CN109879242A - A kind of stress auxiliary positioning nanoprocessing method and its nanostructure of preparation - Google Patents
A kind of stress auxiliary positioning nanoprocessing method and its nanostructure of preparation Download PDFInfo
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- CN109879242A CN109879242A CN201910190126.2A CN201910190126A CN109879242A CN 109879242 A CN109879242 A CN 109879242A CN 201910190126 A CN201910190126 A CN 201910190126A CN 109879242 A CN109879242 A CN 109879242A
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Abstract
The invention discloses a kind of stress auxiliary positioning nanoprocessing method and its nanostructure of preparation, the stress auxiliary positioning nanoprocessing method is to choose core layer material and Shell Materials formation core-shell structure, is heat-treated to the core-shell structure；The interface of the core-shell structure forms non-uniaxial tensile stress；The shape at the interface of the core-shell structure is controlled to position the position of non-uniaxial tensile stress maximum value；The non-uniaxial tensile stress directly breaks the superficial layer for the side that is stretched, and the non-uniaxial tensile stress maximum value is greater than the tensile stress fracture threshold value of the material for the side that is stretched.Alternatively, the non-uniaxial tensile stress maximum value is less than the tensile stress fracture threshold value of the material for the side that is stretched and in the same order of magnitude；The heat treatment carries out in oxidizing gas atmosphere.Accurate positioning nanoprocessing can be realized without high-precision nanoimprinting technology in stress auxiliary positioning nanoprocessing method provided by the invention, it will not be polluted in process and structural damage, high-precision positioning nanoprocessing can be carried out on the especially upright micro-nano structure of existing micro-nano structure, and have batch preparative capacibility.
Description
Technical field
The present invention relates to micro-nano structure processing technique fields, more particularly, to a kind of stress auxiliary positioning nanoprocessing
Method and its nanostructure of preparation.
Background technique
Micro-nano technology technology has been widely used in modern micro-nano electronic device, micro-nano photoelectric device, micro-nano phonon device
The processing and manufacturing of part.Wherein, high-precision positioning nanoprocessing method is the key that production novel nano device, such as ring grid field
Effect transistor, single-electronic transistor, single impurity device, nanometer thermoelectric cooler, spin electric device.
Currently, researchers have developed focused ion beam (FIB) processing, the local based on atomic force microscope (AFM) is lured
The methods of oxidation is led to realize high-precision positioning nanoprocessing.FIB is using specific in focused ion beam bombardment removal material
The atom of position realizes accurate positioning nanoprocessing；But pollution and structural damage are be easy to cause in process.Based on atom
The local induced oxidation of force microscope is by the spacing between diminution AFM probe and material surface in machined material and probe
Between form strong internal field；By providing hydrone, water bridge is formed between probe and material.It will be located at using strong electrical field
Hydrone between probe and machined material is dissociated into hydroxide ion, and hydroxide ion reacts to form oxide with material,
To realize high-precision positioning oxidation.The above-mentioned positioning nanoprocessing method based on FIB and AFM referred to, is difficult to realize
It is prepared by the batch of ordered nano-structure.In addition, traditional from upper in conjunction with electron beam exposure (EBL) and plasma reaction etching etc.
And positioning nanoprocessing also may be implemented in lower preparation process, but is difficult in the especially upright micro-nano of existing micro nano structure
High-precision positioning nanoprocessing is carried out in structure.
Therefore, it is necessary to develop a kind of new positioning nanoprocessing method.
Summary of the invention
The present invention is to overcome be easy to cause pollution and structural damage in process described in the above-mentioned prior art, be difficult to reality
The batch preparation of existing ordered nano-structure, be difficult to carry out on the especially upright micro-nano structure of existing micro-nano structure it is high-precision
The defect for positioning nanoprocessing, provides a kind of stress auxiliary positioning nanoprocessing method, the positioning nanoprocessing method provided without
It needs high-precision nanoimprinting technology that accurate positioning nanoprocessing can be realized, will not pollute in process and be damaged with structure
Wound, can carry out high-precision positioning nanoprocessing on the especially upright micro-nano structure of existing micro-nano structure, and have
Batch preparative capacibility.
Another object of the present invention is to provide nanostructures made from above-mentioned stress auxiliary positioning nanoprocessing method.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of stress auxiliary positioning nanoprocessing method, chooses core layer material and Shell Materials form core-shell structure, to institute
Core-shell structure is stated to be heat-treated；The interface of the core-shell structure forms non-uniaxial tensile stress；
The shape at the interface of the core-shell structure is controlled to position the position of non-uniaxial tensile stress maximum value；
The non-uniaxial tensile stress directly breaks the superficial layer for the side that is stretched, and the non-uniaxial tensile stress maximum value is greater than quilt
The tensile stress of the material of tensile side is broken threshold value.
