CN108892100A - A kind of preparation method of metal nano needle tip array - Google Patents
A kind of preparation method of metal nano needle tip array Download PDFInfo
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- CN108892100A CN108892100A CN201810660814.6A CN201810660814A CN108892100A CN 108892100 A CN108892100 A CN 108892100A CN 201810660814 A CN201810660814 A CN 201810660814A CN 108892100 A CN108892100 A CN 108892100A
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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
- B81C1/00023—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
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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
- B81C1/00349—Creating layers of material on a substrate
- B81C1/0038—Processes for creating layers of materials not provided for in groups B81C1/00357 - B81C1/00373
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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
- B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
- B81C1/00444—Surface micromachining, i.e. structuring layers on the substrate
- B81C1/0046—Surface micromachining, i.e. structuring layers on the substrate using stamping, e.g. imprinting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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Abstract
The invention discloses a kind of preparation methods of metal nano needle tip array, include the following steps：(A) it shifts in ultrathin nanometer template to a flat substrate；(B) metal of nanometer pinpoint to be prepared is placed into the ultrathin nanometer template of the flat substrate surface；(C) extruding metal of heating is formed microtrabeculae into the hole in ultrathin nanometer template and flows to be formed in flat substrate with thermoplastic nanofibers stamping technique and be bonded, be cooled into sandwich structure；(D) under external force, remove flat substrate, microtrabeculae under stretching action constriction, break to form metal nano needle tip.Beneficial effects of the present invention：Sandwich structure is formed by way of thermoplastic molding, by the physics mode of removal bonding substrates to form metal nano needle tip, prepared needle point is regular, uniform, and radius of curvature is in 5-10nm；It is formed using the ultrathin nanometer template with pore structure, the size range of microtrabeculae and needle point fluctuates small, high yield rate；Equipment requirement is low, simple process and low cost.
Description
Technical field
The present invention relates to a kind of preparation methods of metal nano needle tip array.
Background technique
Nanometer pinpoint or nanocone are aobvious in cold-cathode field launching electronics, scanning probe as a kind of special nanostructure
The fields such as micro mirror, biochemistry sensing and anti-reflection coating have a wide range of applications.
Currently used for prepare nanometer pinpoint method mainly include photoetching technique, e-beam induced deposition, laser pyrolysis and
Physical chemistry vapor deposition.Such as：China Patent Publication No. CN 106809802A, publication date are on June 9th, 2017, invention
The patent of entitled " preparation method of large-area metal nanometer pinpoint array in a kind of flexible substrate ", such technology mainly use
Silicon electronics micro-processing technology first obtains reverse pyramid silicon pores array in silicon face, then passes through deposited metal film and carries out
Chemical attack removes silicon base and metal nano needle tip array is finally made.Such technology can get uniform nanometer pinpoint, but needle
The generally very big therefore nano-scale in pointed cone angle is limited only to needle region, while its preparation process can generate largely discarded soda acid
Corrosive liquid；1051301288 A of China Patent Publication No. CN, publication date are on 2 3rd, 2016, a kind of entitled " system
102560616 A of patent and China Patent Publication No. CN of the device and method of standby metal needle point ", publication date 2012
On July 11, entitled " device for being used to prepare metal nano needle tip " patent, such method mainly utilizes wire
It is powered to corroding in the electrolytic solution and nanometer pinpoint is made, step is simple but output is low, can only once do a metal needle point；Chinese patent
Publication number CN107101988A, publication date be August in 2017 29, entitled " a kind of high density of golden film covering is received
The patent of rice pinpoint array and application ", such technology is by lithographic technique first polymer material (typical such as polystyrene)
Then middle acquisition nanometer pinpoint array passes through the metal film of physical deposition nanometer thickness on its surface to obtain metal nano needle tip battle array
Column.This method processing step is more, depends on sophisticated equipment, at high cost.Therefore it develops one kind quickly and low cost prepares metal and receives
The method of rice pinpoint array has practical significance.
Summary of the invention
In order to solve the above technical problem, the present invention provides a kind of quick and low costs to prepare metal nano needle tip array
Method.
