CN112034741B - Liquid-phase micro-nano processing method and equipment - Google Patents

Liquid-phase micro-nano processing method and equipment Download PDF

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CN112034741B
CN112034741B CN202010869933.XA CN202010869933A CN112034741B CN 112034741 B CN112034741 B CN 112034741B CN 202010869933 A CN202010869933 A CN 202010869933A CN 112034741 B CN112034741 B CN 112034741B
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nano
film
processing
micro
phase
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CN112034741A (en
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方绍熙
王德强
何石轩
殷博华
谢婉谊
曾德琳
罗志勇
周大明
王赟姣
唐鹏
石彪
梁丽媛
尹雅洁
周硕
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Chongqing Institute of Green and Intelligent Technology of CAS
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Chongqing Institute of Green and Intelligent Technology of CAS
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    • GPHYSICS
    • G05CONTROLLING; REGULATING
    • G05BCONTROL OR REGULATING SYSTEMS IN GENERAL; FUNCTIONAL ELEMENTS OF SUCH SYSTEMS; MONITORING OR TESTING ARRANGEMENTS FOR SUCH SYSTEMS OR ELEMENTS
    • G05B19/00Programme-control systems
    • G05B19/02Programme-control systems electric
    • G05B19/04Programme control other than numerical control, i.e. in sequence controllers or logic controllers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81CPROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00015Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems

Abstract

The invention provides a liquid-phase micro-nano processing method and equipment, wherein the equipment is combined with the liquid-phase nano processing method, the graphical processing, the solid nanopore processing and the nano 3D printing of a nano film are realized on micro-nano processing equipment based on a nano glass micro-tube, a quartz tuning fork is adopted to control the nano glass micro-tube to directly contact with the nano film for processing, and the nano film is processed in a mode of setting bias voltage or current. The liquid-phase micro-nano processing method and the equipment can realize multiple operations of nano-graphic processing, nano-hole or nano-hole array processing, 3D nano-printing and the like with a platform, thereby realizing material reduction manufacturing and material increase manufacturing, and greatly improving the processing complexity, especially the nano-scale processing complexity.

Description

Liquid-phase micro-nano processing method and equipment
Technical Field
The invention belongs to the technical field of micro-nano processing, and relates to a liquid-phase micro-nano processing method and equipment, which can be used for preparing patterns with various shapes on various types of film base materials.
Background
The micro-nano processing technology is a core technology for breaking through and improving the major enterprises in each country since the development of the integrated circuit technology, and is also the core competitiveness of science and technology among countries. The photoetching equipment is core equipment in the field of micro-nano processing, directly determines the capacity of producing devices, and further influences the long-term development of comprehensive national force of a country. Currently, there are two main forms of lithography, including microlithography and micro-nano fabrication, or photomask fabrication and electron beam lithography.
The ultimate goal of photolithography is to produce various functional patterns and precise positioning on a film, plastic or glass substrate for a structure for selective exposure of a photoresist coating, known as a photolithographic reticle. The existing photoetching equipment mainly comprises an ultraviolet laser etching system and an electron beam exposure system, wherein the ultraviolet with extremely small wavelength is used as a laser light source, and the processing precision is improved to the nanometer level by adopting methods such as immersion processing and the like, so that the existing industrial chip production with the highest speed and the highest processing precision can be realized; the electron beam without diffraction limit is adopted for micro-nano processing, direct etching and exposure of the electron beam are realized, and the electron beam micro-nano processing method can be applied to processing of devices with high precision in small batches in a plurality of special application occasions. However, both of these methods are capital-intensive micro-nano processing methods, and the processing accuracy thereof is greatly affected by the environmental temperature, the photoresist performance, and the like, and the development cycle of the whole equipment is long. Therefore, the research on a new micro-nano processing method and equipment has important significance.
Disclosure of Invention
Based on the needs of reality and production practice, the applicant invests a large amount of funds, and long-term research provides a liquid-phase micro-nano processing method and equipment, which can be used for preparing patterns with various shapes on various types of film base materials, particularly can realize material reduction manufacturing and 3D printing of micro-nano devices on the same platform, further realize the processing and manufacturing of complex micro-nano devices, can realize solid nano hole array processing, particularly can realize the processing of micro-nano devices such as mask plates and the like, and are used for the fields of micro-nano processing and the like.
