EP0525325A1 - Procédé pour la préparation d'articles frittés denses - Google Patents

Procédé pour la préparation d'articles frittés denses Download PDF

Info

Publication number
EP0525325A1
EP0525325A1 EP92108827A EP92108827A EP0525325A1 EP 0525325 A1 EP0525325 A1 EP 0525325A1 EP 92108827 A EP92108827 A EP 92108827A EP 92108827 A EP92108827 A EP 92108827A EP 0525325 A1 EP0525325 A1 EP 0525325A1
Authority
EP
European Patent Office
Prior art keywords
binder
green body
mixture
mold
powder
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.)
Granted
Application number
EP92108827A
Other languages
German (de)
English (en)
Other versions
EP0525325B1 (fr
Inventor
Arie Dr. Ruder
Hans Peter Dr. Buchkremer
Rudolf Prof. Hecker
Detlev Dr. Stöver
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
Publication of EP0525325A1 publication Critical patent/EP0525325A1/fr
Application granted granted Critical
Publication of EP0525325B1 publication Critical patent/EP0525325B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C24/00Coating starting from inorganic powder
    • 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
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/22Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B1/00Producing shaped prefabricated articles from the material
    • B28B1/26Producing shaped prefabricated articles from the material by slip-casting, i.e. by casting a suspension or dispersion of the material in a liquid-absorbent or porous mould, the liquid being allowed to soak into or pass through the walls of the mould; Moulds therefor ; specially for manufacturing articles starting from a ceramic slip; Moulds therefor
    • 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
    • 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

Definitions

  • the invention relates to a method for producing dense sintered workpieces made of metal, a metal alloy or ceramic materials, in which a green body is first formed from a mixture of the metal in powder form, the metal alloy or the ceramic material and a binder, which removes the binder. sintered and the sintered body is compressed, if necessary, by hot isostatic pressing (HIP process).
  • HIP process hot isostatic pressing
  • a viscous mixture of powder and binder has previously been produced, and this mixture has been pressed into the predetermined shape under a pressure of a few hundred bars. Quite apart from the fact that with this procedure narrow cavities of the form to be filled can be inaccessible to the viscous mass, it also shows that during the subsequent binder removal or Sintering process, to which the viscous mass filled under pressure is subjected, the binder is not completely removed from the mass or. the green body escapes so that undesirable residues can remain in the workpiece.
  • This object is achieved in that first the mixture of the powder, the binder, the proportion of which in the mixture is such that it is sufficient to solidify the powder-binder mixture to form the green body and thereby 2 to 5 vol %, and a solvent for the binder is formed so that it is in the form of a flowable, solid, liquid mass (casting mass), after which this mass is poured into the predetermined shape, applied or sprayed on and then dried, the solvent escaping and the remaining binder Powder-binder mixture solidified, so that the green body is formed, which is then debindered and sintered.
  • the green body is removed from the mold after drying and is ready for further processing.
  • the casting compound is expediently produced in a separate vessel, after which it is poured into the mold through a sprue or a funnel.
  • Adequate filling of the form is achieved by gravitation and can be accompanied by targeted vibration of the form. External vibrations and / or rotations of the shape by hand or mechanically are useful for this.
  • the solvent can be removed from the mass filled into the mold under normal pressure and at room temperature. However, this drying process can also take place at elevated temperature and / or under a slight negative pressure or can be accelerated thereby.
  • the filling can be built up in several steps using different materials.
  • a procedure which is expedient for this is that mixtures formed from different materials are poured into the mold one after the other, so that the poured-in mass and thus also the green body formed thereafter consists of layers of different composition arranged one above the other.
  • a second is poured onto the first. This process is continued until the mold is completely filled, so that a layer system green body composed of different materials with a stepped structure, e.g. with regard to material, porosity, grain / particle size distribution.
  • a further process variant consists in that the mixture is filled in via / or around a green body previously introduced into the mold or an already finished workpiece.
  • an inner or outer coating (s) or covering of a solid part that has already been produced can be produced, the casting compound being poured into the cavities and the surface to be coated after being introduced into a suitable mold.
  • the casting compound can also be applied or sprayed on with a brush and then further processed with good success.
  • Composites or graded materials can be made by inserting the insert component into the premix or by inserting it into the mold prior to casting.
  • the general rule is that the proportion of the binder in the mixture should be such that it is sufficient to solidify the mass to form a manageable green body.
  • the amount of binder required for this can easily be determined by means of a few preliminary tests; it is in the range between 2 and 5% by volume.
  • binder fraction 0.02 (2.00% by volume) with particle sizes of approximately 20 ⁇ m have considerable strength. However, when using larger particles with the same binder content, the strength is still sufficient to ensure that the green bodies are handled safely.
  • the proportion of binder can be varied by controlled addition or evaporation of the liquid, volatile solvent component (carrier). In practice, the maximum volume fraction is limited by the solubility limit of the binder in the solvent or by the relative natural porosity, which is approximately 26% for ideally packed spherical particles.
  • the binder condenses as a thin film on the powder particles during the removal (evaporation) of the solvent (carrier) and a rapid, continuous removal of the solvent (carrier) through the free particle spaces takes place.
  • the final strength of the green body is achieved after the solvent (carrier) has been completely removed and after the binder has solidified at room temperature (possibly also at elevated temperature) as a solid network with connecting bridges between adjacent powder particles.
  • the green body After the green body has been formed, it is subjected to a thermally activated debinding and sintering treatment.
  • the green body is heated to remove the binder.
  • This debinding process is not restricted to a specific time-temperature program (profiles, sequences, cycles), although a few partial steps are required to enable complete binder removal.
  • a typical procedure is that the green body is heated at a rate of 3-10 ° C./min to a temperature in the range from 280 to 420 ° C. and, depending on the size of the body, is kept at this temperature until the binder is removed.
  • the body is then heated to sintering temperature up to a rate of> 10 ° C / min.
  • High temperatures promote the rapid splitting of the binder into a vapor that sublimes outside the green body either in the atmosphere or pumped out by a vacuum system. The splitting and removal takes until the binder has burned out.
  • Materials such as super alloys, stainless steel, titanium alloys and aluminum alloys, iron materials, ceramic powders, for example, can be used as the material for the workpieces to be produced.
  • Zirconium oxide, chromium oxide, lathan oxide, perovskite, aluminum oxide, silicon oxide can be provided.
  • Wax, shellac, PMMA and alcohol, trichlorethylene, toluene (toluene) are mentioned as binders.
  • the sintering of the green bodies produced by the process according to the invention was carried out using specific, known schemes for each material. Density measurements showed that the sinterability of the materials is not affected by the process itself.
  • the end product can be sintered to a closed porosity. The sintered parts with closed porosity can therefore be compacted containerless up to the theoretical density by HIP.
  • Chemical analyzes of end products produced by the method according to the invention showed no increase in the concentration of contaminants related to the chemical composition of the binder, such as oxygen, carbon, nitrogen and hydrogen.
  • the overall composition was within the nominal concentrations of the starting products.
  • the mixture was poured into a four-part stable Teflon mold, measuring 80x20x1 mm. After 2 hours of drying in air, the product achieved high strength, making handling easy.
  • the total process time was 4.27 h.
  • the density of the sintered part was 92.5% of the theoretical density of Ti6A14V and the chem. Analysis showed within the measurement accuracy the same composition as that of the starting powder.
  • the mixture was applied to the substrate with a brush.
  • the 50 ⁇ m thick layer produced in this way was then air-dried for half an hour.

