CN111362225B - Nano needle point structure, composite structure and preparation method thereof - Google Patents
Nano needle point structure, composite structure and preparation method thereof Download PDFInfo
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- CN111362225B CN111362225B CN202010189070.1A CN202010189070A CN111362225B CN 111362225 B CN111362225 B CN 111362225B CN 202010189070 A CN202010189070 A CN 202010189070A CN 111362225 B CN111362225 B CN 111362225B
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- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000758 substrate Substances 0.000 claims abstract description 47
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000005530 etching Methods 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 19
- 238000009616 inductively coupled plasma Methods 0.000 claims abstract description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 27
- 229910052710 silicon Inorganic materials 0.000 claims description 27
- 239000010703 silicon Substances 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000004140 cleaning Methods 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 9
- 229910018503 SF6 Inorganic materials 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 claims description 7
- 229960000909 sulfur hexafluoride Drugs 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 229920002120 photoresistant polymer Polymers 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- 238000000151 deposition Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- 238000000137 annealing Methods 0.000 claims description 4
- 238000005566 electron beam evaporation Methods 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims 2
- 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
- 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
- 239000011148 porous material Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 4
- 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
- 230000005672 electromagnetic field Effects 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000003491 array Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000861 blow drying Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Classifications
-
- 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
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 top diameter of each nanometer needle point is 10-20 nm; the height of the nanometer needle point 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 nano needle point structure adopts 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/nanoneedle tip composite structure prepared on the basis can obviously increase surface plasmon effects such as light absorption, raman signal enhancement and the like.
Description
Technical Field
The invention relates to the field of semiconductor process processing, in particular to a nano needle point 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, biomedical and biosensing, etc. Enhanced localized surface plasmon resonance can greatly enhance the local electric field strength around it, which is critical to Surface Enhanced Raman Scattering (SERS).
It is well known that the application of plasma is mainly dependent on local enhancement of the electromagnetic field generated by localized surface plasmon resonance excitation (also known as the "hot spot" effect), which excitation and modulation is affected by a number of factors such as topography, surface charge, etc. Thus, fabrication of various nanostructures has become a common method of enhancing localized surface plasmon resonance effects. 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. Various nanostructures have been prepared. Most SERS effects exist on nanostructures with nanogaps or nanotips. By depositing noble metal particles, a "hot spot" effect is obtained by means of small gaps between the nanoparticles. However, the existing nano-structure with nano-gaps or nano-tips usually adopts electron beam exposure, focused ion beam and other technologies, and has the disadvantages of complex preparation process and high cost. The average period of the common nanostructure array is larger, 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 nanoneedle tip structure, a composite structure and a method for preparing the same, so as to at least partially solve at least one of the above-mentioned technical problems.
As one aspect of the present invention, there is provided a nanoneedle tip structure including a substrate on the surface of which a plurality of nanoneedle tips are formed in an array; wherein the top diameter of each nanometer needle point is 10-20 nm; the height of the nanometer needle point 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 nanoneedle tip structure as described above, comprising the steps of:
transferring an anodic aluminum oxide template having a nanopore array onto a substrate;
etching a substrate with an anodic aluminum oxide template by adopting an inductively coupled plasma etching method, and forming a nano 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/nanoneedle tip composite structure comprising:
a nanoneedle tip structure as described above;
and Ag particles are deposited on the nano needle point structure to form an Ag particle/nano needle point composite structure.
As still another aspect of the present invention, there is also provided a method for preparing the Ag particle/nanoneedle tip composite structure as described above, comprising the steps of:
and (3) depositing a silver film on the nano needle point structure by electron beam evaporation, and annealing to form the Ag particle/nano needle point composite structure.
