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WO1998048077A1 - Couche metallique mince a micropores - Google Patents

Couche metallique mince a micropores Download PDF

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Publication number
WO1998048077A1
WO1998048077A1 PCT/DE1998/000594 DE9800594W WO9848077A1 WO 1998048077 A1 WO1998048077 A1 WO 1998048077A1 DE 9800594 W DE9800594 W DE 9800594W WO 9848077 A1 WO9848077 A1 WO 9848077A1
Authority
WO
WIPO (PCT)
Prior art keywords
metal layer
layer
open porosity
suspension
metal
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/DE1998/000594
Other languages
German (de)
English (en)
Inventor
Hans Peter Buchkremer
Detlev STÖVER
Arno Schirbach
Günther SCHLIEBACH
Werner Mallener
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.)
Forschungszentrum Juelich GmbH
Original Assignee
Forschungszentrum Juelich 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 Forschungszentrum Juelich GmbH filed Critical Forschungszentrum Juelich GmbH
Priority to EP98916815A priority Critical patent/EP0977909B1/fr
Priority to DE59804429T priority patent/DE59804429D1/de
Priority to AT98916815T priority patent/ATE219166T1/de
Publication of WO1998048077A1 publication Critical patent/WO1998048077A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F5/00Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F5/10Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of articles with cavities or holes, not otherwise provided for in the preceding subgroups
    • B22F5/106Tube or ring forms
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/002Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of porous nature
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10Processes characterised by the sequence of their steps
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00Aspects linked to processes or compositions used in powder metallurgy