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Ceramic Engineering (AREA)
  • Metallurgy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)
  • Ceramic Products (AREA)
  • Compositions Of Oxide Ceramics (AREA)
EP92108827A 1991-06-22 1992-05-26 Procédé pour la préparation d'articles frittés denses Expired - Lifetime EP0525325B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4120706A DE4120706C2 (de) 1991-06-22 1991-06-22 Verfahren zur Herstellung poröser oder dichter Sinterwerkstücke
DE4120706 1991-06-22

Publications (2)

Publication Number Publication Date
EP0525325A1 true EP0525325A1 (fr) 1993-02-03
EP0525325B1 EP0525325B1 (fr) 1996-03-06

Family

ID=6434559

Family Applications (1)

Application Number Title Priority Date Filing Date
EP92108827A Expired - Lifetime EP0525325B1 (fr) 1991-06-22 1992-05-26 Procédé pour la préparation d'articles frittés denses

Country Status (3)

Country Link
EP (1) EP0525325B1 (fr)
AT (1) ATE134922T1 (fr)
DE (2) DE4120706C2 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10027551A1 (de) * 2000-06-02 2001-12-13 Thomas Hesse Plastisch verarbeitbare Formmassen auf Basis von Bienenwachs, Lösungsmittel und sinterfähigen Pulvern
US6652804B1 (en) 1998-04-17 2003-11-25 Gkn Sinter Metals Gmbh Method for producing an openly porous sintered metal film

