CN112520690B - Method and device for metal-assisted chemical etching of discrete silicon nanopore patterns - Google Patents
Method and device for metal-assisted chemical etching of discrete silicon nanopore patterns Download PDFInfo
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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
- B81C1/00087—Holes
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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
- B81C1/00523—Etching material
- B81C1/00547—Etching processes not provided for in groups B81C1/00531 - B81C1/00539
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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
- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
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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
Abstract
The invention relates to a method for chemically etching discrete silicon nano-hole patterns by metal assistance, which comprises the following steps: cleaning a receptor substrate and a donor substrate; step two, spin-coating a polydimethylsiloxane layer on the surface of the donor substrate; step three, spin-coating a metal nanoparticle solution on the polydimethylsiloxane layer; moving the target metal nano particles to be below the laser focus under the condition that the laser beam is closed, and moving the target deposition position of the receptor substrate to be above the laser beam focus; and fifthly, irradiating the metal nano particles by focusing laser beams. The method can transfer single nanometer metal particles to the silicon substrate and has higher positioning precision.
Description
Technical Field
The invention relates to the technical field of metal-assisted chemical etching processing, in particular to a method and a device for metal-assisted chemical etching of discrete silicon nanopore patterns.
Background
With the development of the metal-assisted chemical etching silicon nanostructure technology, the silicon nanostructure manufactured by the method has made great progress in the application of the fields of solar energy conversion, heat energy conversion, energy storage, biochemical sensors, bionic super-hydrophobicity and the like. In particular, the silicon nanopore has important application prospect in the technical field of DNA sequencing. The metal auxiliary chemical etching technology has extremely high processing precision, and can manufacture nano-scale silicon nanowires and nano-scale silicon pores on a silicon substrate; in addition, the zigzag or zigzag silicon nanowire can be manufactured by changing the etchant for etching for multiple times and changing the components of the etchant, so that more and more scholars and scientists are invested in the research of the metal-assisted chemical etching technology. At present, the research on the aspect of metal-assisted chemical etching of silicon nano-array structures is mature, but the research on the aspect of etching silicon nano-structures with controllable discrete patterns has many challenges, such as difficult deposition of metal particles with discrete patterns, poor controllability and the like. Therefore, it is necessary to propose a new method for depositing discrete pattern metal nanoparticles on the surface of a silicon substrate to achieve metal-assisted chemical etching of silicon nanostructures with discrete pattern.
At present, in the metal-assisted chemical etching process, the deposition method of the metal nanoparticles mainly includes thermal evaporation, sputtering, electron beam evaporation, electroless deposition, electrode deposition, focused ion beam-assisted deposition, or spin-coating particles by other methods. Among them, due to vacuum physical type deposition methods such as thermal evaporation, sputtering and electron beam evaporation, the morphology of the resulting noble metal film is more easily controlled, and a patterned metal particle arrangement can be obtained on a silicon substrate. However, the patterned metal nanoparticles obtained by these methods are closely arranged and cannot be discretely distributed; and the controllability of the deposition position is poor. In addition, chinese patent CN106006546A proposes a method for transferring and controlling a nanostructure, which can be applied to metal deposition of metal-assisted chemical etching to help construct various two-dimensional, three-dimensional and even heterogeneous structures, but the method transfers a deposited non-discrete pattern nanostructure, and still does not solve direct deposition of discrete patterns; in addition, chinese patent CN106430084B proposes a single micro-nano structure transfer device and a transfer method thereof, in the invention, a micro-nano structure transfer substrate with a periodic raised platform and coordinate marks is used in cooperation with a microscope to observe in real time and operate a micro-nano manipulator in situ, so as to realize precise fixed-point transfer of a single micro-nano structure, and the device can realize deposition of metal particles of discrete patterns, but the transfer positioning precision is 1 micron, and the device is complex, has higher cost and has higher difficulty in realization.
Therefore, it is necessary to provide a new method, which can achieve higher positioning accuracy, lower cost and easy implementation while depositing metal nanoparticles with discrete patterns onto a silicon substrate in a metal-assisted chemical etching process.
