EP2937892A1 - Dispositif de génération de jet et procédé de production d'un jet de liquide - Google Patents

Dispositif de génération de jet et procédé de production d'un jet de liquide Download PDF

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Publication number
EP2937892A1
EP2937892A1 EP15001082.5A EP15001082A EP2937892A1 EP 2937892 A1 EP2937892 A1 EP 2937892A1 EP 15001082 A EP15001082 A EP 15001082A EP 2937892 A1 EP2937892 A1 EP 2937892A1
Authority
EP
European Patent Office
Prior art keywords
liquid
jet
collecting vessel
pump
vacuum chamber
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.)
Withdrawn
Application number
EP15001082.5A
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German (de)
English (en)
Inventor
Manfred Faubel
Stephan Figul
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.)
Microliquids GmbH
Original Assignee
Microliquids 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 Microliquids GmbH filed Critical Microliquids GmbH
Publication of EP2937892A1 publication Critical patent/EP2937892A1/fr
Withdrawn legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B9/00—Spraying apparatus for discharge of liquids or other fluent material, without essentially mixing with gas or vapour
    • B05B9/002—Spraying apparatus for discharge of liquids or other fluent material, without essentially mixing with gas or vapour incorporating means for heating or cooling, e.g. the material to be sprayed
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05G—X-RAY TECHNIQUE
    • H05G2/00—Apparatus or processes specially adapted for producing X-rays, not involving X-ray tubes, e.g. involving generation of a plasma
    • H05G2/001—X-ray radiation generated from plasma
    • H05G2/003—X-ray radiation generated from plasma being produced from a liquid or gas
    • H05G2/006—X-ray radiation generated from plasma being produced from a liquid or gas details of the ejection system, e.g. constructional details of the nozzle
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B14/00—Arrangements for collecting, re-using or eliminating excess spraying material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B9/00—Spraying apparatus for discharge of liquids or other fluent material, without essentially mixing with gas or vapour
    • B05B9/03—Spraying apparatus for discharge of liquids or other fluent material, without essentially mixing with gas or vapour characterised by means for supplying liquid or other fluent material
    • B05B9/04—Spraying apparatus for discharge of liquids or other fluent material, without essentially mixing with gas or vapour characterised by means for supplying liquid or other fluent material with pressurised or compressible container; with pump
    • B05B9/0403—Spraying apparatus for discharge of liquids or other fluent material, without essentially mixing with gas or vapour characterised by means for supplying liquid or other fluent material with pressurised or compressible container; with pump with pumps for liquids or other fluent material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B9/00—Spraying apparatus for discharge of liquids or other fluent material, without essentially mixing with gas or vapour
    • B05B9/03—Spraying apparatus for discharge of liquids or other fluent material, without essentially mixing with gas or vapour characterised by means for supplying liquid or other fluent material
    • B05B9/04—Spraying apparatus for discharge of liquids or other fluent material, without essentially mixing with gas or vapour characterised by means for supplying liquid or other fluent material with pressurised or compressible container; with pump
    • B05B9/0403—Spraying apparatus for discharge of liquids or other fluent material, without essentially mixing with gas or vapour characterised by means for supplying liquid or other fluent material with pressurised or compressible container; with pump with pumps for liquids or other fluent material
    • B05B9/042—Spraying apparatus for discharge of liquids or other fluent material, without essentially mixing with gas or vapour characterised by means for supplying liquid or other fluent material with pressurised or compressible container; with pump with pumps for liquids or other fluent material with peristaltic pumps
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2235/00—X-ray tubes
    • H01J2235/08—Targets (anodes) and X-ray converters
    • H01J2235/081—Target material
    • H01J2235/082—Fluids, e.g. liquids, gases
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
    • H01J49/0431—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for liquid samples
    • H01J49/0445—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for liquid samples with means for introducing as a spray, a jet or an aerosol