Definitions

  • the invention relates to a metal layer with open porosity.
  • Porous metal layers of the type mentioned at the outset, which are used in particular as filters, are known.
  • a metallic fleece is used, small pore sizes in the micrometer range can be achieved. Then the fleece thickness is at least half a millimeter.
  • the layer thicknesses of the aforementioned nonwovens can also not be manufactured very precisely. Relatively large tolerances have to be accepted.
  • Ceramic fil- ter are also relatively thick, and there is a correspondingly large flow resistance. Ductility is also not guaranteed. The brittleness of the ceramic material is also a disadvantage for many purposes.
  • plastic is used as the filter material, increased operating temperatures are not possible.
  • plastic is not a suitable filter material, since it cannot be sterilized according to the requirements that e.g. B. are required in the medical or in the food sector. The filter cannot be re-used in these cases.
  • the object of the invention is to produce a temperature-resistant, sterilizable, simple and reproducible metal layer with continuous porosity, which is ductile, mechanically stable and elastic and in which - if it is used as a filter - low flow pressure losses occur. Microfiltration tasks should also be performed with the metal layer.
  • the object of the invention is achieved by a metal layer with a maximum thickness of 500 ⁇ m, in other words by a metal foil which has an effective pore diameter which is up to a twelfth, preferably up to a fifteenth, of the layer thickness of the metal layer.
  • the pores here are to be understood as the channels that pass through the layer Create open porosity. Occasional "cavities" due to inhomogeneities are not pores in the sense of the claim.
  • the effective pore diameter is in particular up to a quarter, preferably up to a fifth of the mean particle or powder grain diameter of the powder used.
  • the effective size of the pores, which cause the continuous (open) porosity is up to 500/12 mm, i.e. up to approx. 40 ⁇ m. In other words, substances have to be smaller than approx. 40 ⁇ m in order to be able to pass through the metal layer.
  • the layer thickness should be at least three times as thick as the powder diameter, ie at least 150 ⁇ m, in order to reliably avoid cavity problems due to inhomogeneities in the material.
  • the effective pore diameter of the layer is then regularly up to 50/4 ⁇ m (3 * 50/12 ⁇ m), preferably up to 50/5 ⁇ m (3 * 50/15 ⁇ m).
  • the layer thickness of the metal foil is at most 100 ⁇ m, preferably not more than 50 ⁇ m.
  • the effective pore size in the aforementioned sense is in all cases a maximum of 1/12 of the layer thickness.
  • the metal allows elevated temperatures, behaves ductile, mechanically stable and is elastic.
  • the material can be sterilized without any problems.
  • the layer thickness of the layer or film can be produced within narrow tolerance limits in comparison to a nonwoven or a fabric. The production is also inexpensive, in particular in comparison to a fabric.
  • the layer preferably consists of metals that are sinterable. Metals that have this property within the meaning of the claim form sinter bridges between individual metallic powder grains during a sintering process. Steel, stainless steel, bronze and nickel form sintered bridges in the aforementioned sense. These are easier to sinter than reactive metals such as aluminum and titanium.
  • the demanding metal layer can be produced by the film casting known from the ceramic field.
  • a pouring slurry is first provided, in other words a suspension.
  • the slip has metal powder.
  • the average diameter of the metal powder is to be selected to be less than a third of the layer thickness to be produced.
  • the ratio of metal powder to layer thickness ensures that the layer consists of several layers of powder grains. This avoids “holes” that go through the layer and that are considerably larger than the desired effective pore size. The more layers of powder that are possible, the more reliably no “through holes” occur.
  • a metal layer should therefore preferably be made up of 5 to 10 powder layers.
  • the slip consists of a solvent, dispersant, binder and, if necessary, a substance for adapting the viscosity of the slip to a pouring or spraying device used.
  • the thinner the pouring slot in a pouring device used the thinner the slip must be. If necessary, this adjustment is made by the substance to adjust the viscosity.
  • Isopropanol is particularly suitable as the solvent, but also toluene, water, etc.
  • Bis (2-ethylhexyl phthalate) can be used as the dispersant.
  • polyvinyl butyral is suitable as a binder.
  • Fish oil can be used as a substance for adapting the viscosity to equipment conditions.
  • care must be taken that the subsequent sintering is prevented as little as possible. Carbon, oxygen or nitrogen may therefore not be present in high concentrations in the sintered product. Oxide, carbide and nitride formation should be avoided during sintering.
  • the slip should therefore consist of substances that are easily thermally decomposable in order to comply with the aforementioned requirements.
  • the slip preferably also contains a release agent such as polyethylene glycol. The release agent has the effect that a dried layer produced from the slip can be detached from a carrier in a sufficiently uncomplicated manner.
  • the slip is applied in layers on a carrier.
  • a carrier z. B. a plastic or metal foil.
  • the slip is dried and removed from the carrier, or detached if a self-supporting metal layer is to be produced. This green body is then sintered.
  • the sophisticated, porous metal foil can be produced from the suspension, ie from the slip, by means of the spray process known from DE 41 20 706.
  • the layer can be calibrated by rolling in an advantageous further process step.
  • a film 117 ⁇ m thick was rolled to a thickness of exactly 100 ⁇ m.
  • the thickness of the metal layer can thus be produced in a reproducible manner.
  • the pore size can be reduced in a defined manner by means of rolling.
  • a defined pore size can be produced reproducibly in this way.
  • the flow resistance or the flow rate can consequently be calibrated in the layer produced according to the method.
  • the demanding layer can be used as a filter, for sound insulation purposes or for flame flashbacks.
  • the layer is firmly connected to the inner wall of a tube.
  • the tube is completely porous if it is to be used as a filter.
  • the effective pore size in the tube is then preferably larger than that of the metallic layer in order to achieve low flow resistances.
  • the tube then acts as a carrier. If such a tube has no continuous pores, the metallic layer can e.g. B. serve as a catalyst or to generate a turbulent flow in the tube.
  • a suspension as in DE 41 20 706. This suspension is metered into a rotating tube, which is porous depending on the application. By rotating the pipe the suspension is deposited evenly and in layers on the inner wall. The suspension dries during the rotation process. Once the desired layer thickness has been reached, the supply of the suspension is stopped. As soon as the drying process is finished, the rotation is stopped. The tube is then sintered with the dried suspension, i.e. with the green body.
  • the suspension is fed into the tube with the open porosity by means of a tube.
  • the tube is moved in a defined manner in the tube. This ensures an even distribution of the suspension in the pipe.
  • a spray head is inserted into the tube.
  • the spray head or the pipe rotates.
  • the inner walls of the pipe are sprayed.
  • This method corresponds to the spray method known from DE 41 20 706. It is used especially for pipes with an inner diameter of more than 50 mm.
  • a section of a tube wall 2 with open porosity is shown in cross section, on which, according to the method, a metal layer 1 has been applied as an inner coating.
  • the inner coating has a maximum thickness of 500 ⁇ m in the manner shown in the figure.
  • a slip with the following components is produced for the "Foil casting” production method:
  • the sample is mixed for 2-2.5 hours, for example in a tumble mixer and then poured directly onto a film casting bench to thicknesses of, for example, 60 ⁇ m, 120 ⁇ m or thicker (tested up to 400 ⁇ m).
  • a film casting bench After drying (approx. 3 h) and stripping the layer, the sintering process follows.
  • sintering was carried out at 950 ° C for 1-3 hours in vacuum ( ⁇ 10 "2 mbar), argon or argon + 4 vol.% Hydrogen in a tube furnace.
  • the product is a flexible, porous metal foil with a relative density between 55% and 69%
  • the pore maximum for the powder mentioned is about 5-7 ⁇ m in diameter.
  • the spray suspension is first prepared by mixing binder solution and powder in a ratio of 2: 1 (parts by volume). A 9% (% by weight) shellac-ethanol solution was used as the binder solution and a gas-atomized 316 L stainless steel powder with a grain diameter of ⁇ 16 ⁇ m was used as the metal powder.
  • the suspension can be sprayed directly into a suitable system. This is done by spraying 50 - 200 ⁇ m thick layers on polyethylene foils (PE-HD 0.2 mm).
  • the desired film shape is cut out with a punching or cutting tool: here 0 93 mm with a punching tool.
  • a drying time of 1-2 hours here 2 hours
  • the PE film is removed from the green film.
  • the sintering was carried out at 950 ° C. for 1 hour in vacuo.
  • the product has one relative density of 63% and a pore maximum at approx. 6 ⁇ m.
  • the binder solution is a 9% shellac solution (shellac ethanol).
  • the spray suspension consists of a mixture of powder and binder solution in a ratio of 1: 2.
  • Powder and binder solution are homogenized for 8 hours in a tumble mixer.
  • the tube is inserted into the sintering furnace and sintered at 950 ° C. for 1 hour in a vacuum.
  • Inner coatings with porosities between 30 and 50% were produced in a thickness range between 20 and 300 ⁇ m.

