WO1997032200A1 - Process for monitoring a disperse system for non-dispersed impurities and device for carrying out said process - Google Patents

Process for monitoring a disperse system for non-dispersed impurities and device for carrying out said process Download PDF

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Publication number
WO1997032200A1
WO1997032200A1 PCT/CH1997/000064 CH9700064W WO9732200A1 WO 1997032200 A1 WO1997032200 A1 WO 1997032200A1 CH 9700064 W CH9700064 W CH 9700064W WO 9732200 A1 WO9732200 A1 WO 9732200A1
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WO
WIPO (PCT)
Prior art keywords
band
impurities
disperse system
detected
control
Prior art date
Application number
PCT/CH1997/000064
Other languages
German (de)
French (fr)
Inventor
Fredi Stucki
Original Assignee
Borealis A/S
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Filing date
Publication date
Application filed by Borealis A/S filed Critical Borealis A/S
Priority to JP9530487A priority Critical patent/JP2000505552A/en
Priority to EP97904326A priority patent/EP0883800A1/en
Priority to AU17156/97A priority patent/AU1715697A/en
Publication of WO1997032200A1 publication Critical patent/WO1997032200A1/en

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
    • G01N23/06—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and measuring the absorption
    • G01N23/18—Investigating the presence of flaws defects or foreign matter
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/92—Measuring, controlling or regulating
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
    • G01N23/06—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and measuring the absorption
    • G01N23/083—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and measuring the absorption the radiation being X-rays
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
    • G01N23/06—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and measuring the absorption
    • G01N23/16—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and measuring the absorption the material being a moving sheet or film
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92009—Measured parameter
    • B29C2948/92228—Content, e.g. percentage of humidity, volatiles, contaminants or degassing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92009—Measured parameter
    • B29C2948/92295—Errors or malfunctioning, e.g. for quality control
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92323—Location or phase of measurement
    • B29C2948/92438—Conveying, transporting or storage of articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/92723—Content, e.g. percentage of humidity, volatiles, contaminants or degassing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/9279—Errors or malfunctioning, e.g. for quality control
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92819—Location or phase of control
    • B29C2948/92933—Conveying, transporting or storage of articles

Definitions

  • the invention is based on a method for monitoring a disperse system for non-dispersed impurities according to the preamble of claim 1.
  • the invention also relates to a device for performing the method.
  • these inhomogeneities are deposited as defects at the boundary layer with the dielectric during the manufacture of the cables, they can significantly distort the electrical field of the cable locally.
  • these impurities can also contain water-soluble ions. So if there is another in the cable If there is unavoidable residual moisture, these ions can diffuse into the cable insulation and significantly reduce the properties of the cable.
  • the invention relates to a prior art as described in an article by A.A. Farkas et al. "High Performance semi-conductive compounds testing, production and experience", Jicable 91, 3rd International Conference on Polymer Insulated Power Cables, pages 8-11, 24-28 June 1991, Paris, France.
  • a method described in this prior art for monitoring a disperse system of conductive carbon black and polyethylene used in a cable as a semiconducting layer for undispersed impurities a part of the disperse system is extruded into a band, the band is examined for impurities, and only afterwards the disperse System processed.
  • the tape contains a lot of soot and is therefore impermeable.
  • only the surface of the belt is examined for undispersed impurities. Impurities inside the belt cannot be detected.
  • the invention is based on the object of developing the method according to the prior art in such a way that it can also detect undispersed impurities present inside the belt with greater certainty, and at the same time specify a device which can be used in is simply suitable for carrying out this method.
  • the method according to the invention is characterized in particular by the fact that it can continuously detect and display the contaminants distributed on the surface and inside the belt. It is particularly advantageous here that the method works independently of the optical properties of the tape and is able to analyze tapes which are also opaque without problems for trapped impurities.
  • the type, number, size, shape and / or distribution of the included impurities can serve as selection criteria for the degree of impurities.
  • the device for carrying out the method according to the invention enables reliable, continuous and / or step-by-step monitoring of the strip and at the same time can control processes in which the disperse system represented by the strip is further processed, for example by extrusion during cable production .
  • FIG. 2 shows an enlargement of an area shown with a border in the device according to FIG. 1, and
  • Sample images of which the upper image relates to a sample that is free of contaminants and the lower image of a sample in which contaminants are stored.
  • 1 denotes a storage kettle, which is used for the intermediate storage of a disperse system.
  • the disperse system is produced by mixing 10 to 50 percent by volume of an electrically conductive or electrically semiconductive powder, such as, in particular, a carbon black with particle sizes smaller than 0.1 ⁇ m, with a polymer, such as, in particular, polyethylene been.
  • the supply boiler can be connected via a controllable switchover valve 2 to an extruder 3 which is used to produce a high or medium voltage cable.
  • the storage boiler 1 is fed by a transport line 4. A small part of the disperse system led through the transport line 4 is continuously discharged through a by-pass line 5 and fed to a test extruder 6.