Preferably, the heat treatment carries out in vacuum environment, atmosphere of inert gases or oxidizing gas atmosphere.
The present invention also protects another technical solution arranged side by side with the above method.At this point, non-uniaxial tensile stress cannot be direct
Break the superficial layer for the side that is stretched.Using the stretching action of the non-uniaxial tensile stress in nucleocapsid interface, the non-list in core-shell structure interface is improved
The thermal oxide rate of core layer material or Shell Materials at axis tensile stress maximum position realizes positioning oxidation.
A kind of stress auxiliary positioning nanoprocessing method, chooses core layer material and Shell Materials form core-shell structure, to institute
Core-shell structure is stated to be heat-treated；The interface of the core-shell structure forms non-uniaxial tensile stress；
The shape at the interface of the core-shell structure is controlled to position the position of non-uniaxial tensile stress maximum value；
The non-uniaxial tensile stress maximum value is less than the tensile stress fracture threshold value of the material for the side that is stretched and in same number
Magnitude；The heat treatment carries out in oxidizing gas atmosphere.
The principle of stress auxiliary positioning nanoprocessing method of the invention is as follows:
In core-shell structure, due to the volume of the ingredient or atom of core layer material and Shell Materials, lattice constant or
Person's thermal expansion coefficient mismatches, during forming Shell Materials or heat treatment core-shell structure, core layer material and shell material
Effect of the superficial layer of material in nucleocapsid interface by stress.
Select suitable core layer material and Shell Materials that the superficial layer of core layer material or Shell Materials can be made in nucleocapsid circle
Effect at face by non-uniaxial tensile stress.For example, the volume or lattice constant of selection ingredient, atom are greater than stratum nucleare material
The Shell Materials of material, when using plated film or heat treatment method production Shell Materials, stratum nucleare surface will be by the non-single shaft in interface
The effect of tensile stress；Similarly, ingredient, the volume of atom or lattice constant is selected to be less than the Shell Materials of core layer material,
When using plated film or heat treatment method production Shell Materials, shell layer surface is by the effect by the non-uniaxial tensile stress in interface.And
Thermal expansion coefficient is selected to be different from the Shell Materials of core layer material, during being heat-treated the lifting/lowering temperature of core-shell structure, due to core
The degrees of expansion of layer material and Shell Materials has differences, and the superficial layer of core layer material or Shell Materials will be by the non-list in interface
The effect of axis tensile stress.In addition, the non-uniaxial tensile stress in the interface is uneven in the monolayer dispersion of stratum nucleare or Shell Materials, i.e.,
At interface, there are maximum values for specific position.And the non-list in interface can be regulated and controled by controlling the shape and size of core-shell structure
Distribution of the axis tensile stress in nucleocapsid layer surface, the position of maximum non-uniaxial tensile stress and its size.
After selecting suitable core layer material and Shell Materials, positioning nanoprocessing is realized using following two mechanism:
(1) maximum value for the non-uniaxial tensile stress in interface being subject to when the superficial layer of core layer material or Shell Materials, which is greater than, is somebody's turn to do
When the tensile stress of core layer material or Shell Materials is broken threshold value, the superficial layer of the core layer material or Shell Materials will be in nucleocapsid knot
It is directly broken at the non-uniaxial tensile stress maximum position in structure interface, forms nanometer gap.At this point, if the gas that heat treatment is passed through
For oxidizing gas, then the nanostructure of smooth surface can be further formed at nanometer crack.
(2) under the action of the non-uniaxial tensile stress in interface, the lattice of core layer material or Shell Materials is stretched, to drop
Perhaps the Activation energy of Shell Materials and oxidizing gas improves the heat of core layer material or Shell Materials to the low core layer material
Oxidation rate.So heat treatment core-shell structure when be passed through oxidizing gas, when the superficial layer of core layer material or Shell Materials by
To the maximum value of the non-uniaxial tensile stress in interface be less than the tensile stress fracture threshold value of the core layer material or Shell Materials and be in
When the same order of magnitude, then it can use the stretching action of the non-uniaxial tensile stress in nucleocapsid interface, hence it is evident that it is non-to improve core-shell structure interface
The thermal oxide rate of the core layer material or Shell Materials at uniaxial tensile stress maximum position realizes positioning oxidation.
Essence can be realized without high-precision nanoimprinting technology in stress auxiliary positioning nanoprocessing method provided by the invention
True positioning nanoprocessing, will not pollute in process and structural damage, can existing micro-nano structure especially
High-precision positioning nanoprocessing is carried out on upright micro-nano structure, and has batch preparative capacibility.