Definitions

  • the invention relates to a jet generating device, which is adapted to generate a liquid jet in a vacuum environment, in particular a jet generating device for providing a target material in the form of a continuous or intermittent liquid jet, for. B. for an interaction with an electromagnetic radiation, in particular laser or X-ray radiation, or a particle irradiation. Furthermore, the invention relates to a method for generating a liquid jet, in particular with said jet generating device. Applications of the invention are in particular given in the irradiation of liquids with electromagnetic radiation or with particle radiation, for example for the examination of samples or for the generation of short-wave radiation.
  • laminar liquid jets As the target material, e.g., in mass spectrometry ([1]), the photoelectron spectroscopy ([2]) or the nanolithography ([3]), exposure to lasers and / or other beam sources for photons, X-rays or particle beams.
  • mass spectrometry [1]
  • photoelectron spectroscopy [2]
  • nanolithography [3]
  • lasers and / or other beam sources for photons, X-rays or particle beams.
  • As a liquid not only at room temperature liquid substances such as water or ethanol, but also liquefied metals or gases can be used.
  • the irradiation can hit Rayleigh's disintegration point of the liquid jet into beam segments or into a droplet sequence on the liquid before ([4]) or after ([5]).
  • the liquid jets have a diameter of 0.002 mm to 0.2 mm and flow rates of up to several hundred meters per second. If lower layer thicknesses of the target material are desired, layer-shaped flow structures [6] can be produced with the aid of two collimated primary beams converging at an angle [6], which have a local minimum of the radius of curvature at least at the location of the irradiation.
  • the object of the invention is to provide an improved jet generating device and an improved method for producing a liquid jet, with which disadvantages and limitations of conventional techniques are avoided.
  • the beam generation is intended to enable continuous operation of the jet generating device without interrupting the vacuum, to enable a simplified construction of the jet generating device and / or to minimize liquid losses.
  • a jet generating apparatus adapted to generate a liquid jet and comprising a vacuum chamber, a nozzle device having at least one nozzle, a liquid supply device having a liquid reservoir and a first pump, and a collecting device comprising a collecting vessel having an inlet opening which is arranged to catch the liquid jet in the vacuum chamber.
  • the at least one nozzle opens into the vacuum chamber.
  • the liquid supply device is connected via at least one supply line to the at least one nozzle of the nozzle device, so that during operation of the first pump, the liquid is introduced via the at least one nozzle in the vacuum chamber and the liquid jet is generated.
  • a high-pressure pump such as an HPLC pump
  • the jet generating device includes a recovery device arranged for recovering the liquid collected in the collecting vessel.
  • the recovery device comprises a second pump, with which the liquid from the collecting vessel directly in the liquid supply device, in particular in the liquid reservoir, can be conveyed.
  • a return line is provided, which contains the second pump.
  • a method of generating a liquid jet preferably with the jet producing device according to the first aspect of the invention, wherein the liquid is supplied from the liquid supply means to the nozzle means, the liquid exiting the at least one nozzle in the vacuum chamber and forms the liquid jet, in particular a laminar and / or a layered liquid jet, the liquid jet is received in the collecting vessel and the liquid received is subjected to a recovery.
  • the recovery comprises a transport of the received liquid from the collecting vessel via the second pump directly into the liquid supply device.
  • the liquid with the liquid supply device is again supplied to the nozzle device.
  • a circuit is provided with the invention, which allows a return of the collected liquid to the nozzle device during operation without interruption of the vacuum. Fluid losses are almost eliminated, since a possible backflow of liquid vapor from the collecting vessel into the vacuum chamber is negligible compared to the liquid flow through the second pump into the liquid supply device.
  • the liquid collected by the collecting vessel also referred to as a liquid trap, is pumped off continuously or with predetermined cycles of operation with the second pump and used to supply jet generation to the nozzle means.
  • a particular advantage of the invention is that a liquid jet, in particular a stratiform flow structure, can be generated continuously from a liquid storage volume that is significantly reduced compared to the volume required in conventional techniques. Preferred applications therefore arise when the liquid is particularly valuable dissolved or suspended Substances, such as biological samples, which are only available in small quantities and / or can only be diluted within certain limits. Advantages therefore arise in particular for analytical investigations in which the liquid with a sample contained therein as target material z.
  • the invention is applicable to various liquids.
  • the liquid comprises water or an aqueous solution.
  • the invention may also be practiced with liquefied substances which are gaseous at room temperature and under normal pressure, or with liquified metals.
  • the second pump of the jet generating device can be chosen in particular depending on the application of the jet generation and the liquid used.
  • the second pump comprises a peristaltic pump (peristaltic pump).
  • peristaltic pump a peristaltic pump
  • An important advantage of the peristaltic pump is that it allows a reliable liquid transport over the pressure difference from the negative pressure in the collecting vessel (pressure below 1 bar) to an increased pressure in the liquid supply device, in particular to normal pressure (air pressure, atmospheric pressure under normal conditions).
  • the peristaltic pump closes against the side lower Pressure tight, so that they can even build a vacuum. Further advantages result in the recovery of liquids containing sensitive sample molecules. With the peristaltic pump only low shear forces are generated, which can not destroy the molecules.