  • the test extruder 6 produces a test tape 7 of typically 0.2 to 1 mm thick and typically 10 mm bandwidth from the branched-off part of the disperse system. This test tape is opaque since it contains soot in a finely divided form and in a high concentration.
  • the test tape 7 is fed to a measuring head 8 of a device 9 for monitoring the test tape 7 (and thus also the disperse system) for undispersed impurities.
  • the output of the sensor 8 is connected to an evaluation and control device 10.
  • a signal output 11 of the evaluation and control device 10 acts on the controllable changeover valve 2.
  • the transducer 8 has a radiation-protected housing 12 with two narrow openings on the opposite sides of the housing for the passage of the band 7. Each is arranged in the housing 12 on opposite sides of the band a tube 13 for generating soft X-rays (operating voltage of the X-ray tube 13 between 1 and 50 kV) and an X-ray-sensitive image recognition device 14 with a raster 15, a computer-controlled (CCD) camera or a film.
  • X-ray-sensitive image recognition device 14 with a raster 15, a computer-controlled (CCD) camera or a film.
  • Information about the type, the number, the size, the shape and / or the distribution of undesirable impurities inside and on the surface of the test tape 7 and therefore also in the disperse system for further processing in the storage kettle 1 are determined by the measuring sensor 8 and this information is passed on to the evaluation and control device 10.
  • areas of the test tape 7 of, for example, 1 cm 2 are irradiated transversely to the tape plane with soft X-ray radiation.
  • the radiation emerging from the strip can be detected step by step, for example with a film, or else continuously, for example with the raster 15 or a CCD camera.
  • the radiation emerging from the irradiated areas is more strongly absorbed by an impurity 16, typically originating from a grain of sand or another inorganic particle, than at the impurity-free, remaining part of the irradiated band area, which predominantly contains organic substances.
  • a silhouette 17 is therefore generated on the grid 15.
  • the silhouette 17 is detected by adjacent raster points - as indicated in the figure, for example by 2 raster points - and this information is forwarded to the evaluation and control device 10 in the form of electrical signals.
  • all impurities present on the surface and inside the test tape 7 can be detected with a resolution higher than 10 ⁇ m.
  • the supplied electrical signals can be compared with reference signals in the evaluation and control device 10. When a threshold value is exceeded, the evaluation and control device 10 then emits a negative status signal that characterizes the contamination state of the belt 7. This negative status signal is fed via the signal output 11 to a control or regulating element of a device which further processes the disperse system, such as, in particular, the changeover valve 2, and then causes it to be actuated, such as in particular closing the connection to the extruder 3.
  • output signals are advantageously formed in the control and evaluation device 10, which are proportional to the type, number, size, shape and / or distribution of the contaminants. These signals can be extremely valuable when looking for sources of error and at the same time enable particularly simple input of the reference signals requested for the threshold value comparison.
  • the upper picture relates to an area of the test tape 7 which is free of impurities.
  • the diffuse spots of low contrast and typically 60 ⁇ m in diameter that can be seen in the picture come from soot agglomerates.
  • the lower image relates to an area of the test tape 7 in which coarse impurities are stored.
  • These impurities are grains of sand or other inorganic particles, such as metal chips, and have reached the disperse system via the starting components, when the starting components are mixed, or in another manufacturing step.
  • the contaminants lead to a considerably greater contrast than the diffuse spots and have diameters in the millimeter range. Contrast and diameter size can therefore be used as particularly simple criteria when comparing the contamination-free area (upper picture) and the contaminated area of the test tape 7.

Abstract

The invention relates to a process for monitoring a disperse system for non-dispersed impurities (16) before processing of said system into an end product. During said process, part of the disperse system is extruded before processing to form a strip (7) and the impurities in said strip are detected. To this end, weak X-rays are beamed through small areas of the strip (7) continuously or gradually and at right angles to the strip plane. The X-rays emerging from the areas of the strip through which they have passed are subsequently detected in areas. The type, number, size, shape and/ or distribution of the impurities (16) are determined by the detected rays. It is particularly advantageous that impurities inside the strip and also on the surface thereof are detected as a result of X-rays passing through the strip (7). If the impurities (16) exceed a predetermined threshold, the disperse system does not undergo further processing.

Description

B E S C H R E I B U N G DESCRIPTION
Verfahren zur Überwachung eines dispersen Systems auf nichtdispergierte Verunreinigungen und Vorrichtung zurMethod for monitoring a disperse system for undispersed impurities and device for
Durchführung dieses VerfahrensPerforming this procedure
TECHNISCHES GEBIETTECHNICAL AREA
Bei der Erfindung wird ausgegangen von einem Verfahren zur Überwachung eines dispersen Systems auf nichtdispergierte Verunreinigungen nach dem Oberbegriff von Patentanspruch l. Die Erfindung betrifft zugleich auch eine Vorrichtung zur Durchführung des Verfahrens.The invention is based on a method for monitoring a disperse system for non-dispersed impurities according to the preamble of claim 1. The invention also relates to a device for performing the method.
