CN103267874B - The automatic control system for liquid level of atomic force microscope liquid phase imaging - Google Patents

The automatic control system for liquid level of atomic force microscope liquid phase imaging Download PDF

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Publication number
CN103267874B
CN103267874B CN201310179036.6A CN201310179036A CN103267874B CN 103267874 B CN103267874 B CN 103267874B CN 201310179036 A CN201310179036 A CN 201310179036A CN 103267874 B CN103267874 B CN 103267874B
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China
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liquid
micro
pusher
sensing head
contact
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CN201310179036.6A
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CN103267874A (en
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林冬冬
吴珊
沈学
王兰兰
杨新菊
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Fudan University
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Fudan University
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Abstract

The invention belongs to technical field of automatic control, be specially the automatic control system for liquid level of a kind of atomic force microscope liquid phase imaging.System comprises micro sensing head, signal processing circuit, micro liquid pusher; Wherein: micro sensing head suspension by the scan-probe of system, and is connected with signal processing circuit board by wire; Signal that micro sensing head detects by signal processing circuit board amplifies and conversion, and changes into the signal that micro liquid pusher can identify; Be connected by tiny flexible pipe between micro liquid pusher with the liquid injection port on needle point frame, this pusher promotes micro syringe by step motor and controls.Present system can by the propelling movement amount of setting micro liquid pusher and the liquid capacity pushed in the next accurate gated sweep cavity of speed, to ensure that the concentration of solution remains relative constant with the height of liquid level, and pole steady function of injecting slowly can be realized.