This method is using thermoplastic nanofibers stamping technique the ultrathin nanometer mould of the extruding metal of heating to flat substrate surface
In plate, microtrabeculae is formed by the hole in ultrathin nanometer template, then flat substrate surface is adhered to by atom Diffusion Welding, in turn
Sandwich structure is formed, finally applies external force and makes microtrabeculae that constriction occur and break to form nanometer pinpoint.The present invention utilizes heating
Metal material load effect outside lower the characteristics of significant Plastic Flow can occur, by the hole progress of ultrathin nanometer template at
Type obtains uniform micro-pillar array, process and simple process, and the requirement to equipment is low.In addition, uniform micro-pillar array
So that it is regular uniformly based on the nanometer pinpoint that physical method carries out drawing preparation, meanwhile, whole preparation process is without using chemistry
Reagent is handled.
Technical solution provided by the invention is as follows.
A kind of preparation method of metal nano needle tip array, which is characterized in that include the following steps：
(A) it shifts in ultrathin nanometer template to a flat substrate；
(B) metal of nanometer pinpoint to be prepared is placed into the ultrathin nanometer template of the flat substrate surface；
(C) extruding metal of heating is formed into the hole in ultrathin nanometer template with thermoplastic nanofibers stamping technique micro-
Column simultaneously flows to formation bonding in flat substrate, is cooled into sandwich structure；
(D) under external force, remove flat substrate, microtrabeculae under stretching action constriction, break to form metal nano needle tip.
The thickness of above-mentioned ultrathin nanometer template is less than 10 microns.
The pore diameter of above-mentioned ultrathin nanometer template is less than 2 microns.
Above-mentioned ultrathin nanometer template is made via photoetching technique or the method for anodic oxidation.
The material of above-mentioned nano-form is selected from one of silicon, aluminium oxide, silica, zirconium oxide.
The fusing point of above-mentioned flat substrate should be greater than or equal to the metal fusing point.
Above-mentioned metal is selected from one of gold, silver, copper, aluminium, tin, zinc, lead or alloy at least containing more than one elements.
The adhesive strength of metal in above-mentioned inflow ultrathin nanometer template hole and flat substrate with hot pressing time increase
And increase.
Heating temperature is 0.25T in above-mentioned steps (C)m~Tm, applying pressure loading should be greater than the yield spread of coining metal
Stress.
The radius of curvature of metal nano needle tip is less than or equal to 1 micron in above-mentioned steps (D).
Beneficial effects of the present invention：
1, sandwich structure is formed by way of thermoplastic molding, by removing the physics mode of bonding substrates to be formed
Metal nano needle tip, prepared needle point is regular, uniform, and radius of curvature is in 5-10nm；
2, it is formed using the ultrathin nanometer template of pore structure, the size range of needle point fluctuates small, high yield rate；
3, equipment requirement is low, simple process and low cost.
Detailed description of the invention
Fig. 1 is the sandwich structure schematic diagram in a kind of preparation of metal nano needle tip array；
The exemplary gold nano pinpoint array for showing preparation of Fig. 2；
The exemplary silver nanoparticle pinpoint array for showing preparation of Fig. 3；
Appended drawing reference：The flat substrate of 1-, 2- ultrathin nanometer template, 3- sheet metal, 4- stack barrier layer, and 5- metal nano is visited
Needle.
Specific embodiment
Method and scheme of the invention are described further below in conjunction with specific embodiment.It should be noted that this
The content of invention is not limited to these specific embodiments, all implementation under no other inventive embodiments
Example, belongs to protection scope of the present invention.
