CN111362225A - Nano needle tip structure, composite structure and preparation method thereof - Google Patents
Nano needle tip structure, composite structure and preparation method thereof Download PDFInfo
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- CN111362225A CN111362225A CN202010189070.1A CN202010189070A CN111362225A CN 111362225 A CN111362225 A CN 111362225A CN 202010189070 A CN202010189070 A CN 202010189070A CN 111362225 A CN111362225 A CN 111362225A
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- 239000002131 composite material Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000758 substrate Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 22
- 238000005530 etching Methods 0.000 claims abstract description 20
- 239000002245 particle Substances 0.000 claims abstract description 20
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000009616 inductively coupled plasma Methods 0.000 claims abstract description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 30
- 229910052710 silicon Inorganic materials 0.000 claims description 30
- 239000010703 silicon Substances 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 229910052782 aluminium Inorganic materials 0.000 claims description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000000151 deposition Methods 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 230000001939 inductive effect Effects 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- 238000000137 annealing Methods 0.000 claims description 4
- 230000008878 coupling Effects 0.000 claims description 4
- 238000010168 coupling process Methods 0.000 claims description 4
- 238000005859 coupling reaction Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000005566 electron beam evaporation Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- 230000008021 deposition Effects 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 229920002120 photoresistant polymer Polymers 0.000 claims description 2
- 238000001020 plasma etching Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 13
- 230000001965 increasing effect Effects 0.000 abstract description 5
- 238000001069 Raman spectroscopy Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 230000031700 light absorption Effects 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 description 4
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
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- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
- B81B1/00—Devices without movable or flexible elements, e.g. microcapillary devices
- B81B1/006—Microdevices formed as a single homogeneous piece, i.e. wherein the mechanical function is obtained by the use of the device, e.g. cutters
- B81B1/008—Microtips
-
- 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
- B81C1/00023—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems without movable or flexible elements
- B81C1/00111—Tips, pillars, i.e. raised structures
-
- 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
- B81C1/00388—Etch mask forming
- B81C1/00404—Mask characterised by its size, orientation or shape
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- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Micromachines (AREA)
Abstract
A nanometer needle point structure, a composite structure and a preparation method thereof are provided, wherein the nanometer needle point structure comprises a substrate, and a plurality of nanometer needle points are formed on the surface of the substrate in an array manner; wherein the diameter of the top of each nanometer needle tip is 10-20 nm; the height of the nanometer needle tip is 200-350 nm; the distance between adjacent nanometer needle points is 62.5-125 nm, and the 'hot spot' effect is obviously increased. The preparation method of the nanometer needle point structure adopts an Anodic Aluminum Oxide (AAO) template and Inductively Coupled Plasma (ICP) etching, has low cost and simple process, and can realize large-scale preparation. The Ag particle/nanometer needle point composite structure prepared on the basis can obviously increase the surface plasma effect such as light absorption, Raman signal enhancement and the like.
Description
Technical Field
The invention relates to the field of semiconductor process, in particular to a nano needle tip structure, a composite structure and a preparation method thereof.
Background
Localized Surface Plasmon Resonance (LSPR) has attracted extensive research interest due to its wide application in the fields of surface science, environmental monitoring, biomedicine, and biosensing. Enhanced localized surface plasmon resonance can greatly enhance the local electric field strength around it, which is critical for Surface Enhanced Raman Scattering (SERS).
It is well known that the application of plasma depends mainly on the local enhancement of the electromagnetic field (also called "hot spot" effect) generated by the excitation of localized surface plasmon resonance, which is influenced by many factors such as topography, surface charge, etc. Therefore, the fabrication of various nanostructures has become a common method to enhance the localized surface plasmon resonance effect. Because the nanostructure array not only increases the roughness of the substrate, but also helps to create "hot spots" that exist between adjacent nanostructure arrays, enhancing the electromagnetic field around them. A variety of nanostructures have been prepared. The vast majority of the SERS effect is present on nanostructures with nanogaps or nanotips. By depositing noble metal particles, a "hot spot" effect is obtained by virtue of the small gaps between the nanoparticles. However, the existing nano structure with nano gaps or nano tips usually adopts the technologies of electron beam exposure, focused ion beams and the like, and has complex preparation process and high cost. The average period of the common nanostructure array is large, and the condition of generating a hot spot (the period is below 20 nm) cannot be met, which means that the enhancement effect of the nanostructure on the SERS effect is very little.
Disclosure of Invention
In view of the above, the present invention provides a nano-tip structure, a composite structure and a method for manufacturing the same, which are intended to at least partially solve at least one of the above-mentioned technical problems.