In der Elektrotechnik, wie insbesondere in der Kabelindustrie, werden in zunehmendem Masse mit elektrisch leitendem oder elektrisch halbleitendem Pulver, wie etwa Leitfähigkeitsruss, gefüllte Polymere als Werkstoff für halbleitendes Material, wie etwa Abschirm- und Steuerelektroden, eingesetzt. Bei Hoch- oder Mittelspannungskabeln werden aus einem solchen halbleitenden Werkstoff bestehende Schichten zu Abschirm- und Steuerzwecken zwischen dem stromführenden Leiter und der Kabelisolation angeordnet. Betriebsbereitschaft und Lebensdauer des Kabels hängen ganz entscheidend von der Güte dieser halbleitenden Schicht ab. Zum einen werden durch nichtdispergierte Verun¬ reinigungen, welche - wie etwa Sand - mit dem Russ beim Vermi¬ schen von Russ und Polymer in das disperse System eingelagert werden, Inhomogenitäten im halbleitenden Werkstoff gebildet. Falls sich diese Inhomogenitäten beim Herstellen der Kabel als Störstellen an der Grenzschicht zum Dielektrikum ablagern, können sie das elektrische Feld des Kabels lokal ganz erheblich verzerren. Zum anderen können diese Verunreinigungen aber auch wasserlösliche Ionen enthalten. Falls daher im Kabel noch eine nicht zu vermeidende Restfeuchtigkeit vorhanden ist, können diese Ionen in die Kabelisolation diffundieren und die Eigenschaften der Kabel ganz wesentlich herabsetzen.In electrical engineering, in particular in the cable industry, polymers filled with electrically conductive or electrically semiconducting powder, such as conductive carbon black, are increasingly being used as a material for semiconducting material, such as shielding and control electrodes. In the case of high or medium voltage cables, layers consisting of such a semiconducting material are arranged between the current-carrying conductor and the cable insulation for shielding and control purposes. The operational readiness and service life of the cable depend crucially on the quality of this semiconducting layer. On the one hand, inhomogeneities are formed in the semiconducting material by non-dispersed impurities which, like sand, are incorporated into the disperse system when the carbon black and polymer are mixed. If these inhomogeneities are deposited as defects at the boundary layer with the dielectric during the manufacture of the cables, they can significantly distort the electrical field of the cable locally. On the other hand, these impurities can also contain water-soluble ions. So if there is another in the cable If there is unavoidable residual moisture, these ions can diffuse into the cable insulation and significantly reduce the properties of the cable.
STAND DER TECHNIKSTATE OF THE ART
Die Erfindung nimmt auf einen Stand der Technik Bezug, wie er in einem Artikel von A.A.Farkas et al. "High Performance semi- conductive compounds testing, production and experience", Jicable 91, 3rd International Conference on Polymer Insulated Power Cables, pages 8-11, 24-28 June 1991, Versailles, France angegeben ist. Bei einem in diesem Stand der Technik beschriebenen Verfahren zur Überwachung eines in einem Kabel als halbleitende Schicht eingesetzten dispersen Systems aus Leitfähigkeitsruss und Polyäthylen auf nichtdispergierte Verunreinigungen wird ein Teil des dispersen Systems zu einem Band extrudiert, das Band auf Verunreinigungen untersucht, und erst danach das disperse System weiterverarbeitet. Das Band enthält sehr viel Russ und ist daher undurchdichtig. Beim bekannten Verfahren wird lediglich die Oberfläche des Bandes auf nichtdispergierte Verunreinigungen untersucht. Im Inneren des Bandes befindliche Verunreinigungen können hierbei nicht erfasst werden.The invention relates to a prior art as described in an article by A.A. Farkas et al. "High Performance semi-conductive compounds testing, production and experience", Jicable 91, 3rd International Conference on Polymer Insulated Power Cables, pages 8-11, 24-28 June 1991, Versailles, France. In a method described in this prior art for monitoring a disperse system of conductive carbon black and polyethylene used in a cable as a semiconducting layer for undispersed impurities, a part of the disperse system is extruded into a band, the band is examined for impurities, and only afterwards the disperse System processed. The tape contains a lot of soot and is therefore impermeable. In the known method, only the surface of the belt is examined for undispersed impurities. Impurities inside the belt cannot be detected.