Landscapes

  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Powder Metallurgy (AREA)
  • Filtering Materials (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

L'invention concerne une couche métallique à porosité ouverte et présentant une épaisseur maximale de 500 mu m, le diamètre des pores traversants représentant au maximum un douzième de cette épaisseur. Pour réaliser cette couche métallique à porosité ouverte, on applique une suspension qui contient une poudre métallique, un dispersant ainsi que des substances servant à ajuster la viscosité, sur un support, en formant une couche que l'on sèche et que l'on soumet ensuite à un frittage. L'épaisseur de couche de la suspension appliquée sur le support doit être telle que l'épaisseur de la couche métallique après le frittage corresponde à au moins trois fois le diamètre des grains de poudre.
PCT/DE1998/000594 1997-04-21 1998-02-27 Couche metallique mince a micropores Ceased WO1998048077A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
EP98916815A EP0977909B1 (fr) 1997-04-21 1998-02-27 Couche metallique mince a micropores
DE59804429T DE59804429D1 (de) 1997-04-21 1998-02-27 Dünne, feinporige metallschicht
AT98916815T ATE219166T1 (de) 1997-04-21 1998-02-27 Dünne, feinporige metallschicht

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19716595A DE19716595C1 (de) 1997-04-21 1997-04-21 Dünne, feinporige, metallische Innenschicht eines Rohres
DE19716595.8 1997-04-21