As an aspect of the present invention, there is provided a nanoprobe structure, including a substrate on which a plurality of nanoprobes are formed in an array; wherein the diameter of the top of each nanometer needle tip is 10-20 nm; the height of the nanometer needle tip is 200-350 nm; the distance between adjacent nanometer needle points is 62.5-125 nm.
As another aspect of the present invention, there is also provided a method for preparing the nanotip structure as described above, comprising the steps of:
transferring an anodized aluminum template with a nanopore array onto a substrate;
etching the substrate with the anodic aluminum oxide template by adopting an inductive coupling plasma etching method to form a nanometer needle point structure on the substrate;
and removing the residual anodic aluminum oxide template on the substrate to finish the preparation.
As still another aspect of the present invention, there is also provided an Ag particle/nano needle tip composite structure comprising:
a nanotip structure as described above;
and Ag particles are deposited on the nanometer needle point structure to form an Ag particle/nanometer needle point composite structure.
As a further aspect of the present invention, there is also provided a method for preparing the Ag particle/nano needle tip composite structure as described above, comprising the steps of:
and (3) carrying out electron beam evaporation deposition on the nano needle point structure to obtain a silver film, and annealing to form an Ag particle/nano needle point composite structure.
Based on the technical scheme, compared with the prior art, the invention has at least one or one part of the following beneficial effects:
(1) the invention provides a preparation method of a nanometer needle point structure, which combines an Anodic Aluminum Oxide (AAO) template and Inductively Coupled Plasma (ICP) etching, has low cost and simple process and can realize large-scale preparation;
(2) the invention provides a nanometer needle point structure, the diameter of the top of the nanometer needle point structure is only 10nm magnitude, and the 'hot spot' effect can be obviously increased;
(3) the invention provides a nanometer needle point structure, and the Ag particle/nanometer needle point composite structure prepared on the basis can obviously increase the surface plasma effect such as light absorption, Raman signal enhancement and the like.
Drawings
FIG. 1 is a schematic size diagram of a nanotip structure according to an embodiment of the present invention;
FIG. 2 is a flow chart of a method for fabricating a nanotip structure according to an embodiment of the present invention;
FIG. 3 is an SEM image of a nanotip structure according to an embodiment of the present invention;
fig. 4 is an SEM image of an Ag particle/nanoprobe tip composite structure according to an embodiment of the present invention.
Detailed Description
The invention utilizes an Anodic Aluminum Oxide (AAO) template and Inductively Coupled Plasma (ICP) etching to prepare the nanometer needle tip structure. The diameter of the top of the prepared nanometer pinpoint structure is only 10nm magnitude, and the hot spot effect can be greatly increased. The Ag particle/silicon needle point composite structure prepared on the basis can obviously improve the Raman signal enhancement effect.
In order that the objects, technical solutions and advantages of the present invention will become more apparent, the present invention will be further described in detail with reference to the accompanying drawings in conjunction with the following specific embodiments.
The invention provides a nanometer needle point structure, which comprises a substrate made of silicon chip materials, wherein a plurality of nanometer needle points are formed on the surface of the substrate in an array mode; wherein the diameter of the top of each nanometer needle tip is 10-20 nm; the height of the nanometer needle tip is 200-350 nm; the distance between adjacent nanometer needle points is 62.5-125 nm.
In embodiments of the present invention, a nanotip structure with a small gap is provided, especially with sharp top and edge.
In a preferred embodiment of the present invention, as shown in fig. 1, the diameter of the top of the nanoprobe tip structure is 10 nm; the height of the nanometer needle tip is 250 nm; the distance between adjacent nanometer needle points is 100 nm.
In a preferred embodiment of the present invention, the diameter of the top of the nanoprobe tip structure is only in the order of 10nm, significantly increasing the "hot spot" effect.
As another aspect of the present invention, as shown in fig. 2, there is also provided a method for preparing the above-mentioned nano tip structure, comprising the steps of:
step 1: preparing an Anodic Aluminum Oxide (AAO) template;
in other embodiments of the present invention, the preparation is not limited to the self-preparation, and a commercial anodized aluminum template may be selected, and only the appropriate aperture, hole spacing and anodized aluminum template thickness of the anodized aluminum template are selected for the nano-tip structure.
More specifically, in the embodiment of the invention, the aperture of the anodic aluminum oxide template is 72-88 nm; the distance between two adjacent holes of the anodic aluminum oxide template is 110-125 nm; the thickness of the anodized aluminum template was 300 nm.
This is because if the diameter of the anodic alumina template and the hole pitch are too large, the diameter of the top of the etched nano-needle tip is large, and an ideal nano-needle tip structure cannot be formed. On the contrary, if the aperture and the hole pitch are too small, the top of the nanometer needle tip will collapse.