Disclosure of Invention
The invention aims to provide a method and a device for metal-assisted chemical etching of discrete silicon nanopore patterns, which have high positioning accuracy and are easy to realize, aiming at the defects in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for metal-assisted chemical etching of discrete silicon nanopore patterns comprises the following steps:
cleaning a receptor substrate and a donor substrate;
step two, spin-coating a polydimethylsiloxane layer on the surface of the donor substrate, and naturally curing;
step three, diluting the metal nano particle solution, spin-coating the metal nano particle solution on the polydimethylsiloxane layer, and naturally drying the polydimethylsiloxane layer;
moving the target metal nano particles to be below the laser focus under the condition that the laser beam is closed, and simultaneously moving the target deposition position of the receptor substrate to be above the laser beam focus;
irradiating the metal nanoparticles by focused laser beams to release the metal nanoparticles from the donor substrate and transfer the metal nanoparticles to the receptor substrate;
moving the next target metal nano particle to be transferred to a position below the laser focus, simultaneously moving the receptor substrate to a position where the next target is to be deposited, and repeating the fifth step;
and step seven, repeating the step six, and finally depositing the metal nanoparticles with the discrete pattern on the receptor substrate.
In a further description, in the first step, a glass cover glass is selected as a donor substrate and a silicon wafer is selected as an acceptor substrate, and the surfaces of the glass cover glass and the silicon wafer are respectively ultrasonically cleaned by absolute ethyl alcohol and deionized water and dried by nitrogen.
Further, in the second step, the PDMS curing mixture is dropped on the donor substrate in the first step by using a pipette, spin-coated uniformly by using a spin coater, and the donor substrate is removed and naturally cured in a dry and clean environment to obtain a soft and thin polydimethylsiloxane layer.
In a further description, in the third step, the diluted metal nanoparticle dispersion liquid is taken out by using a pipette and dropped on the polydimethylsiloxane layer of the donor substrate in the third step, and after spin-coating by using a spin coater, the donor substrate is taken off and naturally dried.
In the fourth step, the target deposition positions of the target metal nanoparticles and the receptor substrate are moved to the laser focus through the imaging condition of the CCD imaging system in the optical system on the computer display and the computer-aided control of the nano positioning platform, and the laser beam focus is adjusted to further move the target metal nanoparticles below the focus and the receptor substrate target deposition positions above the laser beam focus.
In a further description, in the fifth step, the operating wavelength of the continuous wave laser is selected to be 1064 nm, and the power is 100mW/μm 2.
The device using the method for chemically etching the discrete silicon nano-hole pattern by metal assistance comprises a computer, an acceptor nano-positioning platform, a donor nano-positioning platform and an optical system; the computer is connected with the receptor nano positioning platform, the donor nano positioning platform and the optical system through a communication network; the donor-type solar cell comprises an acceptor nanometer positioning platform, a donor nanometer positioning platform and an optical system, wherein the acceptor nanometer positioning platform is provided with an acceptor substrate, the donor nanometer positioning platform is provided with a donor substrate, the acceptor substrate and one side of the donor substrate, which is coated with raw materials, are arranged oppositely, and the optical system irradiates one side of the donor substrate, which is not coated with raw materials.
Further, the optical system includes a continuous wave laser, a flexible focusing lens group, a liquid crystal optical shutter, a quarter wave plate, a dichroic mirror, an oil immersion objective lens, a condenser lens, a tube lens, a beam splitter, a bulb, a first CCD imaging system and a second CCD imaging system; the continuous wave laser, the flexible focusing lens group, the liquid crystal optical shutter, the quarter-wave plate, the dichroic mirror and the oil immersion objective form a first light path; the tube lens and the beam splitter form a second light path;
the flexible focusing lens group, the liquid crystal optical shutter and the quarter wave plate are sequentially arranged in front of the continuous wave laser; the oil immersion objective lens and the bulb are arranged on one side of the donor substrate; the dichroic mirror is arranged at the intersection point of the oil immersion objective and the light path of the continuous wave laser; the tube lens and the beam splitter are arranged in front of the first CCD imaging system and the second CCD imaging system.