According to the first aspect of the technical scheme of the invention, the liquid phase micro-nano processing equipment is combined with a liquid phase nano processing method, graphical processing, solid nano hole processing and nano 3D printing of a nano film are realized on the micro-nano processing equipment of the nano glass micro tube, a quartz tuning fork is adopted to control the nano glass micro tube to directly contact with the nano film for processing, and the nano film is processed in a mode of setting bias voltage or current.
The liquid-phase micro-nano processing equipment comprises a nano glass micro-tube, a quartz tuning fork probe, a nano control platform, a controller, a signal generator, a phase-locked amplifier, a nano film, an electrode, a nano film substrate, a bias circuit and a control system.
Wherein, the nano glass microtube is used for controlling the contact area and the contact form of the buffer solution and the nano film; drawing the glass capillary by setting drawing parameters of the nano glass capillary under the action of laser to obtain the nano glass capillary, attaching a cantilever of the quartz tuning fork probe to the position 3-5mm away from the tip of the nano glass capillary, fixedly mounting the nano glass capillary by using a nano glass capillary holder, and controlling the nano glass capillary by using a nano control platform and a controller; the nano glass micro tube is connected with a bias circuit through a silver or silver chloride electrode.
In addition, the quartz tuning fork probe is used for detecting the contact displacement change between the two groups of nano glass microtube electrodes and the nano film in the longitudinal direction; the quartz tuning fork probe is connected with the tip of the nano glass microtube in an attaching mode, the quartz tuning fork probe is connected with the signal generator and the phase-locked amplifier through a tuning fork end electrode interface, the signal generator provides a driving signal for the quartz tuning fork, and the phase-locked amplifier detects the change conditions of the amplitude, the frequency and the phase of the quartz tuning fork, so that the transverse stress condition of the cantilever of the quartz tuning fork is calculated, and the direct distance relation between the tip of the nano glass microtube and the nano film is calculated.
According to a second aspect of the patent technical scheme of the invention, a liquid-phase micro-nano processing method is provided, which comprises the following steps:
step 1, drawing a nano glass micro tube, and injecting a buffer solution, wherein the buffer solution injection mode comprises centrifugal injection and microwave injection; installing the nanometer glass microtubule on the upper nanometer control platform and the controller by using the nanometer glass microtubule clamper, connecting an upper electrode, and connecting the electrode with a bias circuit;
fixing the quartz tuning fork probe on the nano control platform and the controller, and respectively connecting 2 groups of quartz tuning fork electrodes to the signal generator and the phase-locked amplifier;
step 3, designing a nanometer control platform and a controller, and respectively controlling two groups of quartz tuning forks and a nanometer thin film chip on the nanometer control platform and the controller;
step 4, selecting a signal generator with at least two detection functions and a phase-locked amplifier device, and controlling and detecting through a computer end;
step 5, preparing a nano film chip; the nano film chip is a sample device to be processed and is divided into a suspended nano film chip of a solid nanopore or nanopore array to be processed and a chip of a photoresist nano film or PMMA nano film with a chromium or gold conducting layer plated at the lower end of the film;
step 7, designing or manufacturing a bias circuit for micro-nano processing, wherein the bias circuit can provide voltage output far higher than the breakdown voltage of the nano film and current output capable of modifying the nano film;
and 8, designing or controlling a computer end system of the whole micro-nano machining process.
Compared with the prior art, the liquid-phase micro-nano processing method and the equipment adopt a liquid-phase contact mode to process the nano film, and combine the electric breakdown and electric field modification modes to process nano-scale patterns, nano holes and the like; the bias circuit is adopted to provide a processing electric field, the range of processable materials is wide, and the range of the provided electric field is large, so that thin film materials with different materials and different thicknesses (0.35nm-300nm) can be processed.
In the invention, the nano detection is carried out by adopting a mode that the quartz tuning fork is vertically attached to the tube tip of the nano glass microtube, so that the quartz tuning fork works under higher quality factors and is less influenced by the weight of the nano glass microtube, further the distance detection precision of nm level can be obtained, and the nano processing precision is greatly improved.
The liquid-phase micro-nano processing method and the equipment can realize multiple operations of nano-pattern processing, nano-hole or nano-hole array processing, 3D printing and the like on the same platform, not only realize material reduction manufacturing, but also realize material increase manufacturing, and can greatly improve the processing complexity, especially the nano-scale processing complexity.