  • a different type of pump may be used, such as. B. a (micro) piston syringe pump or a piezo membrane pump.
  • the second pump in particular the peristaltic pump, with respect to the vertical direction (gravitational direction) at the same height as the liquid reservoir of the liquid supply means or above the liquid reservoir. Normal pressure prevails in the liquid reservoir, so that the liquid conveyed by the second pump can flow freely into the liquid reservoir.
  • the collecting vessel of the collecting device can be arranged completely or partially in the vacuum chamber.
  • an inlet opening of the collecting vessel is arranged in the vacuum chamber.
  • the liquid jet is generated in the vacuum chamber extending in the vertical direction, so that the inlet opening is preferably provided in a lower region, for example at the bottom of the vacuum chamber.
  • the implementation of the invention is not limited to a vertical orientation of the liquid jet. Alternatively, the liquid jet may also be oriented horizontally or otherwise inclined.
  • the inner diameter of the inlet opening in dependence on the outer diameter of the liquid jet chosen so that a backflow of liquid vapor from the collecting vessel is minimized in the vacuum chamber.
  • the inner diameter of the inlet opening is smaller than 10 times, particularly preferably 5 times the outer diameter of the liquid jet.
  • the outer diameter of the liquid jet is determined by the size and arrangement of the at least one nozzle of the nozzle device.
  • the inner diameter of the inlet opening can be selected depending on the size and arrangement of the at least one nozzle.
  • the inlet can z. B. circular, elliptical or rectangular.
  • a backflow of liquid vapor through the inlet opening can be almost completely prevented due to the removal with the recovery device, so that the particular design of the inlet opening, which is described for example in [8], and / or the provision of a cooling device on the collecting vessel can be dispensed with ,
  • the shape of the collecting vessel depending on the specific application of the invention, in particular depending on the space available freely.
  • it has proved to be particularly advantageous if the collecting vessel has a cylindrical shape (pot shape) or a tubular shape.
  • the jet generating device can be operated without cooling the collecting vessel.
  • the collecting vessel is equipped with a heating device.
  • the heating device comprises a heat pipe heating device (so-called "heat pipe”), with which the inlet opening of the collecting vessel is heated.
  • the heating of the inlet opening has the advantage that the risk of freezing of the liquid is avoided in a possible contact with the edge of the inlet opening or other parts of the collecting vessel and thereby resulting interruption of the operation of the jet generating device.
  • a temperature of the collecting vessel in particular in the region of the inlet opening, to a temperature in the range of 0 ° C to 250 ° C, in particular from 20 ° C to 200 ° C, such as from 40 ° C to 150 ° C or 60 ° C to 120 ° C.
  • the heat pipe heating device preferably comprises a tube thermally coupled to the collecting vessel made of a non-magnetic metal, in particular copper, which is flowed through by a heating medium, for example oil or water vapor.
  • a heating medium for example oil or water vapor.
  • the liquid supply means may be equipped with a refill port.
  • the refill port includes a closable opening through which a liquid medium, e.g. As the liquid or a solvent for diluting the liquid can be filled in the liquid reservoir.
  • a liquid medium e.g. As the liquid or a solvent for diluting the liquid
  • the refill port to compensate for any liquid losses during long-term operation of the jet generator device and / or to vary the liquid circulating in the jet generator device (for example dilution or solvent change).
  • the liquid jet is generated in a vacuum environment with a negative pressure relative to the normal pressure.
  • the vacuum chamber is preferably a pressure of less than or equal to 100 mbar, more preferably less than or equal to 10 mbar, such as given less than 6 mbar.
  • this is equipped with at least one vacuum pump, for example at least one turbomolecular pump and / or at least one cryopump, wherein preferably pressures of approx. 10 -5 mbar can be achieved.
  • the nozzle device of the jet generating device according to the invention preferably has a single nozzle, with which the liquid jet is produced, or a combination of two nozzles, with which two primary rays colliding with a laminar flow structure are produced, as is known for example from [6].
  • a single liquid jet in the vertical direction typically with a circular cross-section and a diameter smaller than 2 mm, preferably smaller than 0.5 mm, more preferably smaller than 0.1 mm, such as 0.01 mm to 0 , 1 mm, generated.
  • the primary beams are preferably generated at an angle ⁇ selected in the range of 1 ° to 179 °, preferably 10 ° to 150 °, more preferably 15 ° to 120 °, such as 20 ° to 90 °.
  • the diameter of the primary jets is preferably in the range of 0.01 mm to 0.5 mm, particularly preferably 0.05 mm to 0.4 mm, for example 0.02 mm to 0.3 mm or 0.03 mm to 0.1 mm selected.
  • the diameter of the liquid jet may be less than 2 mm, preferably less than 0.5 mm, more preferably less than 0.1 mm, such as 0.01 mm to 0.1 mm.
  • the nozzles of the nozzle device and the inlet opening of the collecting vessel are arranged so that the inlet opening is located at the location of the constriction of the liquid jet.
  • Another important advantage of the invention is that in the liquid reservoir in comparison to the pressure in the vacuum chamber increased pressure, preferably atmospheric pressure under normal conditions, is given. This simplifies the transport of the liquid into the liquid reservoir and the provision of the liquid at the nozzle device.
  • the jet-generating device is preferably equipped with an irradiation device.
  • the irradiation device comprises, for example, an X-ray source, a laser source or an electron beam source.
  • the electromagnetic Radiation or particle radiation can be generated in the vacuum chamber and fed directly to the liquid jet.
  • an injection of electromagnetic radiation from a source located outside the vacuum chamber may be provided in the interior of the vacuum chamber.
