WO2013131586A1 - Structures nano-sculptées tridimensionnelles de matériaux à haute mobilité d'atomes en surface et leur procédé de fabrication - Google Patents

Structures nano-sculptées tridimensionnelles de matériaux à haute mobilité d'atomes en surface et leur procédé de fabrication Download PDF

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Publication number
WO2013131586A1
WO2013131586A1 PCT/EP2012/056341 EP2012056341W WO2013131586A1 WO 2013131586 A1 WO2013131586 A1 WO 2013131586A1 EP 2012056341 W EP2012056341 W EP 2012056341W WO 2013131586 A1 WO2013131586 A1 WO 2013131586A1
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Prior art keywords
nano
structures
thermal conductive
layer
conductive material
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PCT/EP2012/056341
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English (en)
Inventor
Vojislav Krstic
Jose Manuel Caridad Hernandez
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The Provost, Fellows, Foundation Scholars, And Other Members Of Board, Of The College Of The Holy And Undivided Trinity Of Queen Elizabeth, Near Dublin
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Application filed by The Provost, Fellows, Foundation Scholars, And Other Members Of Board, Of The College Of The Holy And Undivided Trinity Of Queen Elizabeth, Near Dublin filed Critical The Provost, Fellows, Foundation Scholars, And Other Members Of Board, Of The College Of The Holy And Undivided Trinity Of Queen Elizabeth, Near Dublin
Priority to PCT/EP2012/056341 priority Critical patent/WO2013131586A1/fr
Publication of WO2013131586A1 publication Critical patent/WO2013131586A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
    • B81C1/00206—Processes for functionalising a surface, e.g. provide the surface with specific mechanical, chemical or biological properties