Because the whole machine adopts a liquid phase processing mode, the liquid phase micro-nano processing method and the equipment can provide possibility for assembling and adjusting a plurality of biomolecules.
Drawings
FIG. 1 is a schematic diagram of the system architecture of the present invention;
FIG. 2 is a drawing process diagram of the nano-glass micro tube of the present invention;
FIG. 3 is a schematic diagram of a nano-film structure for micro-nano pattern processing;
FIG. 4 is a schematic diagram of a nanofilm structure for nanopore processing;
FIG. 5 is a schematic diagram of a nano-substrate structure for 3D nano-printing;
FIG. 6 is a prepared nanopore IV curve and an electron micrograph of the present invention.
The reference numbers in the drawings are as follows:
in fig. 1, a nano glass microtube 1, a quartz tuning fork probe 2, a nano control platform and controller 3, a signal generator 4, a lock-in amplifier 5, a nano film 6, an electrode and nano film substrate 7, a bias circuit 8 and a control system 9.
In fig. 2, a glass capillary 101, a laser 102, a nano-glass micro tube 1, and drawing parameters 103.
In fig. 3, 4 and 5, a silicon-based material 701, a chrome/gold plating layer 702, and a nano-film 6.
In FIG. 6, the IV curve 601 of the processing of nanopores in a 10nm silicon nitride nanofilm at different voltages (11V, 15V, 20V, 40V) corresponds to the TEM image 602 of 20V processing; transmission electron micrograph 603 for 40V processing.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, not all embodiments. All other embodiments obtained by a person skilled in the art based on the embodiments in the patent of the invention without any inventive work belong to the protection scope of the patent of the invention.
The invention discloses a liquid-phase micro-nano processing method and equipment, belongs to a novel micro-nano processing mode, and realizes micro-nano processing in a liquid-phase environment. According to the system, a quartz tuning fork is adopted to control a nano glass microtube to directly contact with a nano film for processing, and a bias voltage or current mode is adopted to process the nano film, so that the micro-nano processing precision is greatly improved, and the system can be used for graphic processing, nano hole or nano array processing and nano 3D printing. The whole system is small and is not limited by the processing size.
The liquid phase micro-nano processing equipment comprises a nano glass micro-tube (micropipette)1, a quartz tuning fork probe 2, a nano control platform and controller 3, a signal generator 4, a phase-locked amplifier 5, a nano film 6, an electrode and nano film substrate 7, a bias circuit 8 and a control system 9.
The nano glass micro tube (micropipette)1 is used for controlling the contact area and the contact form of a buffer solution and a nano film, and is obtained by setting drawing parameters of the nano glass micro tube and drawing the nano glass micro tube by using a glass capillary 101 under the action of laser 102. The size of the tip of the nano glass microtube is closely related to drawing parameters and directly influences the precision of liquid phase processing and nanopore processing. The nano glass microtube and the quartz tuning fork 2 are jointed with the tip of the nano glass microtube at a position of 3-5mm, so that the contact force between the nano glass microtube and the nano film is detected; fixedly mounting the nano glass micro tube by a nano glass micro tube holder, wherein the nano glass micro tube is controlled by the motion of the nano control platform and the controller 3; the nano glass micro-tube is connected with the bias circuit 8 through a silver or silver chloride electrode, so that the bias circuit applies electric fields or voltage signals with different strengths on the nano glass micro-tube electrode.
And the quartz tuning fork probe 2 is used for detecting the contact displacement change between the longitudinal electrodes of the two groups of nano glass microtubes 1 and the nano film. The quartz tuning fork probe 2 is vertically attached to the tube tip of the nano glass micro tube 1, so that the tuning fork is not influenced by the gravity of the nano glass micro tube, and the contact force is detected; the quartz tuning fork probe 2 is connected with the signal generator 4 and the phase-locked amplifier 5 through a tuning fork end electrode interface, wherein the signal generator 4 provides a driving signal for the quartz tuning fork, and the phase-locked amplifier 5 detects the variation conditions of the amplitude, the frequency, the phase and the like of the quartz tuning fork, so that the transverse stress condition of the cantilever of the quartz tuning fork is calculated, and the direct distance relation between the tip of the nano glass microtube 1 and the nano film 6 is calculated.