The invention has the beneficial effects that: the method can transfer single nano-scale metal particles to the silicon substrate, has higher positioning precision, realizes the arrangement of the metal nanoparticles with discrete patterns on the silicon substrate, but has lower cost and easy realization; the silicon substrate with the discrete pattern metal nano particles is etched by a metal-assisted chemical etching method, so that the discrete pattern silicon nano pore structure is etched on the silicon substrate, and the method has deep application significance in the technical field of DNA sequencing based on nano pores.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 is a schematic view of a receptor substrate and a donor substrate of one embodiment of the present invention;
FIG. 2 is a schematic illustration of a donor substrate coated with a polydimethylsiloxane layer according to one embodiment of the present invention;
FIG. 3 is a schematic illustration of a donor substrate coated with metal nanoparticles according to one embodiment of the present invention;
FIG. 4 is a schematic diagram of the overall structure of one embodiment of the present invention;
FIG. 5 is a schematic diagram of the operation of one embodiment of the present invention;
FIG. 6 is a schematic diagram of a finished product produced in accordance with one embodiment of the present invention.
Wherein: 101. a receptor substrate; 102. a donor substrate; 201. a polydimethylsiloxane layer; 301. a metal nanoparticle; 401. a receptor substrate nanopositioning platform; 402. a donor substrate nanopositioning platform; 403. a condenser lens; 404. a bulb; 405. an oil immersion objective lens; 406. a dichroic mirror; 407. a tube lens; 408. a continuous wave laser; 409. a flexible focusing lens group; 410. a liquid crystal optical shutter; 411. a quarter wave plate; 412. a beam splitter; 413. a donor substrate CCD imaging system; 414. receptor-based CCD imaging tin systems; 415. imaging the donor substrate surface; 416. imaging the surface of the receiver substrate.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
As shown in fig. 1-6, a method for metal-assisted chemical etching of discrete silicon nanopore patterns is characterized by comprising the following steps:
cleaning a receptor substrate and a donor substrate;
step two, spin-coating a polydimethylsiloxane layer on the surface of the donor substrate, and naturally curing;
step three, diluting the metal nano particle solution, spin-coating the metal nano particle solution on the polydimethylsiloxane layer, and naturally drying the polydimethylsiloxane layer;
moving the target metal nano particles to be below the laser focus under the condition that the laser beam is closed, and simultaneously moving the target deposition position of the receptor substrate to be above the laser beam focus;
irradiating the metal nanoparticles by focused laser beams to release the metal nanoparticles from the donor substrate and transfer the metal nanoparticles to the receptor substrate;
moving the next target metal nano particle to be transferred to a position below the laser focus, simultaneously moving the receptor substrate to a position where the next target is to be deposited, and repeating the fifth step;
and step seven, repeating the step six, and finally depositing the metal nanoparticles with the discrete pattern on the receptor substrate.
And heating the metal nanoparticles on the donor substrate by adopting a laser thermal effect method, so that the donor substrate is heated and expanded, and the metal nanoparticles are pushed to the receptor substrate. Firstly, a diluted metal nano particle solution is coated on a donor substrate (a Polydimethylsiloxane (PDMS) layer on a glass cover glass) in a spinning mode, and metal nano particles are deposited on the donor substrate through natural drying and attached to the donor substrate through van der Waals attractive force; a continuous wave laser (operating at 1064 nm wavelength) and an oil immersion objective are used to focus the laser beam, and when the metal nanoparticles are irradiated by the focused laser beam, they absorb the laser energy and heat the donor substrate underneath, which causes rapid thermal expansion of the donor substrate. During the early stages of deformation of the donor substrate, the metal nanoparticles move with the expanded substrate. The velocity of the metal nanoparticles continues to rise as the expansion rate of the donor substrate increases before reaching the steady state temperature. Eventually, the rate of thermal expansion of the substrate and the velocity of the nanoparticles peaks. Then, the thermal expansion rate of the donor substrate starts to decrease, but the metal nanoparticles tend to move upward at a constant speed due to inertia. Since the laser is focused several hundred nanometers above the metal nanoparticles, the optical axial force on the metal nanoparticles first goes up, helping the metal nanoparticles to release, and then changes direction down. The air resistance on the metal nanoparticles always opposes the motion of the metal nanoparticles, slowing the metal nanoparticles. When the metal nanoparticles approach the acceptor substrate, van der waals forces between the metal nanoparticles and the acceptor substrate become large. Thus, the metal nanoparticles are attracted to the receptor substrate and eventually deposited thereon. The temperature of the donor substrate drops after the metal nanoparticles are released from the donor substrate, eventually returning to their normal state due to their high elasticity.
