CN107879309A - The hollow cantilever probe delivered and extracted for micro/nano-scale material - Google Patents

The hollow cantilever probe delivered and extracted for micro/nano-scale material Download PDF

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Publication number
CN107879309A
CN107879309A CN201711111195.7A CN201711111195A CN107879309A CN 107879309 A CN107879309 A CN 107879309A CN 201711111195 A CN201711111195 A CN 201711111195A CN 107879309 A CN107879309 A CN 107879309A
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CN
China
Prior art keywords
probe
cantilever beam
cantilever
hollow
pothole
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Granted
Application number
CN201711111195.7A
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Chinese (zh)
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CN107879309B (en
Inventor
宋杰
齐岱宗
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Shanghai Jiaotong University
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Shanghai Jiaotong University
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Priority to CN201711111195.7A priority Critical patent/CN107879309B/en
Publication of CN107879309A publication Critical patent/CN107879309A/en
Application granted granted Critical
Publication of CN107879309B publication Critical patent/CN107879309B/en
Expired - Fee Related legal-status Critical Current
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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
    • B81B3/00—Devices comprising flexible or deformable elements, e.g. comprising elastic tongues or membranes
    • 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
    • B81C1/00134—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems comprising flexible or deformable structures
    • B81C1/0015—Cantilevers
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
    • G01Q70/00—General aspects of SPM probes, their manufacture or their related instrumentation, insofar as they are not specially adapted to a single SPM technique covered by group G01Q60/00
    • G01Q70/08—Probe characteristics
    • G01Q70/10—Shape or taper
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
    • G01Q70/00—General aspects of SPM probes, their manufacture or their related instrumentation, insofar as they are not specially adapted to a single SPM technique covered by group G01Q60/00
    • G01Q70/16—Probe manufacture
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
    • B81B2203/00—Basic microelectromechanical structures
    • B81B2203/01—Suspended structures, i.e. structures allowing a movement
    • B81B2203/0118—Cantilevers

Abstract

A kind of hollow cantilever probe delivered and extracted for micro/nano-scale material, hollow cantilever probe, is flat cube structure, is made up of the cantilever beam of funnelform probe and tubulose, wherein：Cantilever beam is hollow with probe interior and is connected to convey material, i.e., the needle point open at one end using one end of cantilever beam as top, probe is end, by applying malleation or negative pressure at top, realizes and material is sucked or delivered from end to specimen surface.The present invention imposes appropriate transformation with MEMS technology to conventional cantilever beam and probe, then can obtain the new construction with material delivery and abstraction function, will carry the cantilever beam of transfer passage and the combining structure " hollow cantilever probe " of probe.The present invention reflects the surface topography information of sample by mutually attracting with specimen surface or repelling.