Families Citing this family (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19535444C2 (de) * 1995-01-20 1999-07-22 Scholz Paul Friedrich Dr Ing Verfahren zum pulvermetallurgischen Herstellen von Gegenständen sowie auf diese Weise hergestellte Gegenstände
DE19528031A1 (de) * 1995-07-31 1997-02-06 Krebsoege Sinterholding Gmbh Flachdichtung aus Metall
DE19758454A1 (de) * 1997-04-21 1998-10-22 Forschungszentrum Juelich Gmbh Dünne, feinporige Metallschicht
DE19717460A1 (de) * 1997-04-25 1998-10-29 Karlsruhe Forschzent Verfahren zum Herstellen poröser oder dichter Keramik, insbesondere supraleitende Keramik
DE19722004A1 (de) * 1997-05-27 1998-12-03 Fraunhofer Ges Forschung Verfahren zur Herstellung eines Metall- oder Keramikwerkstücks
DE19748742C1 (de) * 1997-11-05 1999-07-01 Karlsruhe Forschzent Verfahren zur Herstellung von schmelztexturierten Volumenproben auf der Basis der Hochtemperatursupraleiter Nd¶1¶Ba¶2¶Cu¶3¶O¶7¶(Nd-123)
DE19801440C2 (de) * 1998-01-16 2001-08-16 Forschungszentrum Juelich Gmbh Kostengünstiges Verfahren zur Herstellung einer Elektroden-Elektrolyt-Einheit
US5989493A (en) * 1998-08-28 1999-11-23 Alliedsignal Inc. Net shape hastelloy X made by metal injection molding using an aqueous binder
DE19841573C2 (de) * 1998-09-11 2000-11-09 Karlsruhe Forschzent Verfahren zum Herstellen von mechanisch festen, elektrisch leitenden Verbindungen zwischen Hochtemperatursupraleitern (HTSL)
DE19936734C1 (de) * 1999-08-06 2001-02-15 Fraunhofer Ges Forschung Verfahren zur Herstellung eines Metall- oder Keramikwerkstücks
DE19963698A1 (de) * 1999-12-29 2001-07-12 Gkn Sinter Metals Gmbh Dünne poröse Schicht mit offener Porosität und Verfahren zu ihrer Herstellung
DE102005024623B4 (de) * 2005-05-30 2007-08-23 Beru Ag Verfahren zum Herstellen eines keramischen Glühstiftes für eine Glühkerze

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4491559A (en) * 1979-12-31 1985-01-01 Kennametal Inc. Flowable composition adapted for sintering and method of making
EP0177209A2 (fr) * 1984-10-01 1986-04-09 CDP, Ltd. Fabrication d'un article à partir de composants métalliques séparés
EP0260101A2 (fr) * 1986-09-09 1988-03-16 Mixalloy Limited Fabrication de produits plats à partir de poudre
WO1988007901A1 (fr) * 1987-04-09 1988-10-20 Ceramic Systems Corporation Moulage et coulage de precision utilisant des systemes fortement charges
DE4037258A1 (de) * 1989-11-24 1991-05-29 Asea Brown Boveri Verfahren zur herstellung eines komplizierten bauteils ausgehend von pulvern

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5006493A (en) * 1986-03-31 1991-04-09 The Dow Chemical Company Novel ceramic binder comprising poly(ethyloxazoline)
US4882110A (en) * 1987-01-27 1989-11-21 Air Products And Chemicals, Inc. CO2 copolymer binder for forming ceramic bodies and a shaping process using the same

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4491559A (en) * 1979-12-31 1985-01-01 Kennametal Inc. Flowable composition adapted for sintering and method of making
EP0177209A2 (fr) * 1984-10-01 1986-04-09 CDP, Ltd. Fabrication d'un article à partir de composants métalliques séparés
EP0260101A2 (fr) * 1986-09-09 1988-03-16 Mixalloy Limited Fabrication de produits plats à partir de poudre
WO1988007901A1 (fr) * 1987-04-09 1988-10-20 Ceramic Systems Corporation Moulage et coulage de precision utilisant des systemes fortement charges
DE4037258A1 (de) * 1989-11-24 1991-05-29 Asea Brown Boveri Verfahren zur herstellung eines komplizierten bauteils ausgehend von pulvern

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6652804B1 (en) 1998-04-17 2003-11-25 Gkn Sinter Metals Gmbh Method for producing an openly porous sintered metal film
DE10027551A1 (de) * 2000-06-02 2001-12-13 Thomas Hesse Plastisch verarbeitbare Formmassen auf Basis von Bienenwachs, Lösungsmittel und sinterfähigen Pulvern
DE10027551B4 (de) * 2000-06-02 2005-09-29 Hesse, Thomas, Dipl.-Ing. Verfahren zur Herstellung von Formkörpern aus einer plastisch verarbeitbaren Formmasse auf der Basis von Bienenwachs, Lösungsmittel und sinterfähigen Pulvern und eine Verwendung der Formmasse

Also Published As

Publication number Publication date
DE4120706C2 (de) 1994-10-13
ATE134922T1 (de) 1996-03-15
DE59205549D1 (de) 1996-04-11
EP0525325B1 (fr) 1996-03-06
DE4120706A1 (de) 1992-12-24