KURZE DARSTELLUNG DER ERFINDUNGSUMMARY OF THE INVENTION
Der Erfindung, wie sie in den Patentansprüchen angegeben ist, liegt die Aufgabe zugrunde, das Verfahren nach dem Stand der Technik derart weiterzubilden, dass es mit grösser Sicherheit auch im Inneren des Bandes vorhandene nichtdispergierte Verunreinigungen detektieren kann, und zugleich eine Vorrichtung anzugeben, welche in einfacher Weise zur Durchführung dieses Verfahrens geeignet ist. Das Verfahren nach der Erfindung zeichnet sich vor allem dadurch aus, dass es fortlaufend die auf der Oberfläche und im Inneren des Bandes verteilten Verunreinigungen detektieren und anzeigen kann. Hierbei es von besonderem Vorteil, dass das Verfahren unabhängig von den optischen Eigenschaften des Bandes arbeitet und in der Lage ist, auch undurchsichtig ausgebildete Bänder problemlos auf eingeschlossene Verunreinigungen zu analysieren. Als Auswahlkriterien für das Mass der Verunreinigungen können hierbei sowohl die Art, die Anzahl, die Grosse, die Form und/oder die Verteilung der eingeschlossenen Verunreinigungen dienen. Mit dem Verfahren nach der Erfindung können ohne weiteres nicht¬ dispergierte Verunreinigungen von weniger als 1 ppm nachgewiesen werden. Zudem kann sehr exakt zwischen organischen und anorgani¬ schen Verunreinigungen unterschieden werden. Da das Band reprä¬ sentativ für das gesamte disperse System ist, wird die Qualität des dispersen Systems vor seiner Weiterverarbeitung fortlaufend überwacht, und kann der Weiterverarbeitungsprozess beim Auftreten von unzulässig grossen Verunreinigungen sofort unterbrochen werden. Da mit dem erfindungsgemässen Verfahren sowohl die Art, die Anzahl, die Grosse, die Form und/oder die Verteilung der Verunreinigungen ermittelt werden, können in besonders einfacher Weise Rückschlüsse auf die Fehlerquellen gemacht werden, die für die Verunreinigungen verantwortlich sind.The invention, as specified in the claims, is based on the object of developing the method according to the prior art in such a way that it can also detect undispersed impurities present inside the belt with greater certainty, and at the same time specify a device which can be used in is simply suitable for carrying out this method. The method according to the invention is characterized in particular by the fact that it can continuously detect and display the contaminants distributed on the surface and inside the belt. It is particularly advantageous here that the method works independently of the optical properties of the tape and is able to analyze tapes which are also opaque without problems for trapped impurities. The type, number, size, shape and / or distribution of the included impurities can serve as selection criteria for the degree of impurities. With the method according to the invention, undispersed impurities of less than 1 ppm can easily be detected. In addition, a very precise distinction can be made between organic and inorganic contaminants. Since the belt is representative of the entire disperse system, the quality of the disperse system is continuously monitored prior to its further processing, and the further processing process can be interrupted immediately if impermissibly large impurities occur. Since both the type, the number, the size, the shape and / or the distribution of the contaminants are determined with the method according to the invention, conclusions can be drawn in a particularly simple manner on the sources of error which are responsible for the contaminants.
Die Vorrichtung zur Durchführung des Verfahrens nach der Erfin¬ dung ermöglicht eine sichere, kontinuierliche und/oder schritt¬ weise Überwachung des Bandes und kann gleichzeitig Prozesse steuern, bei denen das durch das Band repräsentierte disperse System - etwa durch Extrudieren bei der Kabelherstellung - weiterverarbeitet wird. KURZE BESCHREIBUNG DER ZEICHNUNGThe device for carrying out the method according to the invention enables reliable, continuous and / or step-by-step monitoring of the strip and at the same time can control processes in which the disperse system represented by the strip is further processed, for example by extrusion during cable production . BRIEF DESCRIPTION OF THE DRAWING
Bevorzugte Ausführungsbeispiele der Erfindung und die damit erzielbaren weiteren Vorteile werden nachfolgend anhand von Zeichnungen näher erläutert. Hierbei zeigt:Preferred exemplary embodiments of the invention and the further advantages achievable therewith are explained in more detail below with reference to drawings. Here shows:
Fig.l in schematischer Darstellung eine bevorzugteFig.l in a schematic representation of a preferred
Ausführungsform einer Vorrichtung nach der Erfindung zur Überwachung eines dispersen Systems auf nicht¬ dispergierte Verunreinigungen, mit einem Signalausgang, der auf den Materialflussweg des dispersen System wirkt, wobei das disperse System bei der späteren Herstellung eines Hoch- oder Mittelspannungskabels zusammen mit Isoliermaterial extrudiert wird und dann eine den Kabelleiter umschliessende, zwischen Kabelleiter und Kabelisolation angeordnete, halbleitende Abschirm- und/oder Steuerschicht bildet,Embodiment of a device according to the invention for monitoring a disperse system for non-dispersed impurities, with a signal output which acts on the material flow path of the disperse system, the disperse system being extruded together with insulating material during the subsequent production of a high or medium voltage cable and then forms a semiconducting shielding and / or control layer surrounding the cable conductor and arranged between the cable conductor and cable insulation,
Fig.2 eine Vergrösserung eines in der Vorrichtung gemäss Fig.l umrandet dargestellten Bereichs, und2 shows an enlargement of an area shown with a border in the device according to FIG. 1, and
Fig.3 zwei von der Vorrichtung gemäss Fig.l detektierte3 two detected by the device according to Fig.l.