When the thickness of the anodic aluminum oxide template is too large, the processing procedure after etching is complicated, the workload can be greatly increased, and if the thickness is too thin, the nano needle tip structure can not be etched to the mask with ideal depth.
Step 2: cleaning a silicon wafer; the method comprises the following specific steps: soaking the silicon wafer in H with the concentration of 95-98%2SO4And 30 to 40 wt% of H2O2Taking out the silicon wafer after 10-15 minutes from the solution mixed in the volume ratio of 4: 1, and cleaning the silicon wafer with deionized water, and then sequentially and respectively ultrasonically cleaning the silicon wafer with acetone, ethanol and deionized water for 10-15 minutes.
It is worth mentioning that step 1 and step 2 are not limited to a specific sequence.
And step 3: transferring an Anodic Aluminum Oxide (AAO) template; the method comprises the following specific steps: and carrying out hydrophilic treatment on the cleaned silicon wafer to form a pretreated silicon wafer, then placing the prepared AAO template on the pretreated silicon wafer, putting the pretreated silicon wafer into acetone to enable the AAO template to be tightly attached to the substrate, and finally fishing out and putting the pretreated silicon wafer into a drying oven to dry.
More specifically, the hydrophilic treatment comprises a vacuum plasma photoresist removing treatment on the silicon wafer; the hydrophilic treatment specifically comprises the following operations: and (3) putting the silicon wafer into a plasma degumming machine, and carrying out 3min under the condition that the oxygen power is 300W to obtain the hydrophilic substrate surface.
And 4, step 4: etching a silicon wafer with an anodic aluminum oxide template by Inductive Coupled Plasma (ICP) to form a nanometer needle point structure on the surface of the silicon wafer; the method comprises the following specific steps: placing the silicon wafer transferred by the AAO template into ICP etching equipment under the conditions that the air pressure is 15mT, the temperature of an upper electrode and a lower electrode is 25 ℃, the power of an inductive coupling plasma coil is 1000W, and the power of the lower electrode is 20W; by C4F8And SF6Is an etching gas, wherein C4F8And SF6The volume ratio of (1.5-1.76) to 1, the total flow rate of the etching gas is 125-138 sccm, and the etching time is 120-150 s.
In the preferred embodiment of the present invention, the etching time is selected to be 135 s.
And 5: removing redundant AAO; the method comprises the following specific steps: and (3) putting the etched silicon wafer into a phosphoric acid solution with the mass fraction of 5-10%, putting the silicon wafer into water bath at 60 ℃ for 30-60 minutes, taking out the silicon wafer, cleaning the silicon wafer with deionized water, and blow-drying the silicon wafer with a nitrogen gun to obtain the nano needle tip structure.
In the preferred embodiment of the invention, the etched silicon wafer is put into a phosphoric acid solution with the mass fraction of 5%, is put into water bath at 60 ℃ for 30 minutes, is taken out, is cleaned by deionized water, and is dried by a nitrogen gun to obtain the nanometer pinpoint structure.
As still another aspect of the present invention, there is also provided an Ag particle/nano needle tip composite structure comprising:
a nanotip structure as described above;
and Ag particles are deposited on the nanometer needle point structure to form an Ag particle/nanometer needle point composite structure.
As a further aspect of the present invention, there is also provided a method for preparing the Ag particle/nano needle tip composite structure as described above, comprising the steps of:
and (3) carrying out electron beam evaporation deposition on the nano needle point structure to obtain a silver film, and annealing to form an Ag particle/nano needle point composite structure.
Example 1
The preparation method of the nanometer needle tip structure shown in fig. 2 is adopted, wherein the aperture of the anodic alumina template is 80nm, the distance between the apertures is 125nm, and the thickness of the AAO template is 300 nm; placing the silicon wafer transferred by the AAO template into ICP etching equipment, and adopting C4F8And SF6Etching gas is used for etching, and the etching time is 135 s; putting the etched silicon wafer into a phosphoric acid solution with the mass fraction of 5%, putting the silicon wafer into water bath at 60 ℃ for 30 minutes, taking out the silicon wafer, cleaning the silicon wafer with deionized water, and drying the silicon wafer with a nitrogen gun to obtain a nano needle point structure shown in figure 3, wherein the diameter of the top of the nano needle point is 10 nm; the height of the nanometer needle tip is 250 nm; the distance between adjacent nanometer needle points is 100 nm.
And depositing a silver film on the nano needle point structure shown in the figure 3 by electron beam evaporation, and annealing to form the Ag particle/nano needle point composite structure shown in the figure 4.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A nanometer needle point structure comprises a substrate, and is characterized in that a plurality of nanometer needle points are formed on the surface of the substrate in an array mode; wherein the diameter of the top of each nanometer needle tip is 10-20 nm; the height of the nanometer needle tip is 200-350 nm; the distance between adjacent nanometer needle points is 62.5-125 nm.