Definitions

  • the invention relates to a method for growing materials .
  • the invention relates to a method for growing nanoscaled three-dimensional sculptured structures made of high surface-atom mobility materials, and devices comprising such structures .
  • Three-dimensional (3D) sculptured nano-structures can be designed and tailored by methods such as Physical Vapour Deposition (PVD) of materials, Chemical Vapour Deposition (CVD) and Plasma Enhanced CVD (PECVD) , and the like.
  • PVD Physical Vapour Deposition
  • CVD Chemical Vapour Deposition
  • PECVD Plasma Enhanced CVD
  • the method in which the growth-process temperature is compatible with existing integrated circuit technology is PVD, for example using Glancing Angle Deposition (GLAD) .
  • GLAD Glancing Angle Deposition
  • Some metals such as nickel (Ni) or copper (Cu) are not easy to engineer on the nano-scale due to their high surface-atom mobility, which is often manifested in agglomeration and deformity of the nano-structures .
  • Elias et al An example of this is presented by Elias et al .
  • US 2010/295635 merely describes an idea of how to make a tuneable resonant THz resonator using a metal-semiconductor interface having a depletion layer and a chiral structure .
  • the document postulates that the resonator may be produced by the GLAD method.
  • the GLAD method by itself does not produce regular, well- defined and well-separated 3D nano-sculptured structures made from high surface-atom mobility materials on the nanoscale .
  • US 2005/006754 describes a method for fabricating an LED diode on a heat-sink with microchannels to avoid heating up of the device while it is performing.
  • the method is based on thin-film technology and the heat-sink layer is composed of carbon nanotubes which are grown by a CVD process.
  • the synthesis temperatures are high (750°C to 950°C), which are not suitable for current integrated circuit technology.
  • only devices made from stacked (thin-film like) layers can be grown on top of the nanotube heat-sink layer as the carbon nanotubes sink has a considerably and randomly distributed surface roughness. Therefore, regular, well-defined and well-separated GLAD 3D nano-sculptured structures from high surface-atom diffusion material cannot be fabricated with this carbon nanotube heat-sink .
  • the substrate used in US 2007/051970 must be electrically insulating to provide a device having a good performance.
  • the chemical growth technique does not allow for full structural control of potentially chemically synthesised carbon-based helices.
  • a method of growing 3D sculptured nano-structures of high surface-atom mobility material on a substrate comprising the steps of:
  • the method may further comprise the step of depositing a layer of readily- soluble low thermal conductive material on the layer of high thermal conductive material.
  • the deposition of a readily-soluble, low thermal conductive layer is advantageous in that where it is not desired to have nano- structures grown on the high thermal conductive material; the nano-structures are grown on the readily-soluble low thermal conductive layer .
  • the removal of the low thermal conductive layer after growth of the 3D sculptured nano- structures also removes the unwanted nano-structures .
  • the low thermal conductive layer allows a more efficient heat management and a deliberate positioning of the structures on the substrate.
  • the present invention provides a method of growing 3D sculptured nano-structures of high surface-atom mobility material on a substrate comprising the steps of:
  • the layer of high thermal conductive material has a thermal conductance measurement of ⁇ > 10 Wm ⁇ KT 1 and the layer of readily-soluble low thermal conductive material has a thermal conductance measurement of ⁇ ⁇ 1 Wm ⁇ KT 1 .
  • the term “layer of high thermal conductive material” may be used interchangeably with the term “first layer of thermal conductive material”.
  • layer of readily-soluble low thermal conductive material may be used interchangeably with the term “second layer of readily-soluble thermal conductive material” .
  • the present invention provides a method of growing 3D sculptured nano-structures of high surface-atom mobility material on a substrate comprising the steps of:
  • the first layer of thermal conductive material has a thermal conductance measurement of ⁇ > 10 Wm ⁇ KT 1 and the second layer of readily-soluble thermal conductive material has a thermal conductance measurement of ⁇ ⁇ 1 Wm ⁇ KT 1 .
  • the present invention provides a method for growing regularly shaped and spaced apart 3D sculptured nano- structures on a substrate, while maintaining a low and constant temperature along the structures during the growth phase.
  • the method employs the use of both high thermal conductive metals and low thermal conductive materials to ensure that the temperature of the sculpted nano-structures is maintained at a low and constant level during growth.
  • the combination of both layers allow the creation of arrays of regular shaped, free-standing, 3D sculptured nano- structures made from metals and high surface-atom mobility materials.
  • the combination of layers, and in particular the high thermal conductive material selected acts as a thermal management system. The heat generated during the deposition or growth stage of the process is dissipated through the high thermal conductive material and into the substrate.
  • the substrate acts as a heat sink or an equilibrator , maintaining the temperature at a low and constant level during growth.
  • the thermal management takes away the thermal energy from the growth area so that more control of the atoms is obtained to allow for better sculpting of the nano-structures .
  • the method may further comprise the step of controlling the deposition of said layer of high thermal conductive material .