  • FIG. 1 is a schematic illustration illustrating in particular features of the recovery device.
  • the specific embodiment of the jet-generating device can be selected by the person skilled in the art depending on the specific application of the invention, as is known, for example, from conventional techniques.
  • the jet-generating device 100 comprises the vacuum chamber 10, the nozzle device 20, the liquid supply device 30, the catcher 40 and the recovery device 50.
  • an irradiation device 200 and a detector device 210 which are used for the preferred applications of the invention Beam generating device 100 may be coupled.
  • the beam generating device 100 is equipped with a control device and a sensor device (not shown) to monitor the beam generation and the recovery with sensors and control operating parameters of the beam generating device and optionally the irradiation device 200 and the detector device 210.
  • the vacuum chamber 10 is, for example, a stainless steel recipient equipped with a vacuum pump (not shown) and a coupling window 11, for example for coupling in laser radiation.
  • the vacuum chamber 10 is designed for an operating pressure, for example, below 10 mbar.
  • the nozzle device 20 comprises two nozzles 21, 22, which open into the vacuum chamber 10.
  • the nozzles 21, 22 are connected to the liquid supply device 30 via high-pressure connection lines 23.
  • Each of the nozzles 21, 22 has an axial jet direction.
  • the nozzles 21, 22 are arranged so that the primary beams 1.1, 1.2 form the same angle with the vertical direction and collide at an angle ⁇ .
  • the liquid jet 1 is formed, which in a plane perpendicular to the plane defined by the primary beams 1.1, 1.2 plane as a planar flow structure 2 (see schematic plan view perpendicular to the plane in the inserted field of FIG. 1 ).
  • the flow structure 2 forms a portion of the liquid jet 1 with a minimum radius of curvature, which is designed for a particularly effective irradiation 3 with the irradiation device 200.
  • the liquid supply device 30 comprises a storage vessel 31, which is connected to the first pump 32 (high-pressure pump). With the first pump 32, the liquid can be pumped from the storage vessel 31 via the high-pressure connection lines 23 to the nozzles 21, 22.
  • the first pump 32 comprises, for example, an HPLC pump designed to generate a working pressure in the high-pressure connecting lines 23 of up to 50 MPa.
  • the liquid supply device 30 comprises a refill port 33, via which liquid medium, for example the liquid for producing the liquid jet 1, additional sample substance and / or another solvent can be introduced into the storage vessel 31. Since normal pressure prevails in the liquid feed device 30, in particular in the storage vessel 31, the refill port 33 may comprise a simple, closable line coupling.
  • the collecting device 40 comprises the collecting vessel 41 with the inlet opening 42 and the heat pipe heating device 43.
  • the collecting vessel 41 has, for example, the shape of a hollow cylinder with a frustoconical lid whose open upper side forms the inlet opening 42.
  • the collecting vessel 41 is arranged completely or partially in the vacuum chamber 10, wherein at least the inlet opening 42 is positioned inside the vacuum chamber 10.
  • the inlet opening 42 with a diameter D A of 0.05 mm to 0.7 mm is located in the extended beam direction of the liquid jet 1 at a position at which the flow structure 2 has a constriction.
  • the liquid jet 1 at the position of the inlet opening 42 has its minimum diameter D S , which corresponds to 1.5 times the diameter of the primary rays, which for primary rays of 0.01 mm to 0.1 mm values between 0.015 mm and 0, 15 mm results, so that the inner diameter of the inlet opening 42 can be minimized.
  • D S minimum diameter
  • the collecting vessel 41 a pressure above 6 mbar is given.
  • the collecting vessel 41 is made of a non-magnetic material, for example of copper, titanium, a plastic, in particular a thermally stable plastic, or ceramic.
  • the heat pipe heater 43 includes a heat pipe circuit and a heating source.
  • the heat pipe circuit is formed for example by copper tubes, which are firmly connected to the wall of the collecting vessel 41, preferably in the vicinity of the inlet opening 42.
  • As the heating means for example, an oil is used.
  • the recovery device 50 comprises a return line 51, which connects the collecting vessel 41 with the storage vessel 31.
  • the return line 51 contains the second pump 52, with the liquid from the collecting vessel 41 is transported into the storage vessel 31.
  • a peristaltic pump 42 of the type MAXIFLOW manufactured by MAXIFLOW (manufacturer: Lambda Instruments) is used.
  • a tubular collecting vessel 41 A (shown in dashed lines) may be provided, which is connected directly to the return line 51.
  • the collecting device 40 and the recovery device 50 are a common assembly comprising a flexible hose or pipe extending from the vacuum chamber 10 to the liquid supply means 30, in particular into the liquid reservoir 31 and into the outside of the vacuum chamber 10 the second Pump 52 is integrated.
  • the mouth of the tube or pipe on the side of the vacuum chamber 10 forms the inlet opening 42 for receiving the liquid jet 1.
  • the collected liquid is pumped through the hose or pipe via the second pump 52 directly into the storage vessel 31.
  • the beam generating device 100 is designed for photoelectron spectroscopy studies on aqueous solutions of a biological sample.
  • the aqueous solution of the biological sample forms the liquid for generating the liquid jet 1.
  • the irradiation device 200 comprises a laser source whose radiation is coupled through the coupling window 11 into the vacuum chamber 10 and directed onto the flow structure 2 of the liquid jet 1. With the detector device 210, the induced photoelectrons are detected and evaluated in a conventional manner.
  • the liquid jet 1 is collected during operation of the jet generating device with the collecting vessel 41 and pumped via the return line 51 by means of the second pump 52 continuously or intermittently in the liquid reservoir 31, from which the liquid with the first pump 32 via the high pressure connecting lines 23 again Generation of the liquid jet 1 to the nozzles 21, 22 is performed.

