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WO2017168003A1 - Procédé et dispositif pour déterminer les forces d'interaction entre deux corps - Google Patents

Procédé et dispositif pour déterminer les forces d'interaction entre deux corps Download PDF

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Publication number
WO2017168003A1
WO2017168003A1 PCT/EP2017/057788 EP2017057788W WO2017168003A1 WO 2017168003 A1 WO2017168003 A1 WO 2017168003A1 EP 2017057788 W EP2017057788 W EP 2017057788W WO 2017168003 A1 WO2017168003 A1 WO 2017168003A1
Authority
WO
WIPO (PCT)
Prior art keywords
substrate
rotor
bodies
detection
measuring
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/EP2017/057788
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German (de)
English (en)
Inventor
Dietmar Lerche
Uwe Rietz
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Lum GmbH
Original Assignee
Lum GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Lum GmbH filed Critical Lum GmbH
Publication of WO2017168003A1 publication Critical patent/WO2017168003A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N19/00—Investigating materials by mechanical methods
    • G01N19/04—Measuring adhesive force between materials, e.g. of sealing tape, of coating

Definitions

  • the invention relates to a method and apparatus for determining interaction forces between substrates, e.g. Material surfaces, and test bodies, such as particles, cells, agglomerates, which may be solid, deformable or liquid.
  • substrates e.g. Material surfaces
  • test bodies such as particles, cells, agglomerates, which may be solid, deformable or liquid.
  • the method is based on the measurement of the interaction forces by means of analytical centrifugation.
  • the composite "substrate adhering body" is exposed to a defined increasing centrifugal acceleration and automatically and contactlessly detects the failure of the composite by means of a measuring system during the centrifugation
  • the Detektionsvomchtung can be integrated into the rotor, but also be mounted wholly or partially outside the rotor.
  • the loading of the substrates is carried out in the same device as that of the detection of the separation, by separation of the test body to be examined from a liquid or a gas due to gravitational, centrifugal, electrical or magnetic fields.
  • the load can be through the
  • Pipelines, filters, filling units which must be cleaned or kept free of particles at regular intervals due to the adhesion of individual particles with increasing load. For other applications is a modification of
  • the basic physical mechanism is based on the interaction of the individual particles with each other or with a substrate or a surface.
  • the particles adhere to the substrate due to van der Waals and electrostatic
  • a modern approach is the Atomic Force Microscope (AFM) (R.G.
  • the centrifuge method for determining adhesive forces was first used in 1955 by Beams. In this case, applied to a substrate test body of a
  • Test bodies are a polydispersed system in terms of size, geometry, roughness, magnetization, etc.
  • the method is to be designed such that extensive analysis requirements, e.g. several material combinations, can be studied in parallel and the substrate is loaded with one or a plurality of test bodies or interacts.
  • the respective composite "Substrate adherent (r) test body” is a programmable, defined increasing centrifugal Auszudateen and the detachment of the test body or the test body by means of measuring system during centrifugation in-situ without affecting the programmed acceleration change automatically, non-contact and sequential objective standards
  • the critical centrifugal accelerations and the respective peel events are to be correlated to evaluate the interactions and to calculate adhesive forces and their distributions based thereon.
  • Measuring sample (substrate) with one or a plurality of test bodies (eg particles) is carried out in the device, which is used for the determination of the interaction forces, no manipulation of the composite "substrate test body" is necessary and by suitable forces a variable, but defined contact pressure predetermined and can be realized with a variable, defined contact time.
  • Adhesion force measurement to use an analytical centrifuge with a special rotor, which receives devices for the test samples positioned and exposing them by successively increasing the speed of increasing acceleration and thus centrifugal force.
  • in-situ temporal detection of the sequential events of detachment of the test bodies from the substrate is to be ensured by a non-random measuring method.
  • the rotor (FIG. 1) enables the recording of even numbers of 2, 4, 6, 8 devices with measuring cuvettes (FIG. 3).
  • Fig. 2 shows an example of a
  • Section of a rotor for 4 devices with measuring cuvettes is embodiments with odd numbers, e.g. with a device and a corresponding one