Description

The hollow cantilever probe delivered and extracted for micro/nano-scale material
Technical field
The present invention relates to a kind of technology in micro-nano field, is specifically that a kind of micro/nano-scale material that is used for is delivered and carried The hollow cantilever probe taken, realize that the material of micro/nano-scale is delivered and extracted.
Background technology
Analytical instrument of the AFM (Atomic Force Microscope, AFM) as object surface structure, Occur the interaction of atom level by miniature force sensing element and sample surfaces, and by sensor by it be converted into it is detectable with The electric signal of processing, realize the observation to sample surface morphology and property；Its resolution ratio can essence to nanoscale, three-dimensional can be provided Exterior view and do not require the experimental situation of vacuum or specially treated done to sample, the industry such as biotechnology, translational medicine with Research field is used widely.The core of AFM is its cantilever beam and probe as force sensing element, this Part also determines the overall performance and specific works pattern of machine.
Microelectromechanical systems (Micro Electro Mechanical System, MEMS) be microelectric technique with it is micro- The combination of process technology, made and processing equipment structure on micro/nano-scale；Its ripe bulk silicon micromachining technology may be selected Property with corrosive agent remove substrate, obtain with specific morphology micromechanical component, from its towards yardstick and applicable material All it is to make AFM cantilever beam and the ideal technology of probe portion for upper.
The content of the invention
The present invention is directed to deficiencies of the prior art, and proposition is a kind of to be used for what micro/nano-scale material was delivered and extracted Hollow cantilever probe, appropriate transformation is imposed to conventional cantilever beam and probe with MEMS technology, then can obtain delivered with material and The new construction of abstraction function, the cantilever beam of transfer passage and the combining structure " hollow cantilever probe " of probe will be carried.This hair It is bright to reflect the surface topography information of sample by mutually attracting with specimen surface or repelling, observe in brief；In order to both There is the material for realizing corresponding scale on the basis of AFM observing function to deliver and extraction.
The present invention is achieved by the following technical solutions：
The present invention relates to a kind of preparation method of hollow cantilever probe, by being obtained in substrate surface by anisotropic etch To the pyramid shape pothole with cantilever beam, then a covering is placed on above pothole and carries out low-temperature oxidation deposition, finally Remove the unnecessary substrate in pothole bottom and remove pothole hole and the cantilever beam other end with photo-etching processes, obtain hollow cantilever and visit Pin.
Described anisotropic etch, in particular to：In substrate surface with reactive ion etching (RIE) technique etching off tradition The cantilever beam profile of probe, a pyramid shape pothole is produced using KOH anisotropic etch in this profile adjacent one end.
The lower surface of described coating and the spacing of the upper surface of substrate, i.e., both are not in contact and minimum distance is 1 Micron.
Described coating uses but is not limited to silicon chip.
Described substrate uses but is not limited to silicon chip.
Described removal, which uses, to be singly not limited to halogen gas (F2Or Cl2Gas) unnecessary substrate is removed.
The present invention relates to the hollow cantilever probe that the above method is prepared, and is flat cube structure, by funnelform spy The cantilever beam of pin and tubulose forms, wherein：Cantilever beam is hollow with probe interior and is connected to convey material.
The part length of side of described hollow cantilever probe central sill is~80 μm long ×~10 μm wide ×~2 μ m-thick, and internal diameter is It can ignore in overall dimension with the length and width difference of external diameter, about 1 μm of cavity thickness, needle point bore is~500nm.
The application for the hollow cantilever probe being prepared the present invention relates to the above method, using one end of cantilever beam as top, The needle point open at one end of probe is end, by applying malleation or negative pressure at top, realize suck or deliver from end material to Specimen surface.
Technique effect
Compared with prior art, the present invention realizes suitable with structure dimension material transfer, thus not only can in molecule or Delivered and extracted in micel aspect, can also need to carry out cell and the behaviour of subcellular fraction aspect to biological tissue with research Make.The limit of power of correlative study will be expanded to the optimization design and improvement making of cantilever beam and probe, and be bigger view System research provides basis and may.
Brief description of the drawings
Fig. 1 is present invention process schematic diagram；
In figure：A~f is the corresponding process of the present invention；
Fig. 2 is embodiment effect diagram.
Embodiment
The present embodiment comprises the following steps：
1) in silicon chip surface with the cantilever beam profile of reactive ion etching (RIE) technique etching off conventional probe, in this profile Adjacent one end produces a pyramid shape pothole using KOH anisotropic etch；
2) another to take a silicon chip to cover thereon, two silicon chip surface spacing of control are in 1 microns；
3) oxidation growth layer is formed in silicon chip surface with gate oxidation process, edge of cantilever beam reverse mould profile is also during this It will be connected with top layer silicon chip with the oxide layer grown；
Described gate oxidation process, specifically includes following steps：
3.1) prerinse：O2Kept for 1 hour with 1100 DEG C with the oxidation furnace chamber of HCl mixed gas atmosphere, after with N2Purging, drop Temperature is to 800 DEG C；
3.2) load：In O2And N2Mixed gas atmosphere in by sample load oxidation furnace chamber；
3.3) aoxidize：In O2Aoxidized with HCl mixed gas atmosphere with 1000 DEG C, grow SiO2；
3.4) anneal：In N2With 1050 DEG C of annealing in gas atmosphere；
3.5) cool down：Stop heating and insulation, treat that cavity temperature is down to less than 800 DEG C taking-up samples.
4) with halogen gas (F2Gas or Cl2Gas) elementary silicon substrate is removed；
5) needle point and cantilever beam rear part are removed with photo-etching processes, obtains hollow cantilever probe.
Described photo-etching processes, specifically include following steps：
5.1) gluing：Positive photoresist；
5.2) front baking：80 DEG C of hot plates 4 hours；
5.3) expose：30 minutes 2 hours；
5.4) develop：3 minutes；
5.5) dried after：90 DEG C of baking ovens 5 hours；
5.6) etch；
5.7) remove photoresist.
As shown in Fig. 2 the cantilever probe that the present embodiment is prepared is flat cube structure, the part length of side of its central sill is ~80 μm long ×~10 μm wide ×~2 μ m-thick, internal diameter is that can ignore in overall dimension with the length and width difference of external diameter, and cavity is thick About 1 μm of degree, needle point bore are~500nm；The cantilever beam of funnelform probe and tubulose collectively constitutes new cantilever probe, wherein Empty structure can meet the needs of material conveying.Needle point using the cantilever opening of this hollow cantilever probe as top, probe is opened Mouthful place is end, and top is noted with the certain pressure and not liquid or gas with material reaction, can be by controlling this pressure Specimen surface is delivered to by end by the material suction of specimen surface near end or by the material of intracavitary.
Above-mentioned specific implementation can by those skilled in the art on the premise of without departing substantially from the principle of the invention and objective with difference Mode local directed complete set is carried out to it, protection scope of the present invention is defined by claims and not by above-mentioned specific implementation institute Limit, each implementation in the range of it is by the constraint of the present invention.