The temperature of the heat treatment is lower than the fusing point of the core layer material and Shell Materials.
Preferably, the oxidizing gas in the oxidizing gas atmosphere is in vapor, ozone or nitrous oxide
A combination of one or more.
Preferably, the inert gas is the combination of one or more of nitrogen, argon gas or helium.
Preferably, the molecule of the Shell Materials, the volume of atom or lattice constant or thermal expansion coefficient with it is described
Core layer material has differences.
Preferably, the core layer material is elemental silicon, elemental Germanium, pure boron, GaAs, aluminium nitride, gallium nitride, Buddha's warrior attendant
Stone, silicon carbide, simple substance molybdenum or two-dimensional layer material.
Preferably, the two-dimensional layer material is graphene, graphene oxide, molybdenum disulfide, tungsten disulfide, black phosphorus, two
Titanium sulfide, two selenizing molybdenums, two tungsten selenides, bismuth telluride, antimony telluride or boron nitride.
Preferably, the Shell Materials of the core-shell structure are prepared using plated film or heat treatment method.
The nanostructure that the present invention protects above-mentioned stress auxiliary positioning nanoprocessing method to be prepared simultaneously.
Compared with prior art, the beneficial effects of the present invention are:
Essence can be realized without high-precision nanoimprinting technology in stress auxiliary positioning nanoprocessing method provided by the invention
True positioning nanoprocessing, will not pollute in process and structural damage, can existing micro-nano structure especially
High-precision positioning nanoprocessing is carried out on upright micro-nano structure, and has batch preparative capacibility.
Detailed description of the invention
Fig. 1 is the schematic diagram of stress auxiliary positioning nanoprocessing method of the invention.Fig. 1 (a) is to form nanometer in stratum nucleare
The schematic diagram of structure, Fig. 1 (b) are to form the schematic diagram of nanostructure in shell.
Fig. 2 is the preparation flow schematic diagram of the stress auxiliary positioning nanoprocessing method of embodiment 1.
Typical scan electron microscopic (SEM) shape appearance figure for the silicon nanostructure that the step of Fig. 3 is embodiment 1 (8) obtains.Figure
3 (a) be the typical scan electronics of the silicon nanostructure array of the ordered arrangement obtained after overstress auxiliary positioning nanoprocessing
Micro-image (SEM)；Fig. 3 (b) is that the typical case of the single silicon nanostructure obtained after overstress auxiliary positioning nanoprocessing sweeps
Retouch electron micrograph image (SEM)；Fig. 3 (c) is that the typical case of the nanostructure obtained after overstress auxiliary positioning nanoprocessing is saturating
Penetrate sem image (TEM).
Fig. 4 is the typical scan electron micrograph image (SEM) for the structure that comparative example 3 obtains.
Wherein, 1 stratum nucleare is represented, 2 represent shell, and 3 represent the nanostructure formed in stratum nucleare, what 4 representatives were formed in shell
Nanostructure；5 represent silica dot matrix exposure mask, and 6 represent silicon substrate, and 7 represent silicon cone structure, and 8 represent silica protection
Layer, 9 represent the nanostructure of diameter or width less than 100nm.
Specific embodiment
The present invention is further illustrated With reference to embodiment.
The same or similar label correspond to the same or similar components in the attached drawing of the embodiment of the present invention；It is retouched in of the invention
In stating, it is to be understood that if there is the orientation of the instructions such as term " on ", "lower", "left", "right", "top", "bottom", "inner", "outside"
Or positional relationship is to be based on the orientation or positional relationship shown in the drawings, and is merely for convenience of description of the present invention and simplification of the description, and
It is not that the device of indication or suggestion meaning or element must have a particular orientation, be constructed and operated in a specific orientation, therefore
The terms describing the positional relationship in the drawings are only for illustration, should not be understood as the limitation to this patent.
In addition, if there is the terms such as " first ", " second " to be used for description purposes only, be mainly used for distinguishing different devices,
Element or component (specific type and construction may identical may also be different), is not intended to show or implies indicated fill
It sets, the relative importance and quantity of element or component, and should not be understood as indicating or implying relative importance.
Raw material in embodiment can be by being commercially available；
Unless stated otherwise, the present invention uses reagent, method and apparatus for the art conventional reagent, method and are set
It is standby.