Based on the technical scheme, compared with the prior art, the invention has at least one or a part of the following beneficial effects:
(1) The invention provides a preparation method of a nano needle point structure, which combines Anodic Aluminum Oxide (AAO) templates and Inductively Coupled Plasma (ICP) etching, has low cost and simple process, and can realize large-scale preparation;
(2) The invention provides a nano needle point structure, wherein the diameter of the top of the nano needle point structure is only 10nm, and the hot spot effect can be obviously increased;
(3) The invention provides a nano needle point structure, and the Ag particle/nano needle point composite structure prepared on the basis can obviously increase surface plasma effects such as light absorption, raman signal enhancement and the like.
Drawings
FIG. 1 is a schematic dimensional view of a nanotip structure according to an embodiment of the invention;
FIG. 2 is a flow chart of a method for fabricating a nanotip structure according to an embodiment of the invention;
FIG. 3 is an SEM image of a nanotip structure according to an embodiment of the invention;
fig. 4 is an SEM image of an Ag particle/nanotip composite structure according to an embodiment of the invention.
Detailed Description
The invention prepares the nano needle point structure by utilizing Anodic Aluminum Oxide (AAO) template and Inductively Coupled Plasma (ICP) etching. The diameter of the top of the prepared nano needle point structure is only 10nm, and the hot spot effect can be greatly increased. The Ag particle/silicon needle tip composite structure prepared on the basis obviously increases the Raman signal enhancement effect.
The present invention will be further described in detail below with reference to specific embodiments and with reference to the accompanying drawings, in order to make the objects, technical solutions and advantages of the present invention more apparent.
As one aspect of the present invention, there is provided a nanoneedle tip structure comprising a substrate made of a silicon wafer, and a plurality of nanoneedle tips formed in an array on a surface of the substrate; wherein the top diameter of each nanometer needle point is 10-20 nm; the height of the nanometer needle point 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, particularly where the top and edges are relatively sharp.
In a preferred embodiment of the present invention, as shown in fig. 1, the top diameter of the nanotip structure is 10nm; the height of the nanometer needle point is 250nm; the spacing between adjacent nanotips is 100nm.
In the preferred embodiment of the present invention, the diameter of the top of the nanotip structure is only on 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 nanoneedle tip structure, including the steps of:
step 1: preparing an Anodic Aluminum Oxide (AAO) template;
in other embodiments of the present invention, the present invention is not limited to self-preparation, but can also be used with commercial anodized aluminum templates, and only the pore diameter, the pore spacing and the thickness of the anodized aluminum templates need to be selected appropriately for the above-mentioned nanotip structure.
More specifically, in embodiments of the present invention, the pore size of the anodized aluminum template is 72-88 nm; the spacing between two adjacent holes of the anodic aluminum oxide template is 110-125 nm; the thickness of the anodized aluminum template was 300nm.
This is because if the pore diameter and the pore pitch of the anodized aluminum template are too large, the diameter of the top of the etched nanotip is large, and an ideal nanotip structure cannot be formed. Otherwise, if the aperture and the hole spacing are too small, the top of the nanoneedle point can 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 when the thickness is too thin, the nano needle point structure is etched without etching to an ideal depth mask.
Step 2: cleaning a silicon wafer; the method comprises the following specific steps: soaking silicon wafer in H with concentration of 95-98% 2 SO 4 And 30 to 40wt% H 2 O 2 And (3) in the mixed solution in the volume ratio of 4:1, taking out the silicon wafer after 10 to 15 minutes, cleaning the silicon wafer by deionized water, and then respectively cleaning the silicon wafer by acetone, ethanol and deionized water in an ultrasonic mode for 10 to 15 minutes.
It should be noted that, the steps 1 and 2 are not specifically limited in sequence.
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, placing the pretreated silicon wafer into acetone to enable the AAO template to be tightly attached to a substrate, and finally taking out the silicon wafer and placing the silicon wafer into a drying oven for airing.