Similar Documents

Publication Publication Date Title
EP0525325B1 (fr) Procédé pour la préparation d'articles frittés denses
DE1758845C3 (de) Verfahren zur Herstellung von Prazisions gießformen fur reaktionsfähige Metalle
DE1915977B2 (de) Verfahren zur Herstellung von Zahnersatz und Schmuck aus Metallpulvern
DE2027016A1 (de) Verfahren zum Verdichten von Metall oder Keramikgegenstanden
WO2000006327A2 (fr) Procede de production de composants par un procede de moulage par injection de poudre metallique
DE2650982A1 (de) Verfahren zur isostatischen warmverdichtung
WO1987000781A1 (fr) Elements de construction fabriques par la metallurgie des poudres
EP1579934B1 (fr) Procédé de fabrication d'un moufle pour le moulage de précision ou le moulage sur modèle ainsi que la composition pour sa fabrication
DE2208250B2 (de) Verfahren zur Herstellung eines isostatisch druckgesinterten Körpers
DE4322084A1 (de) Verfahren zur Herstellung eines Setters
DE1150264B (de) Organisches Suspensionsmittel beim Herstellen von zu sinternden Formkoerpern nach dem Schlickerguss-verfahren
WO2018134202A1 (fr) Procédé de production de corps métalliques durs par impression 3d
DE2258485A1 (de) Verfahren und vorrichtung zur herstellung von guss- und pressformen
EP0421084B1 (fr) Procédé d'obtention d'une pièce par métallurgie des poudres
EP0151472B1 (fr) Procédé pour la compression de parties poreuses en céramique pour la compression isostatique à chaud
EP3145662B1 (fr) Procédé de production de composants céramiques et/ou métalliques
DE4037258A1 (de) Verfahren zur herstellung eines komplizierten bauteils ausgehend von pulvern
DE19717460A1 (de) Verfahren zum Herstellen poröser oder dichter Keramik, insbesondere supraleitende Keramik
DE19638927C2 (de) Verfahren zur Herstellung hochporöser, metallischer Formkörper
DE19730742C2 (de) Verfahren zur Herstellung eines Silizium enthaltenden nichtoxidischen Keramikformkörpers oder einer solchen Schicht
DE3808123A1 (de) Verfahren zur herstellung von sinterteilen aus feinkoernigen metall- oder keramikpulvern
DE102014209085A1 (de) Herstellung eines Formkörpers aus einer Dentallegierung
DE3517494C2 (fr)
DE2422425A1 (de) Verfahren und vorrichtung zur herstellung von gegenstaenden
EP0446673A1 (fr) Procédé de préparation d'un article fritté avec une couche externe compacte et une surface lisse

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT CH DE FR GB IT LI SE

17P Request for examination filed

Effective date: 19930528

17Q First examination report despatched

Effective date: 19941005

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AT CH DE FR GB IT LI SE

REF Corresponds to:

Ref document number: 134922

Country of ref document: AT

Date of ref document: 19960315

Kind code of ref document: T

REF Corresponds to:

Ref document number: 59205549

Country of ref document: DE

Date of ref document: 19960411

ITF It: translation for a ep patent filed

Owner name: STUDIO JAUMANN

ET Fr: translation filed
GBT Gb: translation of ep patent filed (gb section 77(6)(a)/1977)

Effective date: 19960521

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

26N No opposition filed
REG Reference to a national code

Ref country code: GB

Ref legal event code: IF02

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: CH

Payment date: 20110525

Year of fee payment: 20

Ref country code: FR

Payment date: 20110603

Year of fee payment: 20

Ref country code: SE

Payment date: 20110523

Year of fee payment: 20

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 20110523

Year of fee payment: 20

Ref country code: AT

Payment date: 20110520

Year of fee payment: 20

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 20110419

Year of fee payment: 20

Ref country code: IT

Payment date: 20110527

Year of fee payment: 20

REG Reference to a national code

Ref country code: DE

Ref legal event code: R071

Ref document number: 59205549

Country of ref document: DE

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

REG Reference to a national code

Ref country code: GB

Ref legal event code: PE20

Expiry date: 20120525

REG Reference to a national code

Ref country code: SE

Ref legal event code: EUG

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Free format text: LAPSE BECAUSE OF EXPIRATION OF PROTECTION

Effective date: 20120525

REG Reference to a national code

Ref country code: AT

Ref legal event code: MK07

Ref document number: 134922

Country of ref document: AT

Kind code of ref document: T

Effective date: 20120526

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DE

Free format text: LAPSE BECAUSE OF EXPIRATION OF PROTECTION

Effective date: 20120527