Embodiment 1
A kind of stress auxiliary positioning nanoprocessing method, specific preparation flow are as shown in Figure 2, comprising the following steps:
(1) as shown in Fig. 2 (i), using plasma enhanced chemical vapor deposition method, deposition thickness is about on silicon substrate 6
The silicon dioxide mask layer of 500nm；Photoresist (the negativity for being about 600nm in silica surface spin coating thickness using sol evenning machine
Photoresist, ARN-7520).Lithography system is recycled to be exposed on a photoresist.Then it is dotted photoresist to be obtained by development
Array, developer solution used in developing process are to be configured by tetramethylammonium hydroxide (TMAH) and ultrapure water according to volume ratio 4: 1
It forms；Then plasma anisotropic etching silicon dioxide is utilized, photoresist array pattern is transferred to earth silicon mask
Layer, to form silica dot matrix exposure mask 5.
(2) as shown in Fig. 2 (ii), using plasma isotropic etching silicon, silicon cone structure 7 is obtained.
(3) as shown in Fig. 2 (iii), after the preparation for completing silicon cone structure 7, retain silica dot matrix exposure mask 5.
Thermal oxide is carried out using the electric tube furnace that is rapidly heated later, forms silicon dioxide layer of protection 8 in silicon cone 7 and 6 surface of silicon substrate.
Used oxidate temperature is 1000 DEG C, and the oxygen flow being passed through is 0.9slm, oxidization time 60min.
(4) it as shown in Fig. 2 (iv), using the silicon dioxide layer of protection 8 of plasma anisotropic etched plane, stays simultaneously
Exposure mask of the silicon dioxide layer of protection 8 of lower silicon pyramid side as next step etching.
(5) as shown in Fig. 2 (v), isotropic etching is carried out to silicon using plasma, obtains silicon nanometer stratum nucleare structure,
That is stratum nucleare 1.The side of the silicon nanometer stratum nucleare structure be rotation the hyperboloid of one sheet, i.e., using at diameter minimum as reference point, silicon it is straight
Diameter is incremented by along the vertical direction；The minimum diameter of the silicon nanometer stratum nucleare structure is 160~300nm, the side at the diameter minimum
Radius of curvature is 200~600nm.
(6) as shown in Fig. 2 (vi), silicon nanometer is etched using the mixed solution (volume ratio 4: 1) of ultrapure water and hydrofluoric acid
The silica dot matrix exposure mask 5 and silicon dioxide layer of protection 8 of stratum nucleare body structure surface.
(7) as shown in Fig. 2 (vii), the silicon nanometer stratum nucleare structure of acquisition is placed in the progress heat in electric tube furnace that is rapidly heated
Oxidation；Oxidate temperature is 1000 DEG C, and the flow of be passed through oxygen is 0.9slm, and oxidization time is 240~450min, and silicon is made to receive
Rice body structure surface generates silica shell, i.e. shell 2, to form core-shell structure.Since the volume of silicon dioxide molecules is big
In the volume of silicon atom, in thermal oxidation process, effect of the silicon in silicon/silicon dioxide interface by non-uniaxial tensile stress.Interface
Non- uniaxial tensile stress is unevenly distributed in silicon face；Its maximum value is present in silicon diameter minimum, and with oxidated layer thickness
Increase and constantly increase.So non-uniaxial draw in the maximum interface being subject at silicon diameter minimum is answered by prolonged thermal oxide
The tensile stress that power is greater than silicon is broken threshold value, and silicon is caused to break to form a nanometer crack, i.e. nanostructure 3, this nanometer of gap here
Length be less than 100nm.
(8) it is heat-treated as shown in Fig. 2 (viii), continued to be passed through oxygen, then can form diameter or width is less than
The nanostructure 9 of 100nm, such as 10nm, 20nm, 30nm, 50nm, 80nm.Recycle the mixed solution of ultrapure water and hydrofluoric acid
Silicon nanostructure as shown in Figure 3 can be obtained in (volume ratio 4: 1) etching surface silica.
Embodiment 2
Experimental method is with embodiment 1, and uniquely the difference is that, silica shell is to utilize coating process system in step (7)
Standby, for example, chemical vapor deposition.
Embodiment 3
Experimental method with embodiment 2, unlike, change the silica membrane in step (7) as shell into other
Ingredient, the volume of atom or lattice constant or thermal expansion coefficient are greater than the material of silicon, for example, elemental Germanium, silicon nitride.
Embodiment 4
Experimental method with embodiment 2, unlike, change the silica membrane in step (7) as shell into other
Ingredient, the volume of atom or lattice constant or thermal expansion coefficient are less than the material of silicon, such as pure boron, finally in shell
Layer forms nanostructure.