Probenbilder, von denen sich das obere Bild auf eine Probe bezieht, welche frei von Verunreinigungen ist, und das untere Bild auf eine Probe, in der Verunreinigungen eingelagert sind.Sample images, of which the upper image relates to a sample that is free of contaminants and the lower image of a sample in which contaminants are stored.
WEGE ZUR AUSFÜHRUNG DER ERFINDUNGWAYS OF CARRYING OUT THE INVENTION
In Fig.l bezeichnet 1 einen Vorratskessel, welcher der Zwischen- speicherung eines dispersen Systems dient. Das disperse System ist durch Mischen von 10 bis 50 Volumenprozent eines elektrisch leitenden oder elektrisch halbleitenden Pulvers, wie insbesondere eines Leitfähigkeitsrusses mit Teilchengrössen kleiner 0,1 μm, mit einem Polymer, wie insbesondere Polyäthylen, hergestellt worden. Der Vorratskessel kann über ein steuerbares Umschaltven¬ til 2 mit einem Extruder 3 verbunden werden, der der Herstellung eines Hoch- oder Mittelspannungskabels dient. Der Vorratskessel 1 wird von einer Transportleitung 4 gespeist. Ein geringer Teil des durch die Transportleitung 4 geführten dispersen Systems wird durch eine By-Pass-Leitung 5 kontinuierlich abgeführt und einem Testextruder 6 zugeführt. Der Testextruder 6 erzeugt aus dem abgezweigten Teil des dispersen Systems ein Testband 7 von typischerweise 0,2 bis l mm Dicke und typischerweise 10 mm Bandbreite. Dieses Testband ist undurchsichtig, da es in fein¬ verteilter Form und in grösser Konzentration Leitfähigskeitsruss enthält. Das Testband 7 wird einem Messkopf 8 einer Vorrichtung 9 zur Überwachung des Testbandes 7 (und damit auch des dispersen Systems) auf nichtdispergierte Verunreinigungen zugeführt. Der Ausgang des Messwertgebers 8 ist mit einer Auswerte- und Steuer¬ vorrichtung 10 verbunden. Ein Signalausgang 11 der Auswerte- und Steuervorrichtung 10 wirkt auf das steuerbare Umschaltventil 2.In FIG. 1, 1 denotes a storage kettle, which is used for the intermediate storage of a disperse system. The disperse system is produced by mixing 10 to 50 percent by volume of an electrically conductive or electrically semiconductive powder, such as, in particular, a carbon black with particle sizes smaller than 0.1 μm, with a polymer, such as, in particular, polyethylene been. The supply boiler can be connected via a controllable switchover valve 2 to an extruder 3 which is used to produce a high or medium voltage cable. The storage boiler 1 is fed by a transport line 4. A small part of the disperse system led through the transport line 4 is continuously discharged through a by-pass line 5 and fed to a test extruder 6. The test extruder 6 produces a test tape 7 of typically 0.2 to 1 mm thick and typically 10 mm bandwidth from the branched-off part of the disperse system. This test tape is opaque since it contains soot in a finely divided form and in a high concentration. The test tape 7 is fed to a measuring head 8 of a device 9 for monitoring the test tape 7 (and thus also the disperse system) for undispersed impurities. The output of the sensor 8 is connected to an evaluation and control device 10. A signal output 11 of the evaluation and control device 10 acts on the controllable changeover valve 2.
Wie aus den Figuren 1 und 2 ersichtlich ist, weist der Messwert¬ geber 8 ein strahlengesichertes Gehäuse 12 auf mit zwei an entge¬ gengesetzten Seiten des Gehäuses angebrachten schmalen Öffnungen zur Durchführung des Bandes 7. Jeweils an entgegengesetzten Seiten des Bandes im Gehäuse 12 angeordnet sind eine Röhre 13 zur Erzeugung weicher Röntgenstrahlen (Betriebsspannung der Röntgen¬ röhre 13 zwischen 1 und 50 kV) sowie eine röntgenstrahlenempfind- liche BilderkennungsVorrichtung 14 mit einem Raster 15, einer computergesteuerten (CCD) Kamera oder einem Film.As can be seen from FIGS. 1 and 2, the transducer 8 has a radiation-protected housing 12 with two narrow openings on the opposite sides of the housing for the passage of the band 7. Each is arranged in the housing 12 on opposite sides of the band a tube 13 for generating soft X-rays (operating voltage of the X-ray tube 13 between 1 and 50 kV) and an X-ray-sensitive image recognition device 14 with a raster 15, a computer-controlled (CCD) camera or a film.
