的单晶硅基片;Choose mirror-polished n-type Si (111) silicon wafers with a resistivity of 50-100Ω·cm, and cut along the long side parallel to the <1-10> direction to make rectangular single-crystal silicon substrates;
将单晶硅基片固定于分子束外延室的真空室样品台上,在真空室压强≤2×10-8Pa条件下,将单晶硅基片加热至1473±10K并保持4s,清洁其表面;此时获得清洁的Si(111)7×7表面;Fix the single crystal silicon substrate on the vacuum chamber sample stage of the molecular beam epitaxy chamber, under the condition of the vacuum chamber pressure ≤ 2×10 -8 Pa, heat the single crystal silicon substrate to 1473±10K and keep it for 4s, clean it surface; at this point a clean Si(111)7×7 surface is obtained;
通过蒸发源向表面经过清洁的单晶硅基片表面沉积0.1层Au原子,在单晶硅基片表面获得(7×7+5×2)金吸附单晶硅表面结构;沉积时控制真空室气压≤1×10-7Pa,单晶硅基片温度为873±10K;Deposit 0.1 layer of Au atoms on the surface of the cleaned single crystal silicon substrate through the evaporation source, and obtain (7×7+5×2) gold adsorption single crystal silicon surface structure on the surface of the single crystal silicon substrate; control the vacuum chamber during deposition Air pressure ≤1×10 -7 Pa, single crystal silicon substrate temperature is 873±10K;
将金属In在室温下通过分子束外延室内的掩模上的狭缝窗口蒸发沉积到单晶硅基片中心位置,在单晶硅基片上获得矩形薄膜片层,矩形薄膜片层的厚度为2.0±0.2ML;掩模的窗口为长方形或狭缝式,宽度在200μm,掩模材质选用钽;在蒸发镀铟膜时,用反射式高能电子衍射装置随时监测衍射斑点花样,当出现√3×√3表面重构的衍射花样时就表明铟的覆盖度刚好为1/3ML(三分之一单原子层),并记录这个时间;根据蒸镀铟的速率和时间就能准确控制沉积铟薄膜的覆盖度大小,当蒸发速率相同,蒸发时间为覆盖度1/3ML的时间的6倍时,既得到覆盖度为2.0ML的铟膜;Metal In is evaporated and deposited on the center of the single crystal silicon substrate through the slit window on the mask in the molecular beam epitaxy chamber at room temperature, and a rectangular thin film layer is obtained on the single crystal silicon substrate. The thickness of the rectangular thin film layer is 2.0 ±0.2ML; the window of the mask is rectangular or slit, the width is 200μm, and the material of the mask is tantalum; when evaporating the indium film, use the reflective high-energy electron diffraction device to monitor the diffraction spot pattern at any time, when √3× √3 The surface reconstructed diffraction pattern shows that the coverage of indium is just 1/3ML (one-third monoatomic layer), and this time is recorded; the deposition of indium film can be accurately controlled according to the rate and time of evaporation indium When the evaporation rate is the same and the evaporation time is 6 times that of the coverage of 1/3ML, an indium film with a coverage of 2.0ML is obtained;
沿着〈1-10〉方向对单晶硅基片上的矩形薄膜片层施加直流电场开始驱动电迁移,控制矩形薄膜片层的电迁移扩散,电流强度为0.1~0.5A,施加电流的时间为1~60min,施加电场时单晶硅基片的温度为763K,在单晶硅基片表面获得准二维金属纳米结构。Apply a DC electric field to the rectangular thin film layer on the single crystal silicon substrate along the <1-10> direction to start driving electromigration, control the electromigration diffusion of the rectangular thin film layer, the current intensity is 0.1-0.5A, and the time for applying the current is 1-60min, when the electric field is applied, the temperature of the single crystal silicon substrate is 763K, and a quasi-two-dimensional metal nanostructure is obtained on the surface of the single crystal silicon substrate.