  • the step of controlling provides a plurality of spaced apart dots of high thermal conductive material on top of said layer of high thermal conductive material forming said pre-patterned substrate, or a plurality of spaced apart dots of arbitrary material on the substrate and on top of these dots and substrate, a layer of high thermal conductive material forming said pre-patterned substrate .
  • the method may comprise the use of objects other than dots, such as any kind of spheres (spherical particles), pillars or cubes for the step of controlling the deposition.
  • the high thermal conductive material may be selected from the group of high thermal conductive metals (e.g. silver, gold, copper) and other non-metallic and molecular high thermal conductive materials such as diamond, graphene and related materials having a thermal conductance of ⁇ > 10 Wm ⁇ KT 1 .
  • high thermal conductive metals e.g. silver, gold, copper
  • other non-metallic and molecular high thermal conductive materials such as diamond, graphene and related materials having a thermal conductance of ⁇ > 10 Wm ⁇ KT 1 .
  • the layer of low thermal conductive material may be selected from the group of lithographical resist with a thermal conductance of K ⁇ 1 Wm ⁇ KT 1 , such as poly (methyl methacrylate) .
  • the method may further comprise a step of removing the layer of low thermal conductive material .
  • the step of removing the layer of low thermal conductive material may be performed by dipping the substrate in a solvent selected from the group consisting of acetone or any other commercially available solvent used for lithography resist.
  • the dots may have a height of between about lOnm to about lOOnm, preferably between about 20nm and about 80nm, and ideally about 50nm.
  • the dots may have a diameter of between about lOnm to about lOOnm, preferably between about 30nm and about 80nm, and ideally about 50nm.
  • the dot-array may have a pitch of between about 5ym to about lOnm, preferably between about 500nm and about 50nm, and ideally about 150nm.
  • said 3D nano- sculptured structures may be grown substantially vertical direction to said substrate .
  • said 3D sculptured nano-structures may be grown without any additional external cooling or heating.
  • the 3D sculptured nano-structures may be grown at ambient temperature .
  • said nano- structures may have the form of a coil, a chevron, and vertical and slanted rods .
  • the substrate may comprise silicon and any types of dielectrics such as Si0 2 , MgO, Si 3 N 4 , or AlTiC
  • a device comprising sculptured nano-structures grown according to the method of the present invention.
  • the device is selected from the group comprising sensors, high efficiency energy harvesting devices, magnetic storage devices, nano- bit magnetic recording, chiral materials for electronic and optical applications, chiral sensors, photonic crystals, meta-material applications, micro- and nano- electromechanical systems, and micro- and nano- electrochemical systems .
  • An example of such devices may be nano-inductors .
  • a surface suitable for growing 3D sculptured nano- structures may comprise a substrate; a pre- or post-patterned layer of high thermal conductive material; and a layer of low thermal conductive material applied onto the layer of high thermal conductive material .
  • the combination of a high thermal conductive layer overlaying the substrate and a readily soluble low thermal conductive layer on top of the high thermal conductive layer produces an efficient and rapid heat transfer from the desired nano-structures to the substrate and a thermal shield from areas of undesired growth of sculptured nano- structures.
  • the rapid heat transfer allows the structures to grow with a constant temperature along the structures .
  • the presence of the high and low thermally conductive layers and the rapid heat transfer to the substrate enables the creation of arrays of regularly shaped 3D sculptured nano-structures made from metals and high surface mobility materials which can be deliberately positioned on desired areas of the substrate.
  • a system adapted for growing 3D sculptured nano ⁇ structures may comprise a rotating substrate holder; at least one motor and at least one electronic circuit adapted to provide arbitrary rotational speeds, and a tilted angle control, characterised in that the motor is a continuous direct current motor which provides a continuous and smooth substrate rotation essential for growing 3D sculptured nanostructures of high-quality.
  • the substrate holder may be tilted at a desired angle during the deposition process.
  • the system is adapted to be portable. In one embodiment, the system is further adapted to be retrofitted to any existing general purpose evaporator.
  • ambient temperature should be understood to mean a temperature of between minus 20°C (-4°F) and 50°C (122°F) .
  • arbitrary rotational speeds should be understood to mean a speed set by the person skilled in the art for depositing 3D sculptured nano-structures .
  • chevron should be understood to mean a pattern having a "V” or an inverted “V” shape forming a zigzag pattern.
  • high electrical conductivity should be understood to mean an electrical conductance measurement of ⁇ > 1 ⁇ 1
  • the term "high thermal conductive” should be understood to mean a thermal conductance measurement of ⁇ > 10 Wm ⁇ KT 1 .
  • the term "low thermal conductive” should be understood to mean a thermal conductance measurement of ⁇ ⁇ 1 Wm ⁇ KT 1 .
  • Figure 2 illustrates a schematic diagram explaining a method of growing nano-structures of the present invention, where (a) illustrates growth of an equally spaced array of a plurality of dots, (b) illustrates deposition of a thin layer of a high thermal conductivity material, (c) illustrates covering the substrate areas with low thermal conductive material (e.g. poly(methyl methacrylate ) (PMMA) ) where growth of nano-structures is not desirous, (d) illustrates growth of the desired nano-structures on the plurality of dots and undesired structures on poly (methyl methacrylate), and (e) illustrates removal of the covering with nano-structures thereon to reveal the desired nano-structures;