More specifically, the hydrophilic treatment comprises vacuum plasma photoresist removing treatment on the silicon wafer; the specific hydrophilic treatment operation comprises the following steps: and (3) placing the silicon wafer into a plasma photoresist remover, and performing 3min under the condition that the oxygen power is 300W to obtain the hydrophilic substrate surface.
Step 4: etching a silicon wafer with an anodic aluminum oxide template through Inductively Coupled Plasma (ICP), and forming a nano 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, and 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 inductively coupled plasma coil is 1000W, and the power of the lower electrode is 20W; by C 4 F 8 And SF (sulfur hexafluoride) 6 Is an etching gas, wherein C 4 F 8 And SF (sulfur hexafluoride) 6 The volume ratio of (1.5-1.76) to 1, the total flow of etching gas is 125-138 sccm, and the etching time is 120-150 s.
In a preferred embodiment of the invention, the etching time is chosen to be 135s.
Step 5: removing redundant AAO; the method comprises the following specific steps: and (3) placing the etched silicon wafer into a phosphoric acid solution with the mass fraction of 5-10%, placing the silicon wafer into a water bath at 60 ℃ for 30-60 minutes, taking out the silicon wafer, cleaning the silicon wafer with deionized water, and drying the silicon wafer by a nitrogen gun to obtain the nano needle point structure.
In the preferred embodiment of the invention, the etched silicon wafer is put into phosphoric acid solution with the mass fraction of 5%, and is put into water bath at 60 ℃ for 30 minutes, then is taken out, is cleaned by deionized water, and is dried by a nitrogen gun, thus obtaining the nano needle point structure.
As still another aspect of the present invention, there is also provided an Ag particle/nanoneedle tip composite structure comprising:
a nanoneedle tip structure as described above;
ag particles are deposited on the nano needle point structure to form an Ag particle/nano needle point composite structure.
As still another aspect of the present invention, there is also provided a method for preparing the Ag particle/nanoneedle tip composite structure as described above, comprising the steps of:
and (3) depositing a silver film on the nano needle point structure by electron beam evaporation, and annealing to form the Ag particle/nano needle point composite structure.
Example 1
The preparation method of the nano needle point structure shown in the figure 2 is adopted, wherein the aperture of the anodic aluminum oxide template is 80nm, the interval between the apertures is 125nm, and the thickness of the AAO template is 300nm; placing the silicon wafer transferred by the AAO template into ICP etching equipment, and adopting C 4 F 8 And SF (sulfur hexafluoride) 6 The etching time is 135s for etching gas; placing the etched silicon wafer into 5% phosphoric acid solution, placing in water bath at 60deg.C for 30 min, taking out, cleaning with deionized water, and blow-drying with nitrogen gun to obtain nanometer needle point structure shown in figure 3, wherein the top of nanometer needle point is provided with a nanometer needle point structureThe diameter is 10nm; the height of the nanometer needle point is 250nm; the spacing between adjacent nanotips is 100nm.
And (3) depositing a silver film on the nano needle point structure shown in fig. 3 by electron beam evaporation, and annealing to form the Ag particle/nano needle point composite structure shown in fig. 4.
The foregoing description of the embodiments has been provided for the purpose of illustrating the general principles of the invention, and is not meant to limit the invention thereto, but to limit the invention thereto, and any modifications, equivalents, improvements and equivalents thereof may be made without departing from the spirit and principles of the invention.