  • Particle mass m of 0.014 mg (e.g., rape pollen) and a distance of the test surface r from the center of rotation corresponding to Eq. 1 are determined.
  • Preparative ultracentrifuges allow e.g. Speeds of 100000 rpm (Optima XPN-100, Beckmann Coulter).
  • a special rotor with low mass and high strength and rigidity for the solution of the measuring task is used (see Fig. 1), which can be accelerated or decelerated by means of a motor, controlled by a microcontroller, wherein the time course of Speed (eg incremental increase, linear
  • the rotor is characterized in that the devices (8), the measuring cuvettes (17) with the samples to be analyzed (substrate (15) with adhering body (20) or a plurality of adhering bodies (20)) with the measuring cuvette holder (13) can be recorded stationary and radially aligned.
  • a special feature of the rotor is further that the devices with measuring cuvette (8) without any mechanical fasteners by insertion into recesses in the rotor easily used and
  • Another embodiment of the invention is that the space is provided for receiving the sensor system. Surprisingly, even at high speeds, the populated rotor only produces a low air resistance, which has a very advantageous effect on the necessary engine power, self-heating and noise emission. In addition, concentricity and axial runout are positively influenced and thus measurement artifacts due to vibrations and imbalance are minimized.
  • the rotor attachment (4) on the motor axis (3) is advantageously solved so that a simple replacement of the rotors by means of standard used
  • the rotor is an assembly (6), in which, for example, coded magnet arrangements or RFID chips are integrated, for the
  • Screw connection (9) mechanically fastened.
  • the rotor identification makes it possible to specify maximum speeds individually for the rotor used, to adapt the temperature control behavior of the basic centrifuge, to specify maximum and minimum acceleration and braking ramps for specific rotors and to display these to the user in the PC operating software for programming the analysis procedure.
  • Another feature of the rotor is that by tempering the
  • a particular embodiment of the object according to the invention consists in that a two-part rotor with an upper part (1) and a lower part (2) can be used.
  • the two parts can be screwed (12) or other suitable
  • Construction measures are linked together. This is on the one hand
  • the introduction of force to the rotor is advantageously carried out both on the upper (1) and on the lower part (2) areally via webs.
  • the outer edge of the rotor base is with a
  • Position detection Furthermore, in this outer area there is a bore (7) into which a magnet is fixed, e.g. is glued. The magnet is detected via a Hall sensor and thus a defined starting point for the count of the rotor placed in the
  • An important feature of the invention is the accurate, non-contact determination of the current rotor speed synchronous to the respective determination of adhering to a substrate body or the amount of detached from the substrate and dislocated by the centrifugal body in a radially displaced in the direction of the rotor edge measurement plane.
  • the cut-outs in the rotor edge (11) can be used not only for position detection but also for speed determination via a time measurement (light barrier principle). This method is particularly advantageous for low speeds and the determination of speed changes.
  • Another embodiment of the speed measurement consists in the use of a Hall sensor, which is placed in the outer region of the rotor and generates a pulse during the passage of the magnet (7). By means of time measurement between two pulses, the microcontroller calculates the current speed and transfers it to the PC software. The placement of several magnets increases the sensitivity with respect to speed changes.
  • the devices (13) for the measuring cuvettes (17) which receive and fix the substrates (15) with the test body (s) (20) are designed in a modular design.
  • a device according to the invention consists of a mechanically stable sheath (13), a mechanical support for the measuring cell bottom (13 a), which has a corresponding Beobachtungsöff ung and a clamping device with
  • the measuring cell (17) itself consists of a body in which a cylindrical or other shaped channel (24) worked as a working space for the analysis and recesses on both ends for O-rings (18)
  • the cylindrical measuring cell body can also be displaced by a few degrees.
  • the configuration of the measuring cuvette depends on the environmental conditions required for the adhesion force determination (eg liquid or gas) and the detector principle used.
  • the inventive solution for the determination of the adhesive force in the substrate-liquid system and a detection device for the quantification of the detached test bodies outside the rotor (FIG. 4) will be described.