In a further description, in the first step, a glass cover glass is selected as a donor substrate and a silicon wafer is selected as an acceptor substrate, and the surfaces of the glass cover glass and the silicon wafer are respectively ultrasonically cleaned by absolute ethyl alcohol and deionized water and dried by nitrogen.
Because the metal-assisted chemical etching is directed to semiconductor materials, particularly monocrystalline silicon, the application provides for the metal-assisted chemical etching, and therefore, the receptor substrate adopts a silicon wafer
Further, in the second step, the PDMS curing mixture is dropped on the donor substrate in the first step by using a pipette, spin-coated uniformly by using a spin coater, and the donor substrate is removed and naturally cured in a dry and clean environment to obtain a soft and thin polydimethylsiloxane layer.
Specifically, the consumption of the PDMS curing mixing agent is 2ml, the PDMS curing mixing agent is uniformly coated in a spinning mode, and the thickness is controlled within 1 micron; controlling the metal nanoparticles within 50 nm; the reason is that the forces generated by the thermal expansion of PDMS are limited and the probability of uncontrollable motion of the oversized metal particles is increased.
In a further description, in the third step, the diluted metal nanoparticle dispersion liquid is taken out by using a pipette and dropped on the polydimethylsiloxane layer of the donor substrate in the third step, and after spin-coating by using a spin coater, the donor substrate is taken off and naturally dried.
And in the fourth step, the target metal nano particles and the target deposition position of the receptor substrate are moved to a laser focus through the imaging condition of a CCD imaging system in the optical system on a computer display and a computer-aided control nano positioning platform, and the laser focus is adjusted to further move the target metal nano particles below the focus and the target deposition position of the receptor substrate above the laser focus.
By means of a CCD imaging system, the metal nano particles of the donor are transferred to the receptor through accurate positioning, and fixed-point transfer of the metal nano particles is achieved.
In a further description, in the fifth step, the operating wavelength of the continuous wave laser is selected to be 1064 nm, and the power is 100mW/μm 2.
A 1064 nm laser is the best value for the overall system operation.
The device using the method for chemically etching the discrete silicon nano-hole pattern by metal assistance comprises a computer, an acceptor nano-positioning platform 401, a donor nano-positioning platform 402 and an optical system; the computer is connected with the receptor nano positioning platform 401, the donor nano positioning platform 402 and the optical system through a communication network; the receptor nano positioning platform 401 is provided with a receptor substrate 101, the donor nano positioning platform 402 is provided with a donor substrate 102, the receptor substrate 101 and the donor substrate 102 are oppositely arranged on the side coated with raw materials, and the optical system irradiates the side of the donor substrate 102 not coated with raw materials. The donor substrate 102 is coated with a polydimethylsiloxane layer 201, and the polydimethylsiloxane layer 201 is spin coated with metal nanoparticles 301.
To be further explained, the optical system comprises a continuous wave laser 408, a flexible focusing lens group 409, a liquid crystal optical shutter 410, a quarter wave plate 411, a dichroic mirror 406, an oil immersion objective 405, a condenser lens 403, a tube lens 407, a beam splitter 412, a bulb 404, a first CCD imaging system 413 and a second CCD imaging system 414; the continuous wave laser 408, the flexible focusing lens group 409, the liquid crystal optical shutter 410, the quarter-wave plate 411, the dichroic mirror 406 and the oil immersion objective 405 form a first optical path; the tube lens 407 and the beam splitter 412 form a second optical path;
the flexible focusing lens group 409, the liquid crystal optical shutter 410 and the quarter wave plate 411 are sequentially arranged in front of the continuous wave laser 408; the oil immersion objective 405 and the bulb 404 are disposed on one side of the donor substrate 102; the dichroic mirror 406 is arranged at the intersection point of the optical paths of the oil immersion objective 405 and the continuous wave laser 408; the tube lens 407 and the beam splitter 412 are arranged before the first CCD imaging system 413 and the second CCD imaging 414 system.