Claims (4)
1. The preparation method of the nano needle point structure is characterized by comprising the following steps:
transferring an anodic aluminum oxide template having a nanopore array onto a substrate;
etching a substrate with an anodic aluminum oxide template by adopting an inductively coupled plasma etching method, and forming a nano needle point structure on the substrate;
removing the residual anodic aluminum oxide template on the substrate to finish the preparation;
wherein the specific steps of transferring the anodized aluminum template to a substrate include: 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;
the hydrophilic treatment comprises vacuum plasma photoresist removing treatment on the substrate, and the specific operation comprises the following steps: placing the substrate into a plasma photoresist remover, and performing for 3min under the condition that the oxygen power is 300W to obtain the hydrophilic substrate surface;
the aperture of the anodic aluminum oxide template is 72-88 nm; the spacing between two adjacent holes of the anodic aluminum oxide template is 110-125 nm; the thickness of the anodic aluminum oxide template is 300nm;
the specific steps for removing the residual anodic aluminum oxide template on the substrate comprise: placing the substrate with the residual anodic aluminum oxide template into a phosphoric acid solution with the mass fraction of 5-10%, soaking for 30-60 minutes at 60 ℃, taking out, washing with deionized water, and drying;
before the step of transferring the anodized aluminum template onto the substrate, the method further comprises the step of cleaning the substrate, and specifically comprises the following steps: soaking the substrate in a cleaning solution for 10-15 minutes; respectively cleaning with deionized water, acetone, ethanol and deionized water for 10-15 minutes; wherein the cleaning solution comprises H with the concentration of 95-98% mixed in the volume ratio of 4:1 2 SO 4 And 30 to 40wt% H 2 O 2 ；
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 inductively coupled plasma coil is 1000W, and the power of the lower electrode is 20W; the etching gas includes C 4 F 8 And SF (sulfur hexafluoride) 6 ，C 4 F 8 And SF (sulfur hexafluoride) 6 The volume ratio of (1.5-1.76): 1, a step of; the total flow of the etching gas is 125-138 sccm; etching time is 120-150 s;
forming a plurality of nanometer needle points on the surface of the substrate in an array manner; wherein the top diameter of each nanometer needle point is 10-20 nm; the height of the nanometer needle point is 200-350 nm; the distance between adjacent nanometer needle points is 62.5-125 nm.
2. The method of claim 1, wherein the nanotip has a top diameter of 10nm; the height of the nanometer needle point is 250nm; the distance between the adjacent nanometer needle points is 100nm.
3. The method of manufacturing according to claim 1, wherein the substrate is a silicon wafer.
4. The preparation method of the Ag particle/nanoneedle point composite structure is characterized by comprising the following steps of:
transferring an anodic aluminum oxide template having a nanopore array onto a substrate;
etching a substrate with an anodic aluminum oxide template by adopting an inductively coupled plasma etching method, and forming a nano needle point structure on the substrate;
removing the residual anodic aluminum oxide template on the substrate to finish the preparation;
wherein the specific steps of transferring the anodized aluminum template to a substrate include:
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;
hydrophilic treatment comprises vacuum plasma photoresist removing treatment on the substrate, and the specific operation comprises the following steps: placing the substrate into a plasma photoresist remover, and performing for 3min under the condition that the oxygen power is 300W to obtain the hydrophilic substrate surface;
the aperture of the anodic aluminum oxide template is 72-88 nm; the spacing between two adjacent holes of the anodic aluminum oxide template is 110-125 nm; the thickness of the anodic aluminum oxide template is 300nm;
the specific steps for removing the residual anodic aluminum oxide template on the substrate comprise: placing the substrate with the residual anodic aluminum oxide template into a phosphoric acid solution with the mass fraction of 5-10%, soaking for 30-60 minutes at 60 ℃, taking out, washing with deionized water, and drying;