  • the illumination method both transmitted light and reflected light can be realized. While in incident light, the illumination of the cuvette is done, for example, with a pulsed laser (21) from the detector direction, in transmitted light centrally through the
  • Substrate plate (15) illuminated through.
  • the inventive task was realized by the exposure time over the pulse duration of the light source. For the required times, only the use of a pulsed high-power laser (21) is possible.
  • the camera (22) is left "open" for a short, defined shutter speed: If the measuring surface is in front of the sensor / objective, or in a measuring position required for the measuring task, the laser (21) is controlled synchronously be exposed several times for a recording.
  • the variability of the material for the substrate plate is a very important
  • Criterion determines the number of substrate-particle combinations to be investigated.
  • An optical transparency of the substrate wafer is not required when using reflected light, which enormously increases the variety of substrate materials.
  • the incident light method further enables tilting of the substrate wafer so as to vary the stress profile for a sample during a measurement. Further rotor outer substrate chip segments are subject to higher
  • FIG. 1 shows the rotor in section.
  • FIG. 2 shows a section of the rotor top view.
  • FIG. 3 shows the device with measuring cuvette.
  • FIG. 4 shows the incident light method.
  • FIG. 5 shows the transmitted-light method.
  • FIG. 6 shows a simulation in the static measurement setup using the example of lily pollen.
  • FIG. 7 shows the number of particles determined by the image evaluation software above the rotational speed (lepidocrocite particles (5 ⁇ to 62 ⁇ ) - focus on the detection side).
  • Figure 8 shows the proportion of on the substrate platelet remaining ceramic particles above the speed (ceramic particles (60 ⁇ ) - focus on the substrate side).
  • Embodiment 1 Measurements in the static system
  • FIG. 6 shows the processed images of the samples with particle masses of 1.2 mg (A), 3.2 mg (B) and 5 mg (C). It can be seen that with increasing particle mass, the number of particles increases. In the diagram in Fig. 6, the particle number is plotted against the respective dry mass, as determined by the image evaluation software.
  • the sample material to be examined is first of all provided and optionally dispersed.
  • an optically transparent plate is now placed on the detection side (16), then placed on top a plate with a hole (19) and a hollow screw (10) tightened up.
  • the lateral fixing screw (14) is tightened.
  • the cuvette is then filled with suspension through the perforated plate at the top. Thereafter, the screw is released at the top of the perforated plate again and the substrate plate (15) inserted and then the upper hollow screw is screwed in again, the lateral fixation is no longer released.
  • the seal is made by O-rings (18), which lie in a groove.
  • Exemplary embodiment 3 Carrying out a measurement The devices with measuring cuvettes are inserted into the rotor with the substrate side after rotor outer, then the centrifuge lid is closed. By starting the centrifugation and rotation at a given speed for a fixed time takes a defined
  • Sample conditioning e.g. Pressing particles to the substrate.
  • the centrifuge lid is opened, the device with the measuring cuvette without further manipulation, rotated by 180 ° and used again in the rotor. (Lowering the device for the cuvettes now shows the direction of the rotor outside).
  • the measurement After closing the centrifuge lid, the measurement begins. Centrifugation is performed at a speed ni for a predetermined time, and at the end of this period an image is taken of the measuring cuvette (detection plate) during the rotation. Now it is accelerated to a higher speed n 2 , this held again for a defined time and taken a picture. This procedure is repeated with increasing speed levels up to the maximum speed.
  • the devices including measuring cuvettes are removed from the receiving devices of the rotor, emptied and cleaned.
  • Lepidocrocite particles with diameters in the range of 5 ⁇ to 62 ⁇ in aqueous solution were investigated. The particles were pressed at 2000 rpm for 2 minutes. In the subsequent experiment, the images were taken during the rotation in each case to the end of the constant held speed levels, it has been focused on the detection side. In Fig. 7 are determined by the image evaluation software
  • Substrate platelets can affect the forces at which the particles will peel off.
  • Exemplary Embodiment 5 Measurements in the Rotating System - Focus on Substrate Platelets Ceramic particles having a diameter of approximately 60 ⁇ m in aqueous solution were used for these measurements. The images were taken again during the rotation, but this time it was focused through the aqueous medium onto the substrate side. Fig. 8 shows the proportion of remaining on the substrate plate

