CN108609578A - A kind of preparation method of multistage micro-nano motor - Google Patents

A kind of preparation method of multistage micro-nano motor Download PDF

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CN108609578A
CN108609578A CN201810412434.0A CN201810412434A CN108609578A CN 108609578 A CN108609578 A CN 108609578A CN 201810412434 A CN201810412434 A CN 201810412434A CN 108609578 A CN108609578 A CN 108609578A
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pedot
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CN108609578B (en
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董任峰
蔡跃鹏
王纯
王庆龙
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South China Normal University
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    • 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
    • B81C1/00349Creating layers of material on a substrate
    • 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
    • B81C1/00436Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
    • B81C1/00523Etching material
    • B81C1/00539Wet etching
    • 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
    • B81C1/00436Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
    • B81C1/00555Achieving a desired geometry, i.e. controlling etch rates, anisotropy or selectivity
    • B81C1/00611Processes for the planarisation of structures
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82BNANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B1/00Nanostructures formed by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • B82B1/002Devices comprising flexible or deformable elements
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y15/00Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81BMICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
    • B81B2201/00Specific applications of microelectromechanical systems
    • B81B2201/03Microengines and actuators
    • B81B2201/037Microtransmissions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81CPROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C2201/00Manufacture or treatment of microstructural devices or systems
    • B81C2201/01Manufacture or treatment of microstructural devices or systems in or on a substrate
    • B81C2201/0101Shaping material; Structuring the bulk substrate or layers on the substrate; Film patterning
    • B81C2201/0102Surface micromachining
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81CPROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C2201/00Manufacture or treatment of microstructural devices or systems
    • B81C2201/01Manufacture or treatment of microstructural devices or systems in or on a substrate
    • B81C2201/0101Shaping material; Structuring the bulk substrate or layers on the substrate; Film patterning
    • B81C2201/0128Processes for removing material
    • B81C2201/013Etching
    • B81C2201/0133Wet etching

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Microelectronics & Electronic Packaging (AREA)
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Abstract

The present invention proposes a kind of preparation method of multistage micro-nano motor, it is proposed that a kind of preparation method of multistage micro-nano motor is prepared for a kind of driving micron motor of chemistry of the driving nano-motor of novel load magnetic field.The motor can be moved first in chemical fields and gradually discharge Magnetic driving nano-motor, and the nano-motor discharged can move under field drives again, to execute respective goal task.The invention further can accurately control the placement position of nano-motor, and fractional motor is made to be run in finer working region;The fractional motor that different driving mode can be loaded simultaneously, realizes it in more various application values.

