WO1992011106A1 - Process and device for manufacturing high-density sintered products - Google Patents
Process and device for manufacturing high-density sintered products Download PDFInfo
- Publication number
- WO1992011106A1 WO1992011106A1 PCT/DE1991/000983 DE9100983W WO9211106A1 WO 1992011106 A1 WO1992011106 A1 WO 1992011106A1 DE 9100983 W DE9100983 W DE 9100983W WO 9211106 A1 WO9211106 A1 WO 9211106A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- pressure
- pressure chamber
- sintered
- sintering
- sample container
- 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
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
Definitions
- the invention relates to a method for producing dense sintered workpieces by sintering powdery material with subsequent hot isostatic pressing (HIP).
- the sintering is carried out under vacuum.
- the sintered intermediate product which is subsequently to be compressed by the HIP step is referred to below as the "sintered intermediate product”.
- Vacuum sintering followed by a HIP step is used to densify workpieces almost to their theoretically possible material density. It has been found that undesired contamination of the sintered intermediate product occurs if, during sintering under vacuum, desorbents dissolve from the walls which enclose the space to be evacuated, which are deposited on the powder particles of the material to be sintered. Passive layers are formed which disturb the sintering processes and prevent a material structure with exclusively closed porosity and impair the product quality. The closed porosity is a prerequisite for an immediately subsequent HIP step with the aim of further densifying the material up to its theoretically possible density.
- a purging gas which is chemically inert to the powder material is then introduced into the pressure chamber in the vicinity of the green body to be sintered while the green body or bodies are vacuum-sintered while maintaining low pressure. Flushing with inert gas prevents chemical reactions with the material of the green body to be sintered, but essentially prevents oxidation. Intermediates with closed porosity are formed during sintering, which can be hot isostatically compressed directly after the vacuum sintering.
- the pressure during vacuum sintering is expediently not set above 10 mbar.
- the pressure is preferably between 1-10 mbar.
- the invention also relates to a pressure chamber for carrying out the method according to the invention.
- the pressure chamber has one on a vacuum pump
- REPLACEMENT LEAF connected vacuum line and a compressed gas line connected to a high pressure pump.
- the sample container can be heated to the sintering and HIP temperature.
- a flushing gas line is introduced according to the invention according to claim 4, which opens at the sample container in such a way that a flushing gas flows in at low pressure via the flushing gas line during sintering into the pressure chamber and surrounds the powdery material to be sintered can.
- the purge gas line opens into a purge gas chamber provided on the sample container. The purge gas flows from this to the green bodies.
- the invention is explained in more detail below on the basis of an exemplary embodiment.
- the drawing shows schematically a pressure chamber with a mold container suitable for sintering.
- a pressure vessel 1 is shown in the drawing, the pressure chamber 2 of which is thermally insulated from the environment. Electrical heating elements 3, 4 are arranged within the pressure chamber 2. The heating elements 3 heat an upper, the heating elements 4 a vertically below heating zone in the pressure chamber. The heating zones are indicated in the drawing with reference numbers 5 and 6.
- thermocouples 7 to 9 The actual temperature in the heating zones is determined by thermocouples 7 to 9.
- a controller 10 which controls the switching on and off of the heating elements 3, 4 regulates the temperature in the pressure chamber 2 via the thermocouples 7 to 9 to a predetermined target temperature.
- the pressure in the pressure chamber 2 is determined outside the pressure vessel.
- the pressure chamber 2 is connected on the one hand to a vacuum line 11 with a vacuum valve 12, and on the other hand to a pressure gas line 13 with a pressure valve
- a sliding loading table 15 with a sample holder 16 for receiving green bodies 17 made of powdered material to be sintered.
- the green bodies 17 have the preform of the sintered body to be produced, they are open-pore.
- a purge gas line 18 leads to the sample container 16 for purging the sample container with argon.
- the purging gas flows into a purging gas chamber 19 and is guided out of this to the green bodies 17.
- the purge gas is withdrawn from the sample container 16 via a suction line 20.
- the temperature of the purge gas after passage of the powdery material is measured by a thermocouple 21.
- the purge gas drawn off flows via the suction line 20 to a gas analyzer 22 and is examined there for its impurities.
- the pressure vessel 1 has thermal insulating plates 23 which protect the pressure chamber 2 against heat losses to the outside.
- green bodies were produced from U 700 (UDIMET 700).
- the powdery material for the green bodies had an average powder grain size of ⁇ 45 ⁇ m.
- Cylindrical green bodies were used to produce ring-shaped sintered pieces.
- the green bodies were stacked on top of one another in the sample container 16 and sintered for half an hour while introducing argon under vacuum at a pressure of 10 mbar and a temperature of 1270 ° C.
- the sintered intermediate products were hot isostatically pressed without prior removal from the pressure chamber 2 and without intermediate cooling at a temperature of 1150 ° C. and a pressure of 150 MPa.
- the HIP process took 3 hours.
- the manufactured workpiece rings had a theoretical density.
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Powder Metallurgy (AREA)
- Press-Shaping Or Shaping Using Conveyers (AREA)
Abstract
Description
B e s c h r e i b u n g Description
Verfahren und Einrichtung zum Herstellen hoch¬ dichter SinterwerkstückeMethod and device for producing high-density sintered workpieces
Die Erfindung bezieht sich auf ein Verfahren zum Herstellen dichter Sinterwerkstücke durch Sintern pulverförmigen Materials mit anschließendem heißiso- statischen Pressen (HIP). Das Sintern wird unter Vakuum durchgeführt. Das gesinterte, nachfolgend noch durch den HIP-Schritt zu verdichtende Zwischen¬ produkt wird im folgenden als "Sinterzwischenpro¬ dukt" bezeichnet.The invention relates to a method for producing dense sintered workpieces by sintering powdery material with subsequent hot isostatic pressing (HIP). The sintering is carried out under vacuum. The sintered intermediate product which is subsequently to be compressed by the HIP step is referred to below as the "sintered intermediate product".
Das Vakuumsinterπ mit anschließendem HIP-Schritt wird angewandt, um Werkstücke annähernd