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Centrifugal Separators (AREA)

Abstract

La présente invention concerne un procédé et des dispositifs pour déterminer les forces d'interaction entre des substrats, par exemple des surfaces de matériau, et des corps à tester, par exemple des particules, des cellules ou des agglomérats pouvant être solides, déformables ou liquides. Selon l'invention, la mesure des forces d'interaction s'effectue par centrifugation analytique. Le composite "corps adhérant au substrat" est soumis à une accélération centrifuge progressive définie et détecte automatiquement et sans contact les défauts du composite durant la centrifugation au moyen d'un système de détection. Selon l'invention, cela est réalisé et quantifié soit directement par la réduction dans le temps de la quantité (du nombre) de corps adhérant au substrat, soit par l'augmentation des corps décollés dans une position radialement plus à l'extérieur grâce à un procédé de détection sensible à la quantité. Les dispositifs de détection peuvent être intégrés dans le rotor mais également montés intégralement ou partiellement à l'extérieur du rotor. Dans le cas de composites préparés par exemple avec une pluralité de particules présentant des forces d'attraction identiques ou différentes, la répartition des forces dans la masse des particules peut être quantifiée en seulement un essai. La charge des substrats s'effectue dans le même dispositif, tout comme la détection du décollement, en séparant les corps à analyser d'un liquide ou d'un gaz en raison de champs gravitationnels, centrifuges, électriques ou magnétiques. Le degré de charge peut être prédéterminé par la concentration initiale.
PCT/EP2017/057788 2016-03-31 2017-03-31 Procédé et dispositif pour déterminer les forces d'interaction entre deux corps Ceased WO2017168003A1 (fr)

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DE102016205403.1 2016-03-31
DE102016205403 2016-03-31

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102018121222A1 (de) * 2018-08-30 2020-03-05 Deutsches Zentrum für Luft- und Raumfahrt e.V. Verfahren und Vorrichtung zur Ermittlung mechanischer Materialkennwertkurven
CN114755176A (zh) * 2022-04-29 2022-07-15 中国地质大学（武汉） 一种测量水合物与特定介质作用力的装置及方法
CN119223816A (zh) * 2024-09-23 2024-12-31 南京工业大学 基于同步带传动的离心式颗粒表面黏附能测量装置、系统及方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3544093B2 (ja) * 1997-01-23 2004-07-21 株式会社リコー 粉体付着力測定装置および遠心分離式付着力測定方法
US20130130884A1 (en) * 2008-12-02 2013-05-23 President And Fellows Of Harvard College Apparatus for measurement of spinning forces relating to molecules
US20140371047A1 (en) * 2013-06-18 2014-12-18 L.U.M. Gmbh Centrifuge rotor
US9019493B2 (en) 2004-03-05 2015-04-28 L.U.M. Gmbh Method and device for the characterization of multiple samples of one or various dispersions

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3544093B2 (ja) * 1997-01-23 2004-07-21 株式会社リコー 粉体付着力測定装置および遠心分離式付着力測定方法
US9019493B2 (en) 2004-03-05 2015-04-28 L.U.M. Gmbh Method and device for the characterization of multiple samples of one or various dispersions
US20130130884A1 (en) * 2008-12-02 2013-05-23 President And Fellows Of Harvard College Apparatus for measurement of spinning forces relating to molecules
US20140371047A1 (en) * 2013-06-18 2014-12-18 L.U.M. Gmbh Centrifuge rotor

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
R.G. REIFENBERGER: "Fundamentals of Atomic Force Microscopy", 2015, WORLD SCIENTIFIC PUBL., ISBN: 978-981-4630-
SALAZAR-BANDA ET AL: "Determination of the adhesion force between particles and a flat surface, using the centrifuge technique", POWDER TECHNOLOGY, ELSEVIER SEQUOIA, LAUSANNE, CH, vol. 173, no. 2, 24 March 2007 (2007-03-24), pages 107 - 117, XP022000669, ISSN: 0032-5910, DOI: 10.1016/J.POWTEC.2006.12.011 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102018121222A1 (de) * 2018-08-30 2020-03-05 Deutsches Zentrum für Luft- und Raumfahrt e.V. Verfahren und Vorrichtung zur Ermittlung mechanischer Materialkennwertkurven
CN114755176A (zh) * 2022-04-29 2022-07-15 中国地质大学（武汉） 一种测量水合物与特定介质作用力的装置及方法
CN119223816A (zh) * 2024-09-23 2024-12-31 南京工业大学 基于同步带传动的离心式颗粒表面黏附能测量装置、系统及方法

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