Description

A kind of preparation method of multistage micro-nano motor
Technical field
The present invention relates to micro-nano motor technologies fields, more particularly, to a kind of preparation method of multistage micro-nano motor.
Background technology
Micro-nano motor be it is a kind of can by multiple kinds of energy (chemical energy, luminous energy, acoustic energy, electric energy, magnetic energy etc.) activate and transport Dynamic (rotation, shuttle, aggregation, diffusion etc.), and size is micron or nano level microdevice.The research boom of micro-nano motor by Multiple subjects such as chemistry, physics, biology, environmentology, tribology, hydrodynamics are gradually penetrated into, current nano science is become Hot spot in research field.By the development in more than ten years, no matter micro-nano motor is from movenent performance, preparation process, or actually answers With achieving considerable progress.It is driving that the energy source driven according to motor can be divided into the chemical energy generated by chemical reaction Or external world's physical energy is driving (luminous energy, acoustic energy, magnetic energy, electric energy).The driving motor of chemical energy, as the term suggests it is passing through of one kind The micro-nano motor that reaction provides energy is learned, currently, usually with H2O2、HCl、N2H4、I2Deng for fuel report it is more;Physical energy drives Ejector half motor refers to then providing energy by extraneous physical field come the micro-nano motor that drives, such as optical drive micro-nano motor, sound-driving Micro-nano motor, Magnetic driving micro-nano motor, electric drive micro-nano motor etc..Meanwhile huge variation also has occurred in the form of motor, is in Existing diversified development.From initial bimetal nano line, more metal nanometer lines, micron tube, Janus balls and spiral till now The forms such as line emerge one after another, and the motor of different shape can drive itself using different energy.Micro-nano motor is as removable Microdevice, matter transportation, cancer cell capture be isolated, DNA is detected, ion identification and identification, organic matter degradation, Oily waste treatment etc. embodies preferable application value.Micro-nano motor is the forward position focus in current nanotechnology research field, Its appearance provides completely new thinking without the practical problem suspected of the following microsystem of solution.
Studies have shown that by the way that the nano particle for being loaded with drug to be attached on the outer surface of micro motor, motor can be with Therapeutic agent is effectively carried to by target location with the speed higher than three orders of magnitude of conventional Brownian movement by predefined path.This A little artificial synthesized microdevices are other than the notable control to the direction of motion, also in early stage in terms of other, wherein Micro-nano motor is explored urgently to realize in the application of biomedical aspect.It is micro-nano motor that cargo is delivered in a manner of controllable and is quick One of main application.However, crucial challenge is how to design, the motor with appropriate function is manufactured and optimizes, to realize The effective delivery and release of cargo.It is expected that reliable delivery vehicle can carry lot cargo to improve validity (such as drug Therapeutic efficiency in delivering), while different types of cargo is delivered for multitask (such as the treatment for overcoming drug resistance Or conjoint therapy), effective cargo (such as Drug controlled release) is discharged in a manner of a kind of response, and discharge when no longer needing Itself.In order to meet these crucial multi-functional requirements, we use template assist in electrodeposition method, make respectively in this patent Nano wire is prepared using AAO templates with two kinds of templates of aluminium oxide (AAO) and makrolon (PC), then using the side of etching Method prepares the nano thread structure of spiral;Using PC templates, micron rocket is prepared.Using the method for vacuum filtration, by spiral Nano thread structure is pumped into micron rocket, successfully constructs a kind of micron fire of new chemical driving and the full load of field drives Arrow, our this motor is referred to as two level motor, has the function of delivery, transmission and release.
The research of current micro-nano motor has been achieved for prodigious progress, and existing research is concentrated mainly on particle, Janus The motor of the micro-nano motor of the patterns such as ball, nano wire, nanometer sheet, helix, these single forms still suffers from sport efficiency not High, carrying capacity deficiency problem.Since fluid viscosity is excessive, the movement of micro-nano motor effect hindered can be made, motor Movement velocity declines, and their running environment is single, and then motor is caused to execute specific task (such as drug carrier, object Quality detection, water process, bacterium and cell capture transport etc.) when efficiency be greatly reduced, which greatly limits motor applications potentiality.
Invention content
The present invention proposes a kind of preparation method of multistage micro-nano motor, which can the first movement and gradual in chemical fields Magnetic driving nano-motor is discharged, the nano-motor discharged can move under field drives again, to execute respective goal task. The invention further can accurately control the placement position of nano-motor, and fractional motor is made to be run in finer working region;Together When can load the fractional motor of different driving mode, realize it in more various application values.
The technical proposal of the invention is realized in this way:A kind of preparation method of multistage micro-nano motor:
Then step 1 uses Pt with one layer of Ag of magnetron sputtering coater sputtering on alumina formwork as working electrode Electrode and Ag/AgCl reference electrodes, are barricaded as three-electrode system, using template assist in electrodeposition method, difference electro-deposition Ag, Au, Pd/ The plating solution of Cu, Pd/Cu alloy includes 30mM PdCl2, 20mM CuCl2With 0.1M HCl;
Step 2, Au layers are polished off with 3-4 μm of aluminum oxide polishing powder, and alumina formwork is dissolved in 3M NaOH solutions Middle 30min is then centrifuged for washing and solution is washed into neutrality, then use Ag sacrificial layers and Cu to discharge nano wire motor completely Concentrated nitric acid etches 10min, obtains the spiral nanometer line motor of Pd;