  • PMMA poly(methyl methacrylate )
  • Figure 3 illustrates a scanning electron microscope (SEM) of samples grown using the methods of the prior art which form agglomerated nano-structures having irregular shapes and defining a porous thin film as the structures are touching each other;
  • Figure 4 illustrates a scanning electron microscope (SEM) of samples of nano-structures grown using the method as illustrated in Figure 2;
  • Figure 5 illustrates a comparison between (left) a nickel thin layer produced by PVD on a S1O 2 substrate and (right) an array of nickel nano-coils (black area) produced by the method of the present invention on a Si0 2 substrate;
  • Figure 6 illustrates a system design of one embodiment the present invention where (a) is a font view showing the rotating substrate holder inserted into an evaporator; (b) is a rear view showing two motors and electronic circuits; and (c) a side view showing the titling angle control; and
  • Figure 7 illustrates (a) a graph representing the steady state operation of the motor illustrated in Figure 6 (b) ; and (b) a circuit which accomplishes a low potential drop converted into rotational motion ( Vb) and high current ( I) for creating high-quality 3D nano-structures .
  • the invention involves growing 3D sculptured nano- structures of high surface-atom diffusion materials on a layer consisting of a high thermal conductivity material (e.g. silver (Ag) ) acting as a fast heat transport material and heat sink in combination with a readily-soluble, low thermal conductive thin layer of poly (methyl methacrylate ) (PMMA) acting as a heat and matter shield covering the substrate areas where no structures are desired.
  • a high thermal conductivity material e.g. silver (Ag)
  • PMMA methyl methacrylate
  • the choice of materials for 3D sculptured nano-structures using PVD/GLAD remains a limiting factor.
  • Some metals such as Ni or Cu
  • GLAD Glancing Angle Deposition
  • Figure 1 One means of depositing the incoming atoms is by Glancing Angle Deposition (GLAD), as illustrated in Figure 1.
  • GLAD is a physical vapour deposition process that is well-known in the art. In this process, the substrate is normally oriented at an angle of tilt ⁇ with respect to the vapour source.
  • the design of the nano-structures can be tailored by controlling the deposition rate r and controlling the motion of the substrate which is achieved by modifying the rotation speed ⁇ and the tilted angle ⁇ .
  • Figure 2 there is illustrated in a schematic diagram a method of the present invention demonstrating how regular 3D sculptured nano-structures of high surface diffusion materials and metals can be created on desired places of arbitrary substrates. The method consists of the following steps:
  • dots 2 are made from a high thermal conductive metal (e.g. Ag) on an area where the nano-structures will be placed ( Figure 2a) . Dots 2 are the starting point from where the nano-structures will grow.
  • a high thermal conductive metal e.g. Ag
  • a thin layer ( ⁇ 50nm) of a high thermal conductive material (e.g. Ag) 3 is deposited on the substrate 4 and covering the spaced array of dots 2 ( Figure 2b) without burying it, that is, preserving the relief introduced by the dot array on the substrate.
  • This layer 3 acts as a fast heat-transport material from the growing structures to the substrate.
  • the layer of high thermal conductive material 3 acts as a thermal management system, transporting heat created during the deposition process away from the structures and dissipating heat into the substrate.
  • a low thermal conductive and readily-soluble material 5 such as PMMA.
  • This layer 5 allows the removal of unwanted nano-structures 6 from regions of the substrate 4 where the growth of nano-structures is not desired.
  • This layer of PMMA 5 also minimises heat transfer from the incoming flux of metal atoms to the substrate 4 in those undesired regions. Thus, these regions do not contribute to heating the substrate 4 and do not increase the temperature of the nanostructures during their growth.
  • the PMMA thin layer 5 is created by coating, spinning and baking liquid PMMA-solution on the substrate 4. Although initially the PMMA layer 5 covers the equally spaced array of dots 2, it is removed by EBL exposure to expose the dots 2 ( Figure 2c) .
  • the nano-structures 7 can be engineered to a desired shape, for example a coil, a chevron (zigzag), or slanted structure, or rods, by rotating the substrate at speed ⁇ , through an angle of tilt ⁇ with respect to the vapour source or maintaining the substrate 4 in one position.
  • a desired shape for example a coil, a chevron (zigzag), or slanted structure, or rods
  • Figure 3 is a SEM micrograph showing samples of Ni nano- structures grown without Ag and PMMA layers (but with the Ag spaced-apart dot pattern) .
  • the nano-structures are agglomerated and the shape is very irregular.
  • the substrate does not prevent the rapid heating of the structures during their growth due to the incoming flux of high-energetic Ni atoms . Consequently, the temperature of the nano-structures will be increasing considerably during the deposition and their shape will begin to deteriorate rapidly. Rather than an array of isolated helices, this picture shows a porous thin film, with the structures touching each other.
  • the nano- structures manifest themselves as an agglomeration with severe structural deformities.
  • Figure 4 is a SEM micrograph showing samples of Ni nano- structures grown on a substrate with both a high thermal conductive Ag layer (including an array of spaced-apart Ag dots) and a low thermal conductive PMMA layer.
  • the Ni nano-structures are highly regularly shaped and spaced apart so that they do not touch each other. This is unlike those nano-structures presented in Figure 3.