Description

The automatic control system for liquid level of atomic force microscope liquid phase imaging
Technical field
The invention belongs to technical field of automatic control, be specifically related to a kind of miniature detecting liquid level and make-up system.
Background technology
The appearance of atomic force microscope makes people become convenient for the material under nano-scale yardstick and fast, relative to scanning electron microscope, atomic force microscope has many advantages.Atomic force microscope can provide real three-dimension surface, atomic force microscope needs to carry out special process to sample unlike scanning electron microscope simultaneously, such as gold-platedly guarantee that sample surfaces has electric conductivity, such process can cause irreversible damage to sample.Secondly, under atomic force microscope does not need to be run at high vacuum condition, it in atmospheric conditions even can works fine under liquid phase environment.Just because of the work that atomic force microscope can be stable under liquid-phase condition, therefore can be used for studying biomacromolecule, the biological tissue even lived.
But, when utilizing atomic force microscope to carry out liquid phase scanning, we find, because the volume scanning cavity is very little, add that instrument is originally in constantly producing heat, cause being scanned liquid to be over regard to evaporation within a few hours, thus interrupted the scanning of atomic force microscope to sample, so just hinder atomic force microscope continues following function for a long time performance to biological sample.Therefore, a kind of detection device for supplying is in real time had to be the key of dealing with problems, the open atomic force microscope liquid cell (CN201034908Y) that can work long hours describes a kind of method and carrys out supply, but there is a lot of defect in its equipment, such as still need people for adding liquid, large liquid cell very wastes detected solution, can not last very long etc.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the invention provides a kind of atomic force microscope liquid phase level automatic control system, to solve the atomic force microscope shortcoming that continuous working period is not grown under liquid phase mode, and realize following object: (1) makes to be scanned liquid level constant on a height, ensures the normal work of microscope under liquid phase; (2) make detected solution concentration keep relatively meticulous constant, evaporate how much water (liquid) is then supply how much water (liquid); (3) realize Intelligent Measurement and Based Intelligent Control, do not need artificial filling.
The technical solution adopted in the present invention is: carry out corresponding liquid supply by the lifting situation detecting liquid level, system comprises micro sensing head, signal processing circuit, micro liquid pusher (as binary channels push-and-pull syringe pump LSP01-1C, being purchased from Baoding LanGe constant flow pump Co., Ltd).The cavity space of placing sample due to atomic force microscope is very little, be unable to hold integrated sensor ready-made on market, the present invention adopts homemade micro sensing head, (Multimode V AFM carries the needle point frame placed the cavity of sample from atomic force microscope, be purchased from Brooker company of the U.S.) top wear come, micro sensing head suspension is on the scan-probe side of system, the contact of micro sensing head is that forked is close to needle point frame upper surface, to increase test surface, the contact of micro sensing head exposes, from needle point frame upper surface distance 0.5-2.0mm (can regulating voluntarily according to the height controlling liquid level).This micro sensing head as the positive pole connected, and scribbles anticorrosive coat, and corresponding negative pole is connected with the small iron plate be arranged on following substrate.Micro sensing head, by positive wire and cathode conductor, is connected with signal processing circuit.
In the present invention, described signal processing circuit, the signal detected by micro sensing head amplifies and conversion, and changes into the signal that micro liquid pusher can identify.
Be connected by tiny flexible pipe between micro liquid pusher with the liquid injection port on needle point frame; Micro liquid pusher promotes micro syringe (KDL1.0ml) by step motor and controls.
In the present invention, described micro sensing head, draw wire by contact and two and form, the copper cash that contact is 0.8mm by commercially available diameter is starting material, has one deck nickel as anticorrosive coat at copper line surface evaporation.Described extraction two wires are wound in one mutually, hole is stretched into from top to bottom through the sensor contact on needle point frame, separate two wire heads again, and folding is close to needle point frame upper surface at an angle of 90, and (two wires are 70 ° of distributions, length is 5mm), finally two wire heads separated are rolled over vertically downward 90 ° and occur that a length is the sagging contact of 0.5-2.0mm, contact glue is fixed on needle point frame; Draw wire directly purchased from OMEGAENGINEERING company, diameter is the thin fine copper wire of the tape insulation protective seam of 0.1mm.Wire welds with contact scolding tin, for being connected to signal processing circuit board.
Native system have employed the working method that negative edge triggers, namely when liquid level declines, owing to losing liquid as conducting medium, and make the iron plate on suspension upper end branch type micro sensing head in a liquid and substrate occur opening a way, thus on current potential, there is a negative edge, this negative edge signal is adjusted by signal processing circuit and exports to micro liquid pusher after amplifying, and triggers micro liquid pusher and carries out fluid injection by tubule toward scanning cavity; When liquid constantly injects scanning cavity, make liquid level increase when encountering again upper end branch type micro sensing contact, the iron plate conducting again on this branch type contact and substrate, there is rising edge in circuit, turns back to high level, thus micro liquid pusher is quit work; Circulation like this, makes the amount of liquid of scanning cavity fluctuate in a less scope always, thus realizes the substantially constant state keeping surface sweeping liquid level.
Compared with prior art, the invention has the beneficial effects as follows the automatic detection of the system of achieving and automatic makeup function, the liquid capacity in accurate gated sweep cavity can be carried out by the propelling movement amount and propelling movement speed controlling micro liquid pusher.The fluid preservation of native system institute supply, in the needle tubing of micro liquid pusher, evaporates how many supplies how many, so can realize the function economized on resources.
Accompanying drawing explanation
Fig. 1 is the planimetric map of atomic-force microscope needle-tip frame.
Fig. 2 is four parts of composed atom force microscope liquid phase scanning cavity.
Fig. 3 is system cloud gray model process flow diagram.
Number in the figure: 1 micro sensing head, 2 liquid filling orifices, 3 fixed grooves+ground connection, 4 pressure electrode, 5 rubber band standing grooves, 6 needle point folders, 7 liquid injection ports; 8 needle point framves, 9 rubber bands, 10 substrates, 11 sensor contact stretch into hole, 12 first wires, 13 second wires, the iron plate of 14 band the second wires; The circuit board of 15 signal processing circuits; 16 micro liquid pushers.
Embodiment
Below in conjunction with accompanying drawing, the present invention is further described.
Needle point frame 8 is fixed on microscope by two fixed grooves 3 of lower surface and the pressure electrode 4 of upper surface, rubber band standing groove 5 overlaps rubber band 9, be used as the sidewall of scanning cavity, together constitute with the iron plate 14 of band second wire (i.e. cathode conductor) cylindrical chamber that is compared sealing.Liquid is entered in cavity by liquid injection port 7 and liquid filling orifice 2.Scan-probe is then clipped on needle point folder 6, and micro sensing head 1 stretches into hole 11 by sensor contact and is suspended on scan-probe side simultaneously, and micro sensing head is connected with signal processing circuit board with the second wire 13 by the first wire (i.e. positive wire) 12.System initial state is for being full of liquid in scanning cavity, and scan-probe is immersed in liquid completely, and micro sensing head 1 also soaks in a liquid simultaneously, because liquid is as conducting medium, makes the iron plate on upper surface branch type contact and substrate be in open-circuit condition.Along with the increase of time, in cavity liquid level due to the factors such as evaporation start decline, when dropping to branch type contact and exposing liquid level, contact changes off state into, now circuit produces the negative edge of an electric signal, after being processed by control circuit board 15, trigger micro liquid pusher 16 and start working.Tiny flexible pipe is had to be connected between pusher 16 with the liquid injection port 7 on needle point frame 8, liquid injects by the propelling movement speed set and propelling movement amount, when being constantly slowly injected into liquid level and flooding micro sensing head 1 again, two contacts start conducting, circuit produces the rising edge of an electric signal, trigger pusher to stop injecting, process such as Fig. 3 constantly circulates, thus reaches the object of design.