Publications (1)

Publication Number Publication Date
WO1998048077A1 true WO1998048077A1 (fr) 1998-10-29

Family

ID=7827146

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/DE1998/000594 Ceased WO1998048077A1 (fr) 1997-04-21 1998-02-27 Couche metallique mince a micropores

Country Status (4)

Country Link
EP (1) EP0977909B1 (fr)
AT (1) ATE219166T1 (fr)
DE (3) DE19758454A1 (fr)
WO (1) WO1998048077A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7306753B2 (en) * 1999-12-29 2007-12-11 Gkn Sinter Metals Gmbh Method of making a thin porous layer

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10041992A1 (de) 2000-08-26 2002-03-14 Gkn Sinter Metals Gmbh Modul zur Verwendung als Filter, Katalysator oder Erhitzer sowie Verfahren zu seiner Herstellung
DE10123199B4 (de) * 2001-05-12 2005-02-24 Gkn Sinter Metals Gmbh Verfahren zur Herstellung von zumindest teilweise innenbeschichteten rohrförmigen Körpern mit einer Beschichtung aus einem sinterfähigen Material

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2323878A1 (de) * 1973-05-11 1974-11-21 Union Carbide Corp Verfahren und vorrichtung zum beschichten von metallsubstraten
US3855638A (en) * 1970-06-04 1974-12-24 Ontario Research Foundation Surgical prosthetic device with porous metal coating
JPS5788967A (en) * 1980-11-21 1982-06-03 Showa Alum Corp Formation of porous layer on metallic surface
FR2520265A1 (fr) * 1982-01-22 1983-07-29 Thermo Electron Corp Meche pour tube de chaleur
EP0436834A2 (fr) * 1990-01-08 1991-07-17 Degussa Aktiengesellschaft Composition contenant de l'or pour la fabrication de revêtements à haute porosité
WO1994019510A1 (fr) * 1993-02-19 1994-09-01 Fabrique De Fer De Maubeuge Procedes et installations pour realiser en continu plusieurs revetements a base d'alliage metallique sur une bande d'acier

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
LU35261A1 (fr) * 1956-07-25
FR2031787A5 (fr) * 1969-02-07 1970-11-20 Onera (Off Nat Aerospatiale)
DE4120706C2 (de) * 1991-06-22 1994-10-13 Forschungszentrum Juelich Gmbh Verfahren zur Herstellung poröser oder dichter Sinterwerkstücke

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3855638A (en) * 1970-06-04 1974-12-24 Ontario Research Foundation Surgical prosthetic device with porous metal coating
DE2323878A1 (de) * 1973-05-11 1974-11-21 Union Carbide Corp Verfahren und vorrichtung zum beschichten von metallsubstraten
JPS5788967A (en) * 1980-11-21 1982-06-03 Showa Alum Corp Formation of porous layer on metallic surface
FR2520265A1 (fr) * 1982-01-22 1983-07-29 Thermo Electron Corp Meche pour tube de chaleur
EP0436834A2 (fr) * 1990-01-08 1991-07-17 Degussa Aktiengesellschaft Composition contenant de l'or pour la fabrication de revêtements à haute porosité
WO1994019510A1 (fr) * 1993-02-19 1994-09-01 Fabrique De Fer De Maubeuge Procedes et installations pour realiser en continu plusieurs revetements a base d'alliage metallique sur une bande d'acier

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
PATENT ABSTRACTS OF JAPAN vol. 006, no. 181 (M - 156) 17 September 1982 (1982-09-17) *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7306753B2 (en) * 1999-12-29 2007-12-11 Gkn Sinter Metals Gmbh Method of making a thin porous layer

Also Published As

Publication number Publication date
EP0977909B1 (fr) 2002-06-12
DE19716595C1 (de) 1998-09-03
DE59804429D1 (de) 2002-07-18
ATE219166T1 (de) 2002-06-15
EP0977909A1 (fr) 2000-02-09
DE19758454A1 (de) 1998-10-22

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