The optical system is carried on the nanometer positioning platform, the control process is observed through the first CCD imaging system 413 and the second CCD imaging system 414, and the operation is repeated to achieve the patterning deposition of the discrete metal nanoparticles 301. In an optical system, a continuous wave laser 408 emits laser, and the laser is finally focused above target metal nanoparticles 301 through a flexible focusing lens group 409, a liquid crystal optical shutter 410, a quarter-wave plate 411, a dichroic mirror 406 and an oil immersion objective 405 to heat the target metal nanoparticles 301; meanwhile, imaging systems of the donor substrate 102 and the acceptor substrate 101 in the first CCD imaging system 413 and the second CCD imaging system 414 are realized through the tube lens 407 and the beam splitter 412 during laser irradiation, and imaging 415 of the surface of the donor substrate and imaging 416 of the surface of the acceptor substrate are observed on a computer. Observation of the donor substrate and the acceptor substrate conditions during non-laser irradiation in the first CCD imaging system 413 and the second CCD imaging system 414 is accomplished by a common bulb 404 and focusing lens 403.
The above description is only a preferred embodiment of the present invention, and for those skilled in the art, the present invention should not be limited by the description of the present invention, which should be interpreted as a limitation.
Claims (6)
1. A method for metal-assisted chemical etching of discrete silicon nanopore patterns is characterized by comprising the following steps:
cleaning a receptor substrate and a donor substrate;
step two, spin-coating a polydimethylsiloxane layer on the surface of the donor substrate, and naturally curing;
step three, diluting the metal nano particle solution, spin-coating the metal nano particle solution on the polydimethylsiloxane layer, and naturally drying the polydimethylsiloxane layer;
moving the target metal nano particles to be below the laser focus under the condition that the laser beam is closed, and simultaneously moving the target deposition position of the receptor substrate to be above the laser beam focus;
irradiating the metal nanoparticles by focused laser beams to release the metal nanoparticles from the donor substrate and transfer the metal nanoparticles to the receptor substrate;
moving the next target metal nano particle to be transferred to a position below the laser focus, simultaneously moving the next target position to be deposited of the receptor substrate to a position above the laser beam focus, and repeating the fifth step;
and step seven, repeating the step six, and finally depositing the metal nanoparticles with the discrete pattern on the receptor substrate.
2. The method of metal assisted chemical etching of discrete silicon nanopore patterns according to claim 1, wherein: in the first step, a glass cover glass is selected as a donor substrate and a silicon wafer is selected as an acceptor substrate, absolute ethyl alcohol and deionized water are respectively used for ultrasonic cleaning, and the surface is dried by nitrogen.
3. The method of metal assisted chemical etching of discrete silicon nanopore patterns according to claim 1, wherein: and in the second step, a PDMS curing mixture is taken by a pipette and dropped on the donor substrate in the first step, the mixture is uniformly spin-coated by a spin coater, and the donor substrate is taken down and naturally cured in a dry and clean environment to obtain a soft and thin polydimethylsiloxane layer.
4. The method of metal assisted chemical etching of discrete silicon nanopore patterns according to claim 1, wherein: and in the third step, a liquid transfer gun is used for taking the diluted metal nanoparticle dispersed liquid to be dripped on the polydimethylsiloxane layer of the donor substrate in the third step, a spin coater is used for spin coating, then the donor substrate is taken down and naturally dried.
5. The method of metal assisted chemical etching of discrete silicon nanopore patterns according to claim 1, wherein: and in the fourth step, the target metal nano particles and the target deposition position of the receptor substrate are moved to a laser focus through the imaging condition of a CCD imaging system in the optical system on a computer display and a computer-aided control nano positioning platform, and the laser focus is adjusted to further move the target metal nano particles below the focus and the target deposition position of the receptor substrate above the laser focus.
6. The method of metal assisted chemical etching of discrete silicon nanopore patterns according to claim 1, wherein: in the fifth step, the working wavelength of the continuous wave laser is selected to be 1064 nanometers, and the power is 100 mW/mum2。
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