Informationen über die Art, die Anzahl, die Grosse, die Form und/oder die Verteilung von unerwünschten Verunreinigungen im Inneren und auf der Oberfläche des Testbandes 7 und daher auch in dem zur Weiterverarbeitung im Vorratskessels l befindlichen dispersen System werden durch den Messwertgeber 8 ermittelt und diese Informationen an die Auswerte- und Steuervorrichtung 10 weitergegeben. Wie aus Fig.2 ersichtlich ist, werden Bereiche des Testbandes 7 von beispielsweise 1 cm2 quer zur Bandebene mit weicher Röntgen¬ strahlung durchstrahlt. Die aus dem Band tretende Strahlung kann schrittweise, beispielsweise mit einem Film, oder aber auch kontinuierlich, beispielsweise mit dem Raster 15 oder einer CCD- Kamera, detektiert werden. Die aus den durchstrahlten Bereichen austretende Strahlung wird an einer typischerweise von einem Sandkorn oder von einem anderen anorganischen Partikel herrührenden Verunreinigung 16 stärker absorbiert als an dem verunreinigungsfreien, verbleibenden Teil des durchstrahlten Bandbereichs, welcher überwiegend organische Substanzen enthält. Auf dem Raster 15 wird daher ein Schattenbild 17 erzeugt. Das Schattenbild 17 wird von benachbarten Rasterpunkten - wie in der Figur angegeben ist beispielsweise von 2 Rasterpunkten - detektiert und diese Information in Form elektrischer Signale an die Auswerte- und Steuervorrichtung 10 weitergeleitet. Je nach Güte des Rasters 15 können so mit einer Auflösung höher 10 μm alle auf der Oberfläche und im Inneren des Testbandes 7 vorhandenen Verunreinigungen erfasst werden.Information about the type, the number, the size, the shape and / or the distribution of undesirable impurities inside and on the surface of the test tape 7 and therefore also in the disperse system for further processing in the storage kettle 1 are determined by the measuring sensor 8 and this information is passed on to the evaluation and control device 10. As can be seen from FIG. 2, areas of the test tape 7 of, for example, 1 cm 2 are irradiated transversely to the tape plane with soft X-ray radiation. The radiation emerging from the strip can be detected step by step, for example with a film, or else continuously, for example with the raster 15 or a CCD camera. The radiation emerging from the irradiated areas is more strongly absorbed by an impurity 16, typically originating from a grain of sand or another inorganic particle, than at the impurity-free, remaining part of the irradiated band area, which predominantly contains organic substances. A silhouette 17 is therefore generated on the grid 15. The silhouette 17 is detected by adjacent raster points - as indicated in the figure, for example by 2 raster points - and this information is forwarded to the evaluation and control device 10 in the form of electrical signals. Depending on the quality of the grid 15, all impurities present on the surface and inside the test tape 7 can be detected with a resolution higher than 10 μm.
In der Auswerte- und Steuervorrichtung 10 können die zugeführten elektrischen Signalen mit Referenzsignalen verglichen werden. Beim Überschreiten eines Schwellwertes gibt dann die Auswerte- und Steuervorrichtung 10 ein den Verunreinigungszustand des Bandes 7 charakterisierendes negatives Statussignal ab. Dieses negative Statussignal wird über den Signalausgang 11 einem Steuer- oder Regelorgan einer das disperse System weiterver¬ arbeitenden Vorrichtung zugeführt, wie insbesondere dem Umschaltventil 2, und bewirkt dann dessen Betätigung, wie insbesondere das Schliessen der Verbindung zum Extruder 3.The supplied electrical signals can be compared with reference signals in the evaluation and control device 10. When a threshold value is exceeded, the evaluation and control device 10 then emits a negative status signal that characterizes the contamination state of the belt 7. This negative status signal is fed via the signal output 11 to a control or regulating element of a device which further processes the disperse system, such as, in particular, the changeover valve 2, and then causes it to be actuated, such as in particular closing the connection to the extruder 3.
Vor dem Vergleich mit den Referenzsignalen werden mit Vorteil in der Steuer- und Auswertevorrichtung 10 Ausgabesignale gebildet, welche proportional der Art, der Anzahl, der Grosse, der Form und/oder der Verteilung der Verunreinigungen sind. Diese Signale können bei der Suche nach Fehlerquellen äusserst wertvoll sein und ermöglichen zugleich eine besonders einfacher Eingabe der für den Schwellwertvergleich angeforderten Referenzsignale.Before the comparison with the reference signals, output signals are advantageously formed in the control and evaluation device 10, which are proportional to the type, number, size, shape and / or distribution of the contaminants. These signals can be extremely valuable when looking for sources of error and at the same time enable particularly simple input of the reference signals requested for the threshold value comparison.