The nano control platform and the controller 3, 3 in total, are used for the motion control of two groups of nanometer glass microtubes and nanometer film chips respectively, the control platform and the controller, the nanometer glass microtubes 1 and the nanometer film chips 6 all adopt the mechanical fixation mode, the control platform and the controller are connected with the control system 9 through a USB serial communication bus or an Ethernet bus, the motion control command sent by the control system 9 is received, 3 control objects are controlled to corresponding positions according to the closed-loop control mode of displacement and drive current, and then position control basis is provided for nanopore processing, nanometer graphic processing and 3D printing.
The signal generator 4 is used for generating an excitation signal required by the vibration of the quartz tuning fork 2, controlling the amplitude, the frequency and the phase parameter provided by the control system 9 to generate a corresponding sine wave signal, and is respectively connected to the input electrodes of the quartz tuning fork 2 through signal lines to serve as the excitation signal and connected to the reference signal input end of the lock-in amplifier 5 to serve as a detection reference signal.
A lock-in amplifier 5 for detecting the variation of the amplitude, frequency and phase of the output signal of the quartz tuning fork 2, which is connected to the signal output electrode of the quartz tuning fork 2 in a connection relationship or a functional relationship with the quartz tuning fork 2, and detecting the variation of the amplitude, frequency and phase of the signal; it is connected with the control system 9 through a serial communication bus, and feeds back detected signals of amplitude, frequency and phase to the control system 9;
the nano film 6 is used for manufacturing a photoetching mask or a nano hole, and grows or transfers the nano film to the film substrate 7 together with the nano film substrate 7 in a growing and transferring mode; the photomask material is a nano film 6, a photoresist coating or a PMMA coating, and the thickness is 5nm-300 nm; the nano film material for processing nano holes can be graphene, silicon nitride, molybdenum disulfide and other materials, and has a thickness range of 0.35-300 nm
And the electrode and nano film substrate 7 is used for providing a fixing support of a nano film or a substrate material for nano processing and 3D printing, and is fixedly connected with the nano control platform and the controller 3 through a mechanical fixing clamp.
The bias circuit 8 is used for providing a processing electric field or voltage for nano processing and nano hole processing and providing a driving current for 3D printing, and the bias circuit, the nano glass microtube 1 and the nano film chip 6 are coated with a conductive electrode by pouring a salt buffer solution into the nano glass microtube 1 and are connected to the positive and negative of the bias circuit 8 through an electrode connecting wire;
and the control system 9 is used for importing a user processing requirement file and controlling each module to process, and is connected with the phase-locked amplifier, the signal generator, the bias circuit and the piezoelectric controller through a serial communication bus to realize the closed-loop operation of uplink signal acquisition and downlink command control.
The liquid-phase micro-nano processing method specifically comprises the following steps:
step 1, drawing a nano glass micro tube 1, injecting a buffer solution, installing the nano glass micro tube on a nano control platform and a controller 3 on the upper side through a nano glass micro tube holder, connecting an upper electrode, and connecting the electrode with a bias circuit 8;
the nano glass micro tube 1 is drawn on a nano glass micro tube drawing instrument by adopting a glass capillary tube, and the drawing process is shown in figure 2. The nano glass microtube is drawn by a laser drawing instrument, and the setting parameters comprise heating temperature, spot diameter, drawing speed, cooling time and tension. The material can be borosilicate, aluminosilicate and quartz glass material. The nano glass micro tube drawing process as shown in fig. 2, wherein the drawing parameters 103 for the nano glass micro tube drawing include: heating temperature, spot diameter, drawing speed, cooling time and tension. The glass capillary 101 material includes three types of borosilicate, aluminosilicate, and quartz.
The diameter range of the tube tip of the nano glass micro tube used in the invention is 5nm-3um, wherein the nano glass micro tube within the range of 5nm-100nm is used for micro-nano processing and 3D printing, and the precision of the micro-nano processing and 3D printing is directly determined to be 5nm-100nm by the size of the tip; the solid nanopore processing uses the tube tip size of 100nm-3um, and the size does not influence the pore diameter test of the nanopore, and can process the solid nanopore with larger pore diameter.
And 2, preparing or purchasing a quartz tuning fork probe 2, fixing the quartz tuning fork probe on the nanometer control platform and the controller 3, and respectively connecting 2 groups of quartz tuning fork electrodes to the signal generator 4 and the phase-locked amplifier 5.