The preparation method of metal nano needle array
Fig. 1 is the schematic diagram of sandwich structure in preparation method of the present invention.It is bottom-up to stack barrier layer 4, metal respectively
The peaceful substrate 1 of piece 3, ultrathin nanometer template 2 is to form stack system.The barrier layer 4 is heat stable material, can be to avoid metal
Piece is be bonded with loads fixture generation.The sheet metal 3 is squeezed by loading device after heating the stack system to target temperature
Pressure, which is flowed into the hole of ultrathin nanometer template 2, to be formed microtrabeculae and is bonded in after contacting with flat substrate 1 by atom Diffusion Welding
Together, sandwich structure is formed.Face external broach is applied to flat substrate 1 again, under a stretching force the metal microtrabeculae in nano die
Constriction occurs until breaking to form metal nano needle tip 5.
Embodiment 1
A kind of preparation method of gold nano pinpoint array, includes the following steps：
(1) bottom-up successively stack stainless steel substrates barrier layer, diameter is about golden thin slice, hole that 5mm thickness is about 0.3mm
Diameter be 280nm hole depth be 1200nm ultra-thin bilateral anodic oxidation aluminium formwork (referred to as ultra-thin AAO template), with a thickness of 40 μm not
The rust flat substrate of steel.
(2) lamination is integrally placed into and is heated on the flat surface fixture of universal testing machine and stablizes its temperature at 530 DEG C
(for flat surface fixture by Resistant heating, temperature can accuracy controlling.Unless otherwise specified, all embodiments be all made of this ten thousand
Energy testing machine carries out hot pressing).
(3) under 530 DEG C of constant temperature, by controlling two flat surface fixtures being placed in parallel of universal testing machine with 1mm/
The speed of min moves towards, to be further applied load to stack system, when load reaches 9kN, (corresponding mean stress is about
Try hard to keep when 500MPa) carrying 400s.
(4) it protects and is unloaded after carrying with the rate of 5kN/s, it is whole that lamination is taken out after the completion of unloading.
(5) side of lamination entirety gold substrate is fixed, a lateral edge face outside direction of the flat substrate of stainless steel is clamped with pliers
Force disengages gold substrate and the flat substrate of stainless steel.To form gold nano in gold surface and the flat substrate surface of stainless steel
Pinpoint array.
Embodiment 2
A kind of preparation method of silver nanoparticle pinpoint array, includes the following steps：
(1) bottom-up successively stack stainless steel substrates barrier layer, diameter is about silver-colored thin slice, hole that 5mm thickness is about 0.3mm
Diameter be 280nm hole depth be 1200nm ultra-thin bilateral anodic oxidation aluminium formwork (referred to as ultra-thin AAO template), with a thickness of 40 μm not
The rust flat substrate of steel.
(2) lamination is integrally placed into and is heated on the flat surface fixture of universal testing machine and stablizes its temperature at 530 DEG C.
(3) under 530 DEG C of constant temperature, by controlling two flat surface fixtures being placed in parallel of universal testing machine with 1mm/
The speed of min moves towards, to be further applied load to stack system, when load reaches 10.5kN, (corresponding mean stress is about
Try hard to keep when 500MPa) carrying 400s.
(4) it protects and is unloaded after carrying with the rate of 5kN/s, it is whole that lamination is taken out after the completion of unloading.
(5) side of lamination entirety SERS substrate is fixed, a lateral edge face outside direction of the flat substrate of stainless steel is clamped with pliers
Force disengages SERS substrate and the flat substrate of stainless steel.To form silver nanoparticle in silver-based bottom surface and the flat substrate surface of stainless steel
Pinpoint array.
Embodiment 3
Sem test
The scanning electron microscope of model Zeiss Sigma 500 is used the gold and silver nanometer pinpoint array that Examples 1 and 2 obtain
It is characterized.
Fig. 2 is the SEM characterization result of embodiment 1.Fig. 2 (a) is the SEM for the gold nano pinpoint array that amplification factor is 15k
Figure, as can be seen from the figure prepared gold nano pinpoint array is of uniform size, arranges regular, most of all to form completely
Needle point.Fig. 2 (b)-(c) is respectively partial enlargement 70k and 120k times of SEM figure, is obtained by measurement, the tip curvature half of needle point
Diameter is 5-10nm.