Zwei von der Bilderkennungsvorrichtung 14 detektierte typische Probenbilder sind in Fig.3 dargestellt. Das obere Bild bezieht sich auf einen Bereich des Testbandes 7, welcher frei von Verun¬ reinigungen ist. Die aus dem Bild erkennbaren diffusen Flecken von geringem Kontrast und von typischerweise 60 μm Durchmesser stammen von Russagglomeraten. Das untere Bild bezieht sich auf einen Bereich des Testbandes 7, in dem grobe Verunreinigungen eingelagert sind. Diese Verunreinigungen sind Sandkörner oder andere anorganische Partikel, wie Metallspäne, und sind über die Ausgangskomponenten, beim Mischen der Ausgangskomponenten oder einem anderen Herstellungsschritt ins disperse Systems gelangt. Die Verunreinigungen führen zu einem erheblich grösseren Kontrast als die diffusen Flecke und weisen Durchmesser im Millimeter¬ bereich auf. Kontrast und Durchmessergrösse können daher als besonders einfache Kriterien beim Vergleich zwischen verunreini¬ gungsfreiem (oberes Bild) und verunreinigtem Bereich des Test¬ bandes 7 verwendet werden. Two typical sample images detected by the image recognition device 14 are shown in FIG. The upper picture relates to an area of the test tape 7 which is free of impurities. The diffuse spots of low contrast and typically 60 μm in diameter that can be seen in the picture come from soot agglomerates. The lower image relates to an area of the test tape 7 in which coarse impurities are stored. These impurities are grains of sand or other inorganic particles, such as metal chips, and have reached the disperse system via the starting components, when the starting components are mixed, or in another manufacturing step. The contaminants lead to a considerably greater contrast than the diffuse spots and have diameters in the millimeter range. Contrast and diameter size can therefore be used as particularly simple criteria when comparing the contamination-free area (upper picture) and the contaminated area of the test tape 7.
B E Z U G S Z E I C H E N L I S T EB E Z U G S Z E I C H E N L I S T E
Vorratskessel Umschaltventil Extruder Transportleitung By-Pass-Leitung Testextruder Testband Messwertgeber Überwachungsvorrichtung Auswerte- und Steuervorrichtung Signalausgang Gehäuse Röntgenröhre Bilderkennungsvorrichtung Raster Verunreinigung Schattenbild Storage boiler changeover valve extruder Transport line By-pass line Test extruder Test tape Transducer Monitoring device Evaluation and control device Signal output Housing X-ray tube Image recognition device Raster contamination Silhouette

Claims

P A T E N T A N S P R Ü C H E PATENT CLAIMS
1. Verfahren zur Überwachung eines in einem Endprodukt verwend¬ baren dispersen Systems auf nichtdispergierte Verunreinigun¬ gen (16), bei dem ein Teil des dispersen Systems vor dessen Weiterverwendung zu einem Band (7) extrudiert und in diesem Band (7) die Verunreinigungen (16) detektiert werden, da¬ durch gekennzeichnet, dass kontinuierlich oder schrittweise erfasste Bereiche des Bandes (7) quer zur Bandebene durch¬ strahlt werden, dass die aus den durchstrahlten Bereichen des Bandes (7) tretende Strahlung bereichsweise detektiert wird, und dass aus der detektierten Strahlung die Art, die Anzahl, die Grosse, die Form und/oder die Verteilung der Verunreinigungen (16) ermittelt werden.1. A method for monitoring a disperse system that can be used in an end product for undispersed impurities (16), in which a part of the disperse system extrudes into a band (7) before it is reused and in this band (7) the impurities ( 16) are detected, characterized in that areas of the band (7) recorded continuously or stepwise are irradiated transversely to the plane of the band, that the radiation emerging from the irradiated areas of the band (7) is detected in areas, and that from the detected radiation, the type, number, size, shape and / or distribution of the contaminants (16) are determined.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass bei einem dispersen System, welches als mit einem feinverteil¬ ten, elektrisch leitenden oder elektrisch halbleitenden Pulver gefüllte Polymerfolie ausgebildet ist, das Band (7) mit weicher Röntgenstrahlung durchstrahlt wird.2. The method according to claim 1, characterized in that in a disperse system which is designed as a polymer film filled with a finely divided, electrically conductive or electrically semiconductive powder, the band (7) is irradiated with soft X-rays.
3. Verfahren nach Anspruch 2, dadurch gekennzeichnet, dass die weiche Röntgenstrahlung mittels einer mit einer Betriebs¬ spannung zwischen 1 und 50 kV beaufschlagten Röntgenröhre (13) erzeugt wird.3. The method according to claim 2, characterized in that the soft X-ray radiation is generated by means of an X-ray tube (13) acted upon with an operating voltage between 1 and 50 kV.
4. Verfahren nach einem der Ansprüche 2 oder 3, dadurch gekennzeichnet, dass die aus dem durchstrahlten Band (7) tretende weiche Röntgenstrahlung mit einer Bilderkennungs¬ vorrichtung (14) detektiert wird.4. The method according to any one of claims 2 or 3, characterized in that the soft X-ray radiation emerging from the irradiated band (7) is detected with an image recognition device (14).
5. Verfahren nach Anspruch 4, dadurch gekennzeichnet, dass in der Bilderkennungsvorrichtung (14) die Verunreinigungen (16) als Schattenbilder (17) erfasst werden. 5. The method according to claim 4, characterized in that in the image recognition device (14) the contaminants (16) are captured as shadow images (17).