before the step of transferring the anodized aluminum template onto the substrate, the method further comprises the step of cleaning the substrate, and specifically comprises the following steps: soaking the substrate in a cleaning solution for 10-15 minutes; respectively cleaning with deionized water, acetone, ethanol and deionized water for 10-15 minutes; wherein the cleaning solution comprises H with the concentration of 95-98% mixed in the volume ratio of 4:1 2 SO 4 And 30 to 40wt% H 2 O 2 ；
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 ℃, and inductively coupled plasma is generatedThe coil power is 1000W, and the lower electrode power is 20W; the etching gas includes C 4 F 8 And SF (sulfur hexafluoride) 6 ，C 4 F 8 And SF (sulfur hexafluoride) 6 The volume ratio of (1.5-1.76): 1, a step of; the total flow of the etching gas is 125-138 sccm; etching time is 120-150 s;
forming a plurality of nanometer needle points on the surface of the substrate in an array manner; wherein the top diameter of each nanometer needle point is 10-20 nm; the height of the nanometer needle point is 200-350 nm; the distance between adjacent nanometer needle points is 62.5-125 nm;
depositing a silver film on the nano needle point structure by electron beam evaporation, and annealing to form an Ag particle/nano needle point composite structure;
wherein Ag particles are deposited on the nano needle point structure to form the Ag particle/nano needle point composite structure.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5399238A (en) * | 1991-11-07 | 1995-03-21 | Microelectronics And Computer Technology Corporation | Method of making field emission tips using physical vapor deposition of random nuclei as etch mask |
| JP2002079499A (en) * | 2000-09-08 | 2002-03-19 | Terumo Corp | Method of manufacturing needle-like article, and manufactured needle |
| JP2012246216A (en) * | 2011-05-25 | 2012-12-13 | Agency For Science Technology & Research | Method for forming nanostructure on substrate and use of the same |
| CN103086321A (en) * | 2013-01-25 | 2013-05-08 | 中国科学院上海微***与信息技术研究所 | Method for manufacturing monocrystalline silicon nano-long needle point on (111) type silicon chip |
| CN103674924A (en) * | 2012-09-13 | 2014-03-26 | 福州高意光学有限公司 | Raman spectrum test probe and manufacturing method thereof |
| CN108374153A (en) * | 2018-01-17 | 2018-08-07 | 南京大学 | A kind of Grown by Magnetron Sputtering large area, the method for high-sequential nano particle |
| WO2018172285A1 (en) * | 2017-03-20 | 2018-09-27 | Universite Catholique De Louvain | Method for producing improved optoelectronic surface on a semiconductor substrate |
| 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 |
| 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 |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6960528B2 (en) * | 2002-09-20 | 2005-11-01 | Academia Sinica | Method of forming a nanotip array in a substrate by forming masks on portions of the substrate and etching the unmasked portions |
| US20100193768A1 (en) * | 2005-06-20 | 2010-08-05 | Illuminex Corporation | Semiconducting nanowire arrays for photovoltaic applications |
| WO2012015443A1 (en) * | 2010-07-30 | 2012-02-02 | Hewlett-Packard Development Company, L.P. | Optical fiber surface enhanced raman spectroscopy (sers) probe |
-
2020
- 2020-03-17 CN CN202010189070.1A patent/CN111362225B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5399238A (en) * | 1991-11-07 | 1995-03-21 | Microelectronics And Computer Technology Corporation | Method of making field emission tips using physical vapor deposition of random nuclei as etch mask |
| JP2002079499A (en) * | 2000-09-08 | 2002-03-19 | Terumo Corp | Method of manufacturing needle-like article, and manufactured needle |
| JP2012246216A (en) * | 2011-05-25 | 2012-12-13 | Agency For Science Technology & Research | Method for forming nanostructure on substrate and use of the same |
| CN103674924A (en) * | 2012-09-13 | 2014-03-26 | 福州高意光学有限公司 | Raman spectrum test probe and manufacturing method thereof |
| CN103086321A (en) * | 2013-01-25 | 2013-05-08 | 中国科学院上海微***与信息技术研究所 | Method for manufacturing monocrystalline silicon nano-long needle point on (111) type silicon chip |
| WO2018172285A1 (en) * | 2017-03-20 | 2018-09-27 | Universite Catholique De Louvain | Method for producing improved optoelectronic surface on a semiconductor substrate |
| CN108374153A (en) * | 2018-01-17 | 2018-08-07 | 南京大学 | A kind of Grown by Magnetron Sputtering large area, the method for high-sequential nano particle |
| 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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