And testing the performance parameters of the two quartz tuning forks, including amplitude, vibration frequency and the like. And respectively moving 2 groups of quartz tuning forks to be close to the tube tip of the nano glass microtube 1, testing the change of the performance parameters of the quartz tuning forks in real time, and detecting and resetting the performance parameter values of the tuning forks when the tuning fork arms are close to the tube tip of the nano glass microtube to serve as a detection device for detecting the distance between the tube tip and the nano film.
When the position of the nano-film 6 is fixed, the nano control platform and the controller are controlled to respectively control the two groups of nano glass micro-tubes to approach the nano-film, and when liquid drops at the tube tips of the nano glass micro-tubes are contacted with the nano-film, the tuning fork drives the transverse shearing force of the tube tips of the nano glass micro-tubes to change due to the influence of the action of the liquid drops and the nano-film, so that the change of parameters such as the vibration frequency of the tuning fork is influenced, and the contact detection of the nano glass micro-tubes and the nano-film is realized. And longitudinal nanometer distance detection basis is provided for subsequent nanometer control.
And 3, designing a nanometer control platform and a controller 3. The nanometer control platform and the controller 3 respectively control the two groups of quartz tuning forks 2 and the nanometer film chip.
The nanopore control platform and the controller 3 are 3 groups in total, two groups of quartz tuning forks and nanometer glass micro-tubes are respectively controlled by tuning fork fixing structures and nanometer glass micro-tube holders, and the nanometer thin film chip is controlled to move by a fixing platform of the nanometer thin film chip. The nanoscale control among the three is realized, each group has at least 3-axis control performance, nanoscale linear interpolation motion and nanoscale circular interpolation motion can be realized, and 3-axis linkage can be realized.
The nanometer control platform and the controller are connected with a computer through an Ethernet cable or a USB communication bus and are controlled by a computer end control module system.
And 4, selecting the signal generator 4 with at least two detection functions and the lock-in amplifier device, and programming, controlling and detecting through a computer terminal.
The signal generator and the phase-locked amplifier are connected with the two groups of quartz tuning fork electrodes, so that the driving of the tuning fork probe is realized, and the detection of the vibration parameters of the probe is also realized.
The signal generator and the phase-locked amplifier are connected with a computer through a serial communication bus and are controlled by a computer end detection module system.
And 5, preparing the nano film chip. The chip is a sample device to be processed and can be divided into a suspended nano film chip of a solid nano hole or a nano hole array to be processed and a photoresist nano film or PMMA nano film 6 with a conductive layer of chromium or gold and the like plated at the lower end of the film.
The nano film material of the suspended nano film chip for processing the nano holes or the nano hole array can be silicon nitride, graphene, molybdenum disulfide, tungsten disulfide and other materials which are conventionally used for processing solid nano holes, and can also be PMMA and other low dielectric constant nano film materials which can be subjected to dielectric breakdown. The lower end of the nano film material needs to be immersed in or contacted with a buffer solution which is the same as that in the nano glass micro-tube to form a trans end and a cis end for processing a nano hole or a nano hole array;
the lower end of the film is plated with a photoresist nano film or a PMMA nano film of conducting layer chromium or gold and the like, the nano film is prepared by spin-coating photoresist or PMMA with nano thickness on a purchased wafer chip plated with chromium or gold, and drying to obtain a nano film material for micro-nano processing. The conductive coating of the nano film has an electrode contact point connected with a bias circuit, and forms a micro-nano processed electrode pair with a nano glass micro-tube electrode.
In addition, when 3D printing is carried out, the nano film is changed into a substrate material for 3D printing, and a metal particle solution or other solvents for 3D printing are added into the nano glass micro-tube, so that nano-scale electrically-driven sample injection is realized.
And 6, designing or manufacturing a bias circuit 8 for micro-nano processing. The bias circuit can provide low ripple voltage of 1-200V and can be set as the output of a constant current source, and the output range of the constant current source is 0.5 nA-1A.
And 7, designing or controlling a computer end system of the whole micro-nano processing process.