Claims (2)

1. an automatic control system for liquid level for atomic force microscope liquid phase imaging, is characterized in that system comprises micro sensing head, signal processing circuit, micro liquid pusher; Wherein:
Described micro sensing head is drawn wire by contact and two and is formed, place from atomic force microscope above the needle point frame the cavity of sample and wear, micro sensing head suspension is on the scan-probe side of system, described two extraction wires are wound in one mutually, hole is stretched into from top to bottom through the sensor contact on needle point frame, separate two wire heads again, folding is close to needle point frame upper surface at an angle of 90, two wire heads separated roll over the sagging described contact that 90 ° of one-tenth length is 0.5-2.0mm vertically downward, and contact glue is fixed on needle point frame; Draw wire scolding tin to weld, for being connected to signal processing circuit board; The contact of micro sensing head is that forked is close to needle point frame upper surface, to increase test surface, described contact is the copper cash of diameter 0.8mm, one deck nickel is had as anticorrosive coat at copper line surface evaporation, the contact of micro sensing head exposes, from needle point frame upper surface distance 0.5-2.0mm, as the positive pole connected, and scribble anticorrosive coat, corresponding negative pole is connected with the iron plate be arranged on following substrate; Micro sensing head, by positive wire and cathode conductor, is connected with signal processing circuit;
Described signal processing circuit, the signal detected by micro sensing head amplifies and conversion, and changes into the signal that micro liquid pusher can identify;
Described micro liquid pusher is connected by tiny flexible pipe with between the liquid injection port on needle point frame; This micro liquid pusher promotes micro syringe by step motor and controls.
2. the control method of the automatic control system for liquid level of an atomic force microscope liquid phase as claimed in claim 1 imaging, it is characterized in that concrete steps are: when liquid level declines, owing to losing liquid as conducting medium, and make the iron plate on suspension upper end branch type micro sensing head in a liquid and substrate occur opening a way, thus on current potential, there is a negative edge, this negative edge signal is adjusted by signal processing circuit and exports to micro liquid pusher after amplifying, and triggers micro liquid pusher and carries out fluid injection by tubule toward scanning cavity; When liquid constantly injects scanning cavity, make liquid level increase when encountering again upper end branch type micro sensing contact, the iron plate conducting again on this branch type contact and substrate, there is rising edge in circuit, turns back to high level, thus micro liquid pusher is quit work; Circulation like this, makes the amount of liquid of scanning cavity fluctuate in a less scope always, thus realizes the substantially constant state keeping scanning liquid level.
CN201310179036.6A 2013-05-15 2013-05-15 The automatic control system for liquid level of atomic force microscope liquid phase imaging Expired - Fee Related CN103267874B (en)

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CN110082014B (en) * 2013-12-07 2021-08-03 布鲁克公司 Atomic force microscope with probe for interacting with a sample
CN106381264B (en) * 2016-11-25 2018-09-07 哈尔滨工业大学 The a wide range of automatic positioning method of micropipette pipe needle point in the micro-injection system of robot assisted

Citations (2)

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CN1339728A (en) * 2001-07-08 2002-03-13 黄武源 Electrode type digital liquid level controlling device
US7823447B2 (en) * 2007-09-17 2010-11-02 Perkinelmer Las, Inc. Method and apparatus for sensing a liquid level

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US7260980B2 (en) * 2003-03-11 2007-08-28 Adams Jesse D Liquid cell and passivated probe for atomic force microscopy and chemical sensing

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CN1339728A (en) * 2001-07-08 2002-03-13 黄武源 Electrode type digital liquid level controlling device
US7823447B2 (en) * 2007-09-17 2010-11-02 Perkinelmer Las, Inc. Method and apparatus for sensing a liquid level

Non-Patent Citations (1)

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