  • it is possible to achieve regularly shaped and spaced apart 3D sculptured nano-structures from high surface-atom mobility materials grown on any substrate.
  • the regular shapes and spaced apart sculptured 3D structures are achieved due to the presence of the low and the high thermal conductive layers .
  • the high thermal conductive layer is a plurality of spaced apart dots of Ag overlaid with a further layer of Ag .
  • the substrate only receives heat from the area where the desired structures grow (this area is small in comparison with the substrate and thin film volume), which maintains the structures during the growth phase with a low and constant temperature along the sculptured structures .
  • None of the prior art methods provide structures with low and constant temperatures along the sculptured nano-structures during the growth phase.
  • the PMMA layer also allows the elimination of the nanostructures deposited on undesired areas of the substrate. Furthermore, the deposition of the high surface mobile materials is carried out without any additional external cooling or heating at ambient temperature.
  • the prior art PVD methods of growing 3D sculptured nano-structures of high surface-atom diffusion (mobility) metals causes agglomeration and deformity in the nano-structures .
  • the growth temperature of the prior art PVD methods are strongly increasing during growth.
  • the advantages of the method of the present invention is that heat transfer from the structures to the substrate is favoured by inserting a thin layer of a high conductive material between the nano-structures and the substrate.
  • the high conductive material acts as a fast heat transport material and as a heat-sink during the deposition, providing a thermal management system.
  • the combination of a high thermal conductive layer and a readily-soluble low thermal conductive layer produce a fast heat transfer from the desired nano-structures to the substrate, which maintains a low and constant temperature along the nano-structures during growth. Both layers allow the creation of arrays of regular shaped 3D sculptured nano-structures made from high surface mobility materials which can be deliberately positioned on desired areas of the substrate.
  • FIG. 6 there is illustrated a controlled substrate motion system 10 which can be placed inside a general purpose evaporator for growing the nano- sculptured structures of the present invention.
  • the system provided by the present invention is portable, low cost and can be retro-fitted to any existing evaporator.
  • the system consists of an electronically controlled direct current (DC) motor 11,12 fixed on mechanical pieces 14 which are mounted on a wafer holder 16 provided by the evaporator (see Figure 6(a) -(c)) .
  • DC direct current
  • the available dedicated GLAD deposition systems use stepper motors, which provide rough, non-uniform rotation at low rotational speeds . Uniform, continuous rotation at low rotational speed is an essential requirement to grow nano- structures such as coils with a non-disrupted, smooth surface.
  • the present invention utilises DC motors 11,12 ( Figure 6(b)) rather than stepper motors.
  • DC motors provide a continuous and smooth substrate rotation required to grow structures at the nano scale with non-disruptive, smooth surface.
  • the substrate rotation speed provided by the DC motor 11,12 is controlled by an analog electronic circuit 18,19 ( Figure 6(b) and Figure 7) . Applying a voltage Vm to the DC motor produces a torque k, resulting in rotational motion. As the motor torque is proportional to the applied current I, the steady state operation of the motor is described by
  • Vb represents the potential drop converted into rotational motion.
  • the substrate holder may also be tilted at a desired angle during the deposition process.
  • the adjustable tilted platform 20 is illustrated in Figure 6 (c) .
  • FIG. 7 (b) A circuit which accomplishes these requirements (low Vb and high I) is illustrated in Figure 7 (b) .
  • the voltage supplied by the source Vs is stabilised and reduced through Zener diodes Zl, Z2 and resistances R1,R2.
  • Transistor Tl is connected in common collector configuration to amplify the current at the output .
  • Potentiometer RP1 allows the fine tuning of the voltage applied to the motor Vm.
  • This simple electronic circuit provides a smooth and stable rotational speed required to create high-quality sculptured 3D nano-structures .
  • the system can be readily manufactured at low cost and can be retrofitted in a general purpose evaporator. Furthermore, the system is fully portable as it does not need an external power supply when fitted to an evaporator. The system is powered by an internal battery. Therefore, the evaporator does not require any modifications to encompass the system.

Abstract

L'invention concerne un procédé pour faire croître des structures nano-sculptées tridimensionnelles de matériaux à haute mobilité d'atomes en surface sur un substrat arbitraire, le procédé comprenant les étapes qui consistent à : déposer des couches de matériaux à haute et faible conductivité thermique et à faire croître les nanostructures sur celles-ci ; tout en maintenant une température faible et constante le long de la structure pendant la croissance des nano-structures 3D.
PCT/EP2012/056341 2012-04-05 2012-04-05 Structures nano-sculptées tridimensionnelles de matériaux à haute mobilité d'atomes en surface et leur procédé de fabrication WO2013131586A1 (fr)

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Cited By (2)

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CN108659536A (zh) * 2018-03-23 2018-10-16 昆山德睿懿嘉电子材料科技有限公司 导热材料及其制备方法
CN110133876A (zh) * 2019-06-18 2019-08-16 南开大学 一种焦距可调的太赫兹石墨烯超表面透镜及设计方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108659536A (zh) * 2018-03-23 2018-10-16 昆山德睿懿嘉电子材料科技有限公司 导热材料及其制备方法
CN110133876A (zh) * 2019-06-18 2019-08-16 南开大学 一种焦距可调的太赫兹石墨烯超表面透镜及设计方法

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