实施例6Example 6
电场控制在单晶硅基片表面制备纳米结构装置同实施例1;The nanostructure device prepared on the surface of a single crystal silicon substrate by electric field control is the same as that in Example 1;
选用镜面抛光的电阻率为50~100Ω·cm的n型Si(111)硅圆晶片,沿长边平行于〈1-10〉方向进行切割制成长方形的单晶硅基片;Choose mirror-polished n-type Si (111) silicon wafers with a resistivity of 50-100Ω·cm, and cut along the long side parallel to the <1-10> direction to make rectangular single-crystal silicon substrates;
将单晶硅基片固定于分子束外延室的真空室样品台上,在真空室压强≤2×10-8Pa条件下,将单晶硅基片加热至1473±10K并保持6s,清洁其表面;此时获得清洁的Si(111)7×7表面;Fix the single crystal silicon substrate on the vacuum chamber sample stage of the molecular beam epitaxy chamber, under the condition of vacuum chamber pressure ≤ 2×10 -8 Pa, heat the single crystal silicon substrate to 1473±10K and keep it for 6s, clean it surface; at this point a clean Si(111)7×7 surface is obtained;
通过蒸发源向表面经过清洁的单晶硅基片表面沉积1层Au原子,在单晶硅基片表面获得α-√3×√3金吸附单晶硅表面结构;沉积时控制真空室气压≤1×10-7Pa,单晶硅基片温度为873±10K;Deposit a layer of Au atoms on the surface of the cleaned single crystal silicon substrate through the evaporation source, and obtain an α-√3×√3 gold adsorption single crystal silicon surface structure on the surface of the single crystal silicon substrate; control the vacuum chamber pressure ≤ during deposition 1×10 -7 Pa, the temperature of single crystal silicon substrate is 873±10K;
将金属In在室温下通过分子束外延室内的掩模上的狭缝窗口蒸发沉积到单晶硅基片中心位置,在单晶硅基片上获得矩形薄膜片层,矩形薄膜片层的厚度为2.0±0.2ML;掩模的窗口为长方形或狭缝式,宽度在50μm,掩模材质选用钽;在蒸发镀铟膜时,用反射式高能电子衍射装置随时监测衍射斑点花样,当出现√3×√3表面重构的衍射花样时就表明铟的覆盖度刚好为1/3ML(三分之一单原子层),并记录这个时间;根据蒸镀铟的速率和时间就能准确控制沉积铟薄膜的覆盖度大小,当蒸发速率相同,蒸发时间为覆盖度1/3ML的时间的6倍时,既得到覆盖度为2.0ML的铟膜;Metal In is evaporated and deposited on the center of the single crystal silicon substrate through the slit window on the mask in the molecular beam epitaxy chamber at room temperature, and a rectangular thin film layer is obtained on the single crystal silicon substrate. The thickness of the rectangular thin film layer is 2.0 ±0.2ML; the window of the mask is rectangular or slit, the width is 50μm, and the mask material is tantalum; when evaporating indium film, use the reflective high-energy electron diffraction device to monitor the diffraction spot pattern at any time, when √3× √3 The surface reconstructed diffraction pattern shows that the coverage of indium is just 1/3ML (one-third monoatomic layer), and this time is recorded; the deposition of indium film can be accurately controlled according to the rate and time of evaporation indium When the evaporation rate is the same and the evaporation time is 6 times that of the coverage of 1/3ML, an indium film with a coverage of 2.0ML is obtained;
沿着〈1-10〉方向对单晶硅基片上的矩形薄膜片层施加直流电场开始驱动电迁移,控制矩形薄膜片层的电迁移扩散,电流强度为0.1~0.5A,施加电流的时间为1~60min,施加电场时单晶硅基片的温度为630K,在单晶硅基片表面获得准二维金属纳米结构。Apply a DC electric field to the rectangular thin film layer on the single crystal silicon substrate along the <1-10> direction to start driving electromigration, control the electromigration diffusion of the rectangular thin film layer, the current intensity is 0.1-0.5A, and the time for applying the current is 1-60min, when the electric field is applied, the temperature of the single crystal silicon substrate is 630K, and a quasi-two-dimensional metal nanostructure is obtained on the surface of the single crystal silicon substrate.
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