The computer system comprises a detection control module which can control the phase-locked amplifier and the signal generator to detect the two groups of quartz tuning forks; the motion control system module for controlling the 3 groups of nano control platforms and the controller can realize linear interpolation motion and circular motion and can realize 3-axis linkage; the processing system module controls the bias circuit to output voltage and current and can detect the change of the voltage and the current in real time; the graphic command conversion system module is used for converting the graphic required to be processed by the user into a conversion system module for controlling the nano control platform and the instruction parameters of the controller; and the central control system module is used for combining detection signals of the quartz tuning fork, the nano control platform and the controller displacement sensor, the application of the bias circuit and detected micro-nano processing signals to be used as a reference basis for nano control and processing to form a closed-loop automatic micro-nano processing system.
More specifically, the following describes the application of the present invention by taking nanopatterning, nanopore array processing, and 3D printing as examples, respectively.
Processing a nanometer pattern:
as shown in fig. 3, the nano film structure for processing the micro-nano pattern is processed, and the nano pattern processing is a processing technology commonly used in the field of micro-nano processing and can be used for mask plate manufacturing and etching.
The silicon-based material 701 is flat in surface and easy to purchase; a chrome/gold plating layer 702, approximately 5nm-20nm thick, readily available for purchase and electroplating;
(1) and (5) preparing. Preparing a PMMA nano film plated with a chromium layer, wherein the lowermost layer of the PMMA nano film is a silicon wafer, the middle layer of the PMMA nano film is a chromium layer with the thickness of 5-20nm, and a joint for connecting a bias circuit electrode is reserved; drawing a 10nm nano glass micro-tube pair, filling 1M LiCl buffer solution, and installing on a nano control platform and a controller above the nano film; respectively adjusting two groups of quartz tuning forks to be close to the tips of the nano glass microtubes, and stopping the two groups of quartz tuning forks to be close to the tips of the nano glass microtubes after the vibration frequency reaches a preset value;
(2) and preparing a processing pattern. The method comprises the following steps of importing a graph to be processed into a system, converting the graph into a nanometer control platform, a controller motion track and a command file corresponding to processing parameters through a graph conversion module, and storing the nanometer control platform, the controller motion track and the command file into a cache, wherein the motion tracks and the working efficiency of two groups of nanometer glass micro-tubes are fully planned in the part of work, so that the two groups of nanometer glass micro-tubes can be processed at the same time, and the purpose of improving the processing efficiency is achieved;
(3) an initial position is located. And adjusting the horizontal initial positions of the two groups of nano glass micro tubes, namely controlling the horizontal positions of the two groups of nano glass micro tubes to the initial processing position of the graph to be processed. Then, respectively controlling the tube tips of the two groups of nano glass microtubes to be close to the nano film, and stopping approaching when the tube tip solution contacts the nano film;
(4) and (5) micro-nano processing. Controlling the nano control platform, the controller and the bias module according to the motion trail and the processing parameters in the step (2), processing the nano film at the corresponding point position, and finally finishing graphical processing according to the motion trail;
(5) and cleaning and characterizing the processing pattern. And lifting the nano glass microtube, and cleaning the processed nano film, so that the nano glass microtube is convenient for later-stage graphic representation and subsequent processing.
Processing a nanopore and a nanopore array:
as shown in fig. 4, the nano-film structure processing for nano-pore processing, nano-pore and nano-pore array processing can effectively replace the transmission electron microscope nano-pore processing and focused ion beam processing.
(1) And (5) preparing. Preparing a nano film chip with a suspension window structure, fixing the chip in a flow cell, ensuring that a lower windowing part is in contact with a solution at the lower end of the flow cell, and connecting an electrode; drawing 100nm-3um nanometer glass micro-tube pairs, filling 1M LiCl buffer solution, and installing on a nanometer control platform and a controller above the nanometer film; respectively adjusting two groups of quartz tuning forks to be close to the tips of the nano glass microtubes, and stopping the approach after the vibration frequency reaches a preset value (if only a single nanopore is processed, only one nano glass microtube needs to be controlled);
(2) and (4) processing the nano-holes. The positions of the nano holes or nano arrays to be processed, the pore diameters of the nano holes and other parameters are led into a system, and finally the parameters are converted into processing positions of a nano control platform and a controller and command files corresponding to the processing parameters, and the processing positions and the processing efficiency of the nano control platform and the controller are stored in a cache;
(3) an initial position is located. And adjusting the horizontal initial positions of the two groups of nano glass micro tubes, namely controlling the horizontal positions of the two groups of nano glass micro tubes to the first nano position of the nano hole to be processed.