Fig. 3 is the SEM figure of the silver nanoparticle pinpoint array of above-mentioned preparation.Fig. 3 (a) can be seen that prepared silver nanoparticle needle point
Array sizes are uniform, arrange regular, largely form complete needle point.By gradually partial enlargement (Fig. 3 (b)-Fig. 3 (c)),
It can measure and show that the tip curvature radius of acupuncture needle point is 5-10nm.
In conclusion metal nano needle tip array sizes prepared by physical method of the present invention using sandwich structure are equal
Even, range of curvature radius 5-10nm arranges regular, can largely form the needle point of completion, high yield rate.Device requirement is low, work
Skill is simple, is easy to cost control, is a kind of preparation method of promising metal nano needle array.
The foregoing is only a preferred embodiment of the present invention, but the scope of protection of the invention be not limited thereto,
Any modification that anyone skilled in the art is made in the technical scope disclosed by the present invention, equivalent replacement and
Improve etc., it should be included within the protection scope of invention.
Claims (10)
1. a kind of preparation method of metal nano needle tip array, which is characterized in that include the following steps：
(A) it shifts in ultrathin nanometer template to a flat substrate；
(B) metal of nanometer pinpoint to be prepared is placed into the ultrathin nanometer template of the flat substrate surface；
(C) extruding metal of heating is formed microtrabeculae simultaneously into the hole in ultrathin nanometer template with thermoplastic nanofibers stamping technique
It flows to and forms bonding in flat substrate, be cooled into sandwich structure；
(D) under external force, remove flat substrate, microtrabeculae under stretching action constriction, break to form metal nano needle tip.
2. a kind of preparation method of metal nano needle tip array according to claim 1, it is characterised in that：It is described ultra-thin to receive
The thickness of rice template is less than 10 microns.
3. a kind of preparation method of metal nano needle tip array according to claim 1, it is characterised in that：It is described ultra-thin to receive
The pore diameter of rice template is less than 2 microns.
4. a kind of preparation method of metal nano needle tip array according to claim 1, it is characterised in that：It is described ultra-thin to receive
Rice template is made via photoetching technique or the method for anodic oxidation.
5. a kind of preparation method of metal nano needle tip array according to claim 1, it is characterised in that：The nanometer mould
The material of plate is selected from one of silicon, aluminium oxide, silica, zirconium oxide.
6. a kind of preparation method of metal nano needle tip array according to claim 1, it is characterised in that：The flat substrate
Fusing point should be greater than or equal to the metal fusing point.
7. a kind of preparation method of metal nano needle tip array according to claim 1, it is characterised in that：The metal choosing
From one of gold, silver, copper, aluminium, tin, zinc, lead or alloy at least containing more than one elements.
8. a kind of preparation method of metal nano needle tip array according to claim 1, it is characterised in that：Described flow into surpasses
The adhesive strength of metal and flat substrate in thin nano-form hole increases with the increase of hot pressing time.
9. a kind of preparation method of metal nano needle tip array according to claim 1, it is characterised in that：The step
(C) heating temperature is 0.25T inm~Tm, applying pressure loading should be greater than the yield spread stress of coining metal.
10. a kind of preparation method of metal nano needle tip array according to claim 1, it is characterised in that：The step
(D) radius of curvature of metal nano needle tip is less than or equal to 1 micron in.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109879242A (en) * | 2019-03-13 | 2019-06-14 | 中山大学 | A kind of stress auxiliary positioning nanoprocessing method and its nanostructure of preparation |
| CN110921614A (en) * | 2019-11-25 | 2020-03-27 | 武汉大学 | Preparation method of heterogeneous micro-nano structure |
| CN111620298A (en) * | 2020-05-28 | 2020-09-04 | 武汉大学 | Method for cutting metal nano structure, assembling nano device and characterizing nano device in situ |
| CN112479154A (en) * | 2020-11-13 | 2021-03-12 | 中南大学深圳研究院 | Preparation method of ordered metal nano needle tip array |
| CN113328325A (en) * | 2021-04-22 | 2021-08-31 | 江苏度微光学科技有限公司 | Flexible polymer random laser and preparation method thereof |
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Application publication date: 20181127 |