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  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Optics & Photonics (AREA)
  • Plasma & Fusion (AREA)
  • Jet Pumps And Other Pumps (AREA)
  • X-Ray Techniques (AREA)
EP15001082.5A 2014-04-25 2015-04-15 Dispositif de génération de jet et procédé de production d'un jet de liquide Withdrawn EP2937892A1 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE102014006063.2A DE102014006063A1 (de) 2014-04-25 2014-04-25 Strahlerzeugungsvorrichtung und Verfahren zur Erzeugung eines Flüssigkeitsstrahls

Publications (1)

Publication Number Publication Date
EP2937892A1 true EP2937892A1 (fr) 2015-10-28

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US (1) US20150306620A1 (fr)
EP (1) EP2937892A1 (fr)
DE (1) DE102014006063A1 (fr)

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CN109530119A (zh) * 2018-11-01 2019-03-29 河南中南工业有限责任公司 一种粘合剂喷涂装置及方法
EP3736445A1 (fr) * 2019-05-09 2020-11-11 Excillum AB Source de rayons x comportant une pompe électromagnétique
CN114354887A (zh) * 2021-12-30 2022-04-15 武汉大学 一种激光-液氮磨料射流联合破岩试验装置

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CN107020214B (zh) * 2016-01-29 2019-03-05 天津亚轩科技有限公司 一种喷漆收集装置
CN108246548B (zh) * 2018-01-16 2019-07-23 广东中恒安检测评价有限公司 一种石油专用管道涂料回收装置
US11272607B2 (en) 2019-11-01 2022-03-08 Kla Corporation Laser produced plasma illuminator with low atomic number cryogenic target
US11259394B2 (en) 2019-11-01 2022-02-22 Kla Corporation Laser produced plasma illuminator with liquid sheet jet target

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