Claims (6)

1. a kind of hollow cantilever probe, it is characterised in that be flat cube structure, by funnelform probe and the cantilever beam of tubulose Composition, wherein：Cantilever beam is hollow with probe interior and is connected to convey material.
2. a kind of application of hollow cantilever probe according to claim 1, it is characterised in that using one end of cantilever beam as the beginning End, the needle point open at one end of probe are end, by applying malleation or negative pressure at top, realize and material is sucked or delivered from end To specimen surface.
3. the preparation method of a kind of hollow cantilever probe according to described in claim 1 or 2, it is characterised in that by base Basal surface obtains the pyramid shape pothole with cantilever beam by anisotropic etch, and then a covering is placed on above pothole And low-temperature oxidation deposition is carried out, finally remove the unnecessary substrate in pothole bottom and remove pothole hole and cantilever beam with photo-etching processes The other end, obtain hollow cantilever probe.
4. according to the method for claim 3, it is characterized in that, described anisotropic etch, in particular to：In substrate surface With the cantilever beam profile of reactive ion etching (RIE) technique etching off conventional probe, this profile adjacent one end using KOH it is each to Anisotropic etch produces a pyramid shape pothole.
5. the method according to claim 11, it is characterized in that, between the lower surface of described coating and the upper surface of substrate Away from that is, both are not in contact and minimum distance is 1 micron.
6. according to the method for claim 3, it is characterized in that, methods described specifically includes：
1) in silicon chip surface with the cantilever beam profile of reactive ion etching process etching off conventional probe, in this profile adjacent one end profit A pyramid shape pothole is produced with KOH anisotropic etch；
2) another to take a silicon chip to cover thereon, two silicon chip surface spacing of control are in 1 microns；
3) oxidation growth layer is formed in silicon chip surface with gate oxidation process, edge of cantilever beam reverse mould profile also will be with during this Top layer silicon chip is connected with the oxide layer grown；
4) elementary silicon substrate is removed with halogen gas；
5) needle point and cantilever beam rear part are removed with photo-etching processes, obtains hollow cantilever probe.
CN201711111195.7A 2017-11-13 2017-11-13 Hollow cantilever probe for delivering and extracting micro-nano scale substances Expired - Fee Related CN107879309B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112816739A (en) * 2019-11-18 2021-05-18 中国科学院大连化学物理研究所 Scanning chemical reaction microscopic imaging method and application
CN114082455A (en) * 2021-10-21 2022-02-25 华南理工大学 Recyclable hollow cantilever probe front end loading and cleaning method

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6156215A (en) * 1997-08-26 2000-12-05 Canon Kabushiki Kaisha Method of forming a projection having a micro-aperture, projection formed thereby, probe having such a projection and information processor comprising such a probe
US20040004182A1 (en) * 2000-06-09 2004-01-08 Christine Kranz Sample for simultaneously conducting electro-chemical and topographic near-field microscopy
US20050079711A1 (en) * 2003-10-10 2005-04-14 Cabot Microelectronics Corp. Hollow tip array with nanometer size openings and formation thereof
US20070151989A1 (en) * 2003-03-19 2007-07-05 Espinosa Horacio D Nanotipped device and method
US20080302960A1 (en) * 2007-05-11 2008-12-11 Andre Meister Probe arrangement
CN101854870A (en) * 2007-10-08 2010-10-06 奥赛路斯有限公司 Needleless device for delivery of an agent through a biological barrier
CN102565460A (en) * 2010-12-17 2012-07-11 彭倍 Continuous direct-writing nano particle solution scanning probe and manufacturing method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6156215A (en) * 1997-08-26 2000-12-05 Canon Kabushiki Kaisha Method of forming a projection having a micro-aperture, projection formed thereby, probe having such a projection and information processor comprising such a probe
US20040004182A1 (en) * 2000-06-09 2004-01-08 Christine Kranz Sample for simultaneously conducting electro-chemical and topographic near-field microscopy
US20070151989A1 (en) * 2003-03-19 2007-07-05 Espinosa Horacio D Nanotipped device and method
US20050079711A1 (en) * 2003-10-10 2005-04-14 Cabot Microelectronics Corp. Hollow tip array with nanometer size openings and formation thereof
US20080302960A1 (en) * 2007-05-11 2008-12-11 Andre Meister Probe arrangement
CN101854870A (en) * 2007-10-08 2010-10-06 奥赛路斯有限公司 Needleless device for delivery of an agent through a biological barrier
CN102565460A (en) * 2010-12-17 2012-07-11 彭倍 Continuous direct-writing nano particle solution scanning probe and manufacturing method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112816739A (en) * 2019-11-18 2021-05-18 中国科学院大连化学物理研究所 Scanning chemical reaction microscopic imaging method and application
CN114082455A (en) * 2021-10-21 2022-02-25 华南理工大学 Recyclable hollow cantilever probe front end loading and cleaning method

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