2. The nanotip structure of claim 1, wherein the nanotip has a top diameter of 10 nm; the height of the nanometer needle tip is 250 nm; the distance between adjacent nanometer needle points is 100 nm.
3. The nanotip structure of claim 1, wherein said substrate is a silicon wafer.
4. A method of fabricating a nanotip structure according to any one of claims 1 to 3, comprising the steps of:
transferring an anodized aluminum template with a nanopore array onto a substrate;
etching the substrate with the anodic aluminum oxide template by adopting an inductive coupling plasma etching method to form a nanometer needle point structure on the substrate;
and removing the residual anodic aluminum oxide template on the substrate to finish the preparation.
5. The method of fabricating a nanotip structure according to claim 4, wherein the step of transferring said anodized aluminum template onto a substrate comprises:
carrying out hydrophilic treatment on the substrate to form a pretreated substrate;
placing the anodic aluminum oxide template on the pretreated substrate, tightly attaching the anodic aluminum oxide template in acetone, and drying to finish transfer;
wherein the hydrophilic treatment comprises a vacuum plasma photoresist stripping treatment of the substrate;
wherein the hydrophilic treatment specifically comprises the following operations: putting the substrate into a plasma degumming machine, and carrying out 3min under the condition that the oxygen power is 300W to obtain the hydrophilic substrate surface;
wherein the aperture of the anodic aluminum oxide template is 72-88 nm; the distance between two adjacent holes of the anodic aluminum oxide template is 110-125 nm; the thickness of the anodic aluminum oxide template is 300 nm.
6. The method for preparing the nano needle tip structure according to claim 4, wherein the specific conditions of the inductively coupled plasma etching method are as follows: the air pressure is 15mT, the temperature of the upper electrode and the lower electrode is 25 ℃, the power of the inductive coupling plasma coil is 1000W, and the power of the lower electrode is 20W;
the etching gas comprises C4F8And SF6，C4F8And SF6The volume ratio of (1.5-1.76) to 1; the total flow of the etching gas is 125-138 sccm; the etching time is 120-150 s.
7. The method for preparing a nanotip structure according to claim 4, wherein the step of removing the remaining anodized aluminum template comprises: and (3) placing the substrate with the residual anodized aluminum template in a phosphoric acid solution with the mass fraction of 5-10%, soaking for 30-60 minutes at 60 ℃, taking out, cleaning with deionized water, and drying.
8. The method for preparing a nanotip structure according to claim 4, further comprising a step of cleaning the substrate prior to the step of transferring the anodized aluminum template onto the substrate, in particular comprising: soaking the substrate in a cleaning solution for 10-15 minutes; sequentially washing the substrate with deionized water, acetone, ethanol and deionized water for 10-15 minutes respectively;
wherein the cleaning solution comprises 95-98% H mixed in a volume ratio of 4: 12SO4And 30 to 40 wt% of H2O2。
9. An Ag particle/nanoprobe tip composite structure, comprising:
the nanotip structure of any one of claims 1 to 3;
and Ag particles are deposited on the nanometer needle point structure to form an Ag particle/nanometer needle point composite structure.
10. A method for preparing an Ag particle/nano needle tip composite structure according to claim 9, comprising the steps of:
and (3) carrying out electron beam evaporation deposition on the nano needle point structure to obtain a silver film, and annealing to form an Ag particle/nano needle point composite structure.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114231928A (en) * | 2021-12-22 | 2022-03-25 | 杭州电子科技大学 | Preparation method of annular stepped nanostructure |
| CN115029384A (en) * | 2022-04-13 | 2022-09-09 | 王烨 | Anodic aluminum oxide biochip, preparation method thereof, intracellular delivery system and use method |
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| CN110556453A (en) * | 2018-05-30 | 2019-12-10 | 中国科学院苏州纳米技术与纳米仿生研究所 | Controllable epitaxial growth method of ordered Si-based Al 1-x Ga x N quantum dots |
| CN109786537A (en) * | 2018-12-27 | 2019-05-21 | 华中科技大学鄂州工业技术研究院 | Full-inorganic LED encapsulation structure and preparation method thereof |
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| CN114231928A (en) * | 2021-12-22 | 2022-03-25 | 杭州电子科技大学 | Preparation method of annular stepped nanostructure |
| CN114231928B (en) * | 2021-12-22 | 2023-12-29 | 杭州电子科技大学 | Preparation method of annular stepped nano structure |
| CN115029384A (en) * | 2022-04-13 | 2022-09-09 | 王烨 | Anodic aluminum oxide biochip, preparation method thereof, intracellular delivery system and use method |
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