(4) And (4) processing a nano hole. Setting a bias circuit to be in a constant current source working state according to the processing parameters in the step (2), and limiting the corresponding processing electric field to the parameter value corresponding to the aperture of the processed nano hole; respectively controlling the tube tips of the two groups of nano glass micro-tubes to approach the nano thin film in a nano mode, and finishing the processing of nano holes when the tube tip solution contacts the nano thin film; if only 1 or two nano holes are processed, directly jumping to the step 6;
(5) and (4) processing a nanopore array. Lifting the needle point of the nano glass micro tube, adjusting the two groups of nano glass micro tubes to the position of the second/group of nano holes to be processed, setting processing parameters, continuing to control the nano glass micro tubes to approach the nano film, finishing nano processing when the tube tip solution contacts the nano film, and repeating the steps until all the nano holes are processed.
(6) Nanopore characterization and testing. Lifting the nano glass microtube, and cleaning and characterizing the processed nano holes, or directly carrying out a nano hole test experiment and a nano array test experiment.
Nanometer 3D printing:
the processing of the nano-film structure for 3D nano-printing as shown in fig. 5 can realize electrically driven sample injection of 3D printed samples, realize the combination of electric field effect, and also perform operations related to biomolecules.
(1) And (5) preparing. Preparing a 3D printing substrate plated with a conductive layer and connecting the substrate to a bias circuit; drawing a 10-300 nm nano glass micro-tube pair, filling a metal nano particle solution or other 3D printing solutions for 3D printing, and installing the nano glass micro-tube pair on a nano control platform and a controller above a nano film; respectively adjusting two groups of quartz tuning forks to be close to the tips of the nano glass microtubes, and stopping the two groups of quartz tuning forks to be close to the tips of the nano glass microtubes after the vibration frequency reaches a preset value;
(2) and preparing a printing graph. The method comprises the following steps of importing a graph to be printed into a system, converting the graph into a nanometer control platform, a controller motion track and a command file corresponding to printing parameters through a graph conversion module, and storing the nanometer control platform, the controller motion track and the command file into a cache, wherein the motion tracks and the working efficiency of two groups of nanometer glass micro-tubes are fully planned in the part of work, so that the two groups of nanometer glass micro-tubes can be processed at the same time, and the purpose of improving the printing efficiency is achieved;
(3) an initial position is located. And adjusting the horizontal initial positions of the two groups of nano glass micro tubes, namely controlling the horizontal positions of the two groups of nano glass micro tubes to the initial printing position of the graph to be printed. Then, respectively controlling the tube tips of the two groups of nano glass microtubes to be close to the nano film, and stopping approaching when the tube tip solution contacts the nano film;
(4) and (4) nano 3D printing. Controlling the nano control platform, the controller and the bias module according to the motion trail and the processing parameters in the step (2), printing on corresponding point positions, and finally finishing graphical 3D printing according to the motion trail;
(5) printing pattern cleaning and characterization. And lifting the nano glass microtube, and cleaning the printed nano graph, so that later graph representation and subsequent use are facilitated.
The above description is only a preferred embodiment of the present invention, but the protection scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the embodiments of the present invention disclosed herein should be covered within the protection scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.