Embodiment 5
Experimental method with embodiment 2, unlike, the silicon for forming stratum nucleare structure is substituted for elemental Germanium, pure boron, arsenic
Gallium, aluminium nitride, gallium nitride, diamond, silicon carbide, simple substance molybdenum, two-dimensional layer material such as graphene, graphene oxide, two sulphur
Change one of molybdenum, tungsten disulfide, black phosphorus, titanium disulfide, two selenizing molybdenums, two tungsten selenides, bismuth telluride, antimony telluride, boron nitride.
Embodiment 6
Experimental method with embodiment 2, unlike, change the be passed through gas of heat treatment into vacuum or vapor, smelly
One of oxygen, nitrous oxide or one of a variety of or nitrogen, argon gas, helium or a variety of.
Comparative example 1
Side the difference is that, is uniquely that bi-curved silicon nanometer stratum nucleare structure changes cylinder into embodiment 1 by experimental method
Shape silicon nanowire structure is evenly distributed so as to cause silicon face in the non-uniaxial tensile stress that nucleocapsid interface is subject to, and there is no answer
The maximum position of power finally cannot achieve positioning process and form nanostructure.
Comparative example 2
Experimental method uniquely the difference is that, only prepares silicon nanometer stratum nucleare structure and does not prepare Shell Materials, directly with embodiment 1
Capable heat treatment is tapped into, positioning process is finally cannot achieve and forms nanostructure.
Comparative example 3
Experimental method with embodiment 1, unlike, the interface that the thickness for changing silicon dioxide layer is subject to silicon core surface is non-
The order of magnitude (GPa) locating for tensile stress fracture threshold value of the uniaxial tensile stress much smaller than silicon, finally cannot achieve positioning process and is formed
Nanostructure removes surface silica dioxide, obtained structure using the mixed solution (volume ratio 4:1) of ultrapure water and hydrofluoric acid
As shown in Figure 4.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description
To make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.It is all this
Made any modifications, equivalent replacements, and improvements etc., should be included in the claims in the present invention within the spirit and principle of invention
Protection scope within.
Claims (10)
1. a kind of stress auxiliary positioning nanoprocessing method, which is characterized in that choose core layer material and Shell Materials form nucleocapsid
Structure is heat-treated the core-shell structure；The interface of the core-shell structure forms non-uniaxial tensile stress；
The shape at the interface of the core-shell structure is controlled to position the position of non-uniaxial tensile stress maximum value；
The non-uniaxial tensile stress directly breaks the superficial layer for the side that is stretched, and the non-uniaxial tensile stress maximum value, which is greater than, to be stretched
The tensile stress of the material of side is broken threshold value.
2. stress auxiliary positioning nanoprocessing method according to claim 1, which is characterized in that the heat treatment is in vacuum
It is carried out in environment, atmosphere of inert gases or oxidizing gas atmosphere.
3. stress auxiliary positioning nanoprocessing method according to claim 1, which is characterized in that the non-uniaxial tensile stress
Maximum value is less than the tensile stress fracture threshold value of the material for the side that is stretched and in the same order of magnitude；The heat treatment is in oxidisability gas
It is carried out in body atmosphere.
4. stress auxiliary positioning nanoprocessing method according to claim 2 or 3, which is characterized in that the oxidisability gas
Oxidizing gas in body atmosphere is the combination of one or more of vapor, ozone or nitrous oxide.
5. described in any item stress auxiliary positioning nanoprocessing methods according to claim 1~3, which is characterized in that the shell
The molecule of layer material, the volume of atom or lattice constant or thermal expansion coefficient have differences with the core layer material.
6. stress auxiliary positioning nanoprocessing method according to claim 5, which is characterized in that the core layer material is single
Matter silicon, elemental Germanium, pure boron, GaAs, aluminium nitride, gallium nitride, diamond, silicon carbide, simple substance molybdenum or two-dimensional layer material.
7. stress auxiliary positioning nanoprocessing method according to claim 6, which is characterized in that the two-dimensional layer material
For graphene, graphene oxide, molybdenum disulfide, tungsten disulfide, black phosphorus, titanium disulfide, two selenizing molybdenums, two tungsten selenides, bismuth telluride,
Antimony telluride or boron nitride.
8. described in any item stress auxiliary positioning nanoprocessing methods according to claim 1~3, which is characterized in that the core
The Shell Materials of shell structure are prepared using plated film or heat treatment method.
9. described in any item stress auxiliary positioning nanoprocessing methods according to claim 1~3, which is characterized in that the heat
The temperature of processing is lower than the fusing point of the core layer material and Shell Materials.
10. the nanostructure that any one of the claim 1~9 stress auxiliary positioning nanoprocessing method is prepared.
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