6. Verfahren nach einem der Ansprüche 4 oder 5, dadurch gekennzeichnet, dass in der Bilderkennungsvorrichtung (14) aus der detektierten Strahlung elektrische Signale erzeugt werden, dass die elektrischen Signale nachfolgend einer Auswerte- und Steuervorrichtung (10) zugeführt und mit Referenzsignalen verglichen werden, und dass beim Überschreiten eines Schwellwertes von der Auswerte- und Steuervorrichtung (10) ein den Verunreinigungszustand des Bandes (7) charakterisierendes Statussignal abgegeben wird.6. The method according to any one of claims 4 or 5, characterized in that electrical signals are generated in the image recognition device (14) from the detected radiation, that the electrical signals are subsequently fed to an evaluation and control device (10) and compared with reference signals, and that when a threshold value is exceeded, the evaluation and control device (10) emits a status signal which characterizes the contamination state of the belt (7).
7. Verfahren nach Anspruch 6, dadurch gekennzeichnet, dass das Statussignal einem Steuer- oder Regelorgan (2) einer das disperse System weiterverarbeitenden Vorrichtung zugeführt wird.7. The method according to claim 6, characterized in that the status signal is fed to a control or regulating element (2) of a device which further processes the disperse system.
8. Verfahren nach einem der Ansprüche 6 oder 7, dadurch gekennzeichnet, dass vor dem Vergleich mit den Referenzsignalen in der Steuer- und Auswertevorrichtung (10) Ausgabesignale gebildet werden, welche proportional der Art, der Anzahl, der Grosse, der Form und/oder der Verteilung der Verunreinigungen (16) sind.8. The method according to any one of claims 6 or 7, characterized in that prior to the comparison with the reference signals in the control and evaluation device (10) output signals are formed, which are proportional to the type, number, size, shape and / or the distribution of impurities (16).
9. Vorrichtung zur Durchführung des Verfahrens nach einem der Ansprüche 1 bis 8 mit einem die Verunreinigungen (16) des Bandes (7) erfassenden Messwertgeber (8) und einer dem Messwertgeber (8) nachgeschalteten Auswerte- und Steuer¬ vorrichtung (10), dadurch gekennzeichnet, dass der Messwert¬ geber (8) ein die durchstrahlten Bereiche des Bandes (7) umschliessendes strahlengesichertes Gehäuse (12) mit zwei an entgegengesetzten Seiten des Gehäuses (12) angebrachten schmalen Öffnungen zur Durchführung des Bandes (7) aufweist sowie jeweils auf entgegengesetzten Seiten des Bandes (7) im Gehäuse (12) angeordnet eine Röhre (13) zur Erzeugung weicher Röntgenstrahlen und eine Bilderkennungsvorrichtung (14). 9. The device for carrying out the method according to one of claims 1 to 8 with a the contaminants (16) of the belt (7) sensing transducer (8) and the transducer (8) downstream evaluation and control device (10), thereby characterized in that the transducer (8) has a radiation-protected housing (12) enclosing the irradiated areas of the band (7) with two narrow openings on opposite sides of the housing (12) for the passage of the band (7) as well as on opposite ones A tube (13) for generating soft X-rays and an image recognition device (14) are arranged on the sides of the band (7) in the housing (12).
10. Vorrichtung nach Anspruch 9, dadurch gekennzeichnet, dass die Bilderkennungsvorrichtung (14) einen Film, ein Raster (15) und/oder eine computergesteuerte Kamera enthält.10. The device according to claim 9, characterized in that the image recognition device (14) contains a film, a grid (15) and / or a computer-controlled camera.
11. Vorrichtung nach einem der Ansprüche 9 oder 10, dadurch gekennzeichnet, dass die Auswerte- und Steuereinheit (10) einen mit einem Steuer- oder Regelorgan (2) einer Vorrichtung zur Verarbeitung des dispersen Systems verbindbaren Signalausgang (11) aufweist. 11. Device according to one of claims 9 or 10, dadurc h in that the evaluation and control unit (1 0) (2) has a control element with a control or of a device for processing of the disperse system connectable to the signal output (11).
PCT/CH1997/000064 1996-02-29 1997-02-21 Process for monitoring a disperse system for non-dispersed impurities and device for carrying out said process WO1997032200A1 (en)

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JP9530487A JP2000505552A (en) 1996-02-29 1997-02-21 Method for monitoring a dispersion system for undispersed impurities and apparatus for implementing the method
EP97904326A EP0883800A1 (en) 1996-02-29 1997-02-21 Process for monitoring a disperse system for non-dispersed impurities and device for carrying out said process
AU17156/97A AU1715697A (en) 1996-02-29 1997-02-21 Process for monitoring a disperse system for non-dispersed impurities and devi ce for carrying out said process

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CA2247377A1 (en) 1997-09-04
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