Claims (7)

1. A liquid phase micro-nano processing device is characterized in that: the method is combined with a liquid phase nano processing method, the graphical processing, the solid nano hole processing and the nano 3D printing of the nano film are realized on micro-nano processing equipment of the nano glass microtube, a quartz tuning fork probe is adopted to control the nano glass microtube to directly contact with the nano film for processing, and the nano film is processed in a mode of setting bias voltage or current;
the liquid-phase micro-nano processing equipment comprises a nano glass micro-tube (1), a quartz tuning fork probe (2), a nano control platform and controller (3), a signal generator (4), a phase-locked amplifier (5), a nano film (6), an electrode and nano film substrate (7), a bias circuit (8) and a control system (9);
the nano glass microtube (1) is used for controlling the contact area and the contact form of the buffer solution and the nano film; the quartz tuning fork probe (2) is used for detecting the contact displacement change between the longitudinal direction of the electrodes of the two groups of nano glass microtubes (1) and the nano film; the nano control platform and the controller (3) are 3 groups in total and are respectively used for controlling the motion of two groups of nano glass micro-tubes and nano film chips;
the signal generator (4) is used for generating an excitation signal required by the vibration of the quartz tuning fork probe (2), the control system (9) provides amplitude, frequency and phase parameters and controls to generate corresponding sine wave signals, the sine wave signals are respectively connected to the input electrodes of the quartz tuning fork probe (2) through signal lines, and the sine wave signals are connected to the reference signal input end of the phase-locked amplifier (5) to serve as a detection reference signal;
the phase-locked amplifier (5) detects the change conditions of the amplitude, the frequency and the phase of the quartz tuning fork probe, further calculates the transverse stress condition of the cantilever of the quartz tuning fork probe, and calculates the direct distance relationship between the tip of the nano glass microtube (1) and the nano film (6);
the nano film (6) is used for manufacturing a photoetching mask or a nano hole; the electrode and nano-film substrate (7) is used for providing a fixing support of a nano-film or a substrate material for nano-processing and 3D printing; the bias circuit (8) is used for providing a processing electric field or voltage for nano processing and nano hole processing and providing a driving current for 3D printing.
2. The liquid-phase micro-nano processing equipment according to claim 1, characterized in that: drawing by using a glass capillary (101) under the action of laser (102) by setting drawing parameters of the nano glass micro tube to obtain the nano glass micro tube (1), attaching a cantilever of a quartz tuning fork probe (2) to a tube tip of the nano glass micro tube (1) at a position of 3-5mm, fixedly mounting the nano glass micro tube by using a nano glass micro tube holder, and controlling the nano glass micro tube by using a nano control platform and a controller (3) in a motion manner; the nano glass microtube is connected with a bias circuit (8) through a silver or silver chloride electrode.
3. The liquid-phase micro-nano processing equipment according to claim 2, characterized in that: the quartz tuning fork probe (2) is vertically attached to the tube tip of the nano glass microtube (1), the quartz tuning fork probe (2) is connected with the signal generator (4) and the phase-locked amplifier (5) through a tuning fork end electrode interface, and the signal generator (4) provides a driving signal for the quartz tuning fork probe.
4. The liquid-phase micro-nano processing equipment according to claim 2, characterized in that: the nanometer control platform and the controller are mechanically fixed with the nanometer glass microtube (1) and the nanometer film (6), are connected with the control system (9) through a USB serial communication bus or an Ethernet bus, and receive a motion control command sent by the control system (9).
5. The liquid-phase micro-nano processing equipment according to claim 2, characterized in that: the nano film (6) and the electrode and nano film substrate (7) grow or transfer the nano film to the electrode and nano film substrate (7) in a growing and transferring mode.
6. The liquid-phase micro-nano processing equipment according to claim 2, characterized in that: the electrode and the nano film substrate (7) are fixedly connected with the nano control platform and the controller (3) through a mechanical fixing clamp.
7. The processing method using the liquid-phase micro-nano processing equipment of any one of claims 1 to 6, characterized by comprising the following steps: which comprises the following steps:
step 1, drawing a nano glass micro tube (1), injecting a buffer solution, installing the nano glass micro tube on an upper side nano control platform and a controller (3) by using a nano glass micro tube holder, connecting an upper electrode, and connecting the electrode with a bias circuit (8);
fixing quartz tuning fork probes on a nanometer control platform and a controller (3), and respectively connecting 2 groups of quartz tuning fork probe electrodes to a signal generator (4) and a phase-locked amplifier (5);
step 3, designing a nanometer control platform and a controller (3), and respectively controlling two groups of quartz tuning fork probes (2) and a nanometer film on the nanometer control platform and the controller (3);
step 4, selecting a signal generator (4) with at least two detection functions and a phase-locked amplifier device, and controlling and detecting through a computer end;
step 5, preparing a nano film chip; the nano film chip is a sample device to be processed and is divided into a suspended nano film chip of a solid nanopore or nanopore array to be processed and a chip of a photoresist nano film or PMMA nano film with a chromium or gold conducting layer plated at the lower end of the film;
step 7, designing or manufacturing a bias circuit for micro-nano processing, wherein the bias circuit can provide voltage output far higher than the breakdown voltage of the nano film and current output capable of modifying the nano film;
and 8, designing or controlling a computer end system of the whole micro-nano machining process.
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