Step 3 on the glass sheet by the spiral nanometer line motor tiling of obtained Pd is sputtered with magnetron sputtering coater One layer of W metal, then ultrasound release Pd/Ni spiral nanometer line;
Step 4, with template assist in electrodeposition method, we use magnetron sputtering plating in 2 μm of polycarbonate template first Machine sputters layer of Au, electro-deposition PEDOT outer layers, and plating solution includes 8 μ L 3,4-rthylene dioxythiophenes (EDOT), 0.075g nitric acid Potassium (KNO3), 2.88g dodecyl sodium sulfates (SDS) and 10mL water;Then using the method for vacuum filtration, by the spiral shell of Pd/Ni Rotation nano wire is pumped into the polycarbonate template of PEDOT outer layers;
The PEDOT polycarbonate templates of spiral nanometer line containing Pd/Ni are barricaded as three-electrode system by step 5 again, Template assist in electrodeposition method is equally used, electrodeposit metals Zn, plating solution includes 80g L-1 ZnSO4With 20g L-1 H3BO3, directly Cover with the template in 2 μm of apertures completely to metal Zn;
Template is dissolved in 10min in dichloromethane solution by step 6, to discharge motor completely, is then centrifuged for, is washed, To obtain the full load micron rocket of PEDOT/Zn/Pd/Ni;
The full load micron rocket of PEDOT/Zn/Pd/Ni is placed in containing 0.3M HCl and 1.7% triton X- by step 7 In 100 running environment, the case where being observed the motion conditions of motor with inverted fluorescence microscope and discharged nano wire fractional motor, and Motion conditions of the nano wire fractional motor in magnetic field are observed, then the speed with corresponding software detection full load micron rocket is big It is small.
As a kind of perferred technical scheme, it is CHI660E using electrochemical workstation model in step 1.
Above-mentioned technical proposal is used, beneficial effects of the present invention are:The preparation method of multistage micro-nano motor of the invention, carries A kind of model by big motor delivery fractional motor is gone out, and can accurately control the placement position of fractional motor, so as to fractional motor More efficient completion task, provides for motor and is widely applied range.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this Some embodiments of invention without having to pay creative labor, may be used also for those of ordinary skill in the art With obtain other attached drawings according to these attached drawings.
Fig. 1 is Pd/Cu nanometer spirals line specific experiment flow chart of the present invention;
Fig. 2 is that the SEM of Pd helixes of the present invention schemes;
Fig. 3 is preparation flow such as figure below of the multistage micron rocket of the present invention;
Fig. 4 is that the SEM of PEDOT/Zn/Pd/Ni two levels motor of the present invention schemes;
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on Embodiment in the present invention, those of ordinary skill in the art are obtained every other without creative efforts Embodiment shall fall within the protection scope of the present invention.
As shown in Figs 1-4, a kind of preparation method of multistage micro-nano motor, includes the following steps:
Then step 1 uses Pt with one layer of Ag of magnetic controlled ion plating film machine sputtering on alumina formwork as working electrode Electrode and Ag/AgCl reference electrodes, are barricaded as three-electrode system, use electrochemical workstation, model CHI660E, using template Assist in electrodeposition method, electro-deposition Ag, Au, Pd/Cu, the plating solution of wherein Ag, Au directly buy commercial plating solution, Pd/Cu conjunctions respectively The plating solution of gold includes 30mM PdCl2, 20mM CuCl2With 0.1M HCl.In Fig. 1, a is that electro-deposition one cuts Au;B is electro-deposition Pd/ Cu alloys;C is to dissolve template, discharges Pd/Cu nano wires;D is to etch away Ag and Cu;E is sputtering layer of Ni.
Step 2 polishes off Au layers with 3-4 μm of aluminum oxide polishing powder, and the NaOH that 3M is dissolved on alumina formwork is molten Liquid 30min is then centrifuged for washing and solution is washed into neutrality, then use Ag sacrificial layers and Cu to discharge nano wire motor completely Concentrated nitric acid etches 10min, obtains the spiral nanometer line motor of Pd;
Step 3 on the glass sheet by the spiral nanometer line motor tiling of obtained Pd is sputtered with magnetic controlled ion plating film machine One layer of W metal, then ultrasound release Pd/Ni spiral nanometer line;
Step 4, with template assist in electrodeposition method, we use magnetic controlled ion plating film in 2 μm of polycarbonate template first Machine sputters layer of Au, as working electrode, then uses Pt electrodes and Ag/AgCl reference electrodes, is barricaded as three-electrode system, electro-deposition PEDOT outer layers, plating solution include 8 μ L 3,4-rthylene dioxythiophenes (EDOT), 0.075g potassium nitrate (KNO3), 2.88g dodecanes Base sodium sulfonate (SDS) and 10mL water;Then using the method for vacuum filtration, the spiral nanometer line of Pd/Ni is pumped into PEDOT outer layers Polycarbonate template in;
The PEDOT polycarbonate templates of spiral nanometer line containing Pd/Ni are barricaded as three-electrode system by step 5 again, Template assist in electrodeposition method is equally used, electrodeposit metals Zn, plating solution includes 80g L-1 ZnSO4With 20g L-1 H3BO3It (uses Sulphur acid for adjusting pH is 2.5), until metal Zn covers with the template in 2 μm of apertures completely;
Template is dissolved in 10min in dichloromethane solution by step 6, to discharge motor completely, is then centrifuged for, is washed, To obtain the full load micron rocket of PEDOT/Zn/Pd/Ni;
The full load micron rocket of PEDOT/Zn/Pd/Ni is placed in containing 0.3M HCl and 1.7% triton X- by step 7 In 100 running environment, the case where being observed the motion conditions of motor with inverted fluorescence microscope and discharged nano wire fractional motor, and Motion conditions of the nano wire fractional motor in magnetic field are observed, then the speed with corresponding software detection full load micron rocket is big It is small.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.

Claims (2)

1. a kind of preparation method of multistage micro-nano motor, which is characterized in that include the following steps:
Step 1 sputters one layer of Ag on alumina formwork with magnetron sputtering coater, as working electrode, then uses Pt electrodes With Ag/AgCl reference electrodes, it is barricaded as three-electrode system, using template assist in electrodeposition method, distinguishes electro-deposition Ag, Au, Pd/Cu, The plating solution of Pd/Cu alloys includes 30mM PdCl2, 20mM CuCl2With 0.1M HCl;
Step 2, Au layers are polished off with 3-4 μm of aluminum oxide polishing powder, and alumina formwork is dissolved in 3M NaOH solutions 30min is then centrifuged for washing and solution is washed into neutrality to discharge nano wire motor completely, then by Ag sacrificial layers and Cu with dense Nitric acid etching 10min obtains the spiral nanometer line motor of Pd;
Step 3 on the glass sheet by the spiral nanometer line motor tiling of obtained Pd sputters one layer with magnetron sputtering coater W metal, then ultrasound release Pd/Ni spiral nanometer line;
Step 4, with template assist in electrodeposition method, we are splashed in 2 μm of polycarbonate template with magnetron sputtering coater first Layer of Au, electro-deposition PEDOT outer layers are penetrated, plating solution includes 8 μ L 3,4-rthylene dioxythiophenes (EDOT), 0.075g potassium nitrate (KNO3), 2.88g dodecyl sodium sulfates (SDS) and 10mL water;Then using the method for vacuum filtration, by the spiral of Pd/Ni Nano wire is pumped into the polycarbonate template of PEDOT outer layers;
The PEDOT polycarbonate templates of spiral nanometer line containing Pd/Ni are barricaded as three-electrode system, equally by step 5 again Using template assist in electrodeposition method, electrodeposit metals Zn, plating solution includes 80g L-1ZnSO4With 20g L-1H3BO3, until metal Zn covers with the template in 2 μm of apertures completely;
Template is dissolved in 10min in dichloromethane solution by step 6, to discharge motor completely, is then centrifuged for, is washed, with To the full load micron rocket of PEDOT/Zn/Pd/Ni;
The full load micron rocket of PEDOT/Zn/Pd/Ni is placed in containing 0.3M HCl and 1.7% triton x-100 by step 7 In running environment, the case where being observed the motion conditions of motor with inverted fluorescence microscope and discharged nano wire fractional motor, and observe Motion conditions of the nano wire fractional motor in magnetic field, then with the velocity magnitude of corresponding software detection full load micron rocket.
2. a kind of preparation method of multistage micro-nano motor as described in claim 1, which is characterized in that using electrification in step 1 It is CHI660E to learn work station model.
CN201810412434.0A 2018-05-03 2018-05-03 Preparation method of multistage micro-nano motor Expired - Fee Related CN108609578B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110002397A (en) * 2019-04-04 2019-07-12 南京航空航天大学 A kind of preparation method of complex configuration nano-motor
CN109998489A (en) * 2019-04-15 2019-07-12 哈尔滨工业大学 Photoacoustic signal detection and imaging method based on micro-nano motor
CN110203880A (en) * 2019-06-04 2019-09-06 百色学院 A kind of preparation method of CD-ROM drive magnetic control integration micro-nano motor

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CN104089940A (en) * 2014-07-22 2014-10-08 中国科学院烟台海岸带研究所 Tubular protein blot catalytic magnetic micro-motor as well as preparation method and application of tubular protein blot catalytic magnetic micro-motor
CN106756813A (en) * 2016-12-18 2017-05-31 江苏师范大学 A kind of micro-nano motor and preparation method thereof
CN107425749A (en) * 2017-08-08 2017-12-01 哈尔滨工业大学深圳研究生院 A kind of nano-motor and preparation method thereof

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CN102530853A (en) * 2012-01-11 2012-07-04 哈尔滨工业大学 Preparation method of artificial nanometer pipes and application of utilizing artificial nanometer pipes as nanometer motors
KR101367374B1 (en) * 2013-03-12 2014-03-19 서울대학교산학협력단 Nanowire storing biochemical material and manufacturing method thereof
CN104089940A (en) * 2014-07-22 2014-10-08 中国科学院烟台海岸带研究所 Tubular protein blot catalytic magnetic micro-motor as well as preparation method and application of tubular protein blot catalytic magnetic micro-motor
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110002397A (en) * 2019-04-04 2019-07-12 南京航空航天大学 A kind of preparation method of complex configuration nano-motor
CN109998489A (en) * 2019-04-15 2019-07-12 哈尔滨工业大学 Photoacoustic signal detection and imaging method based on micro-nano motor
CN109998489B (en) * 2019-04-15 2021-09-17 哈尔滨工业大学 Photoacoustic signal detection and imaging method based on micro-nano motor
CN110203880A (en) * 2019-06-04 2019-09-06 百色学院 A kind of preparation method of CD-ROM drive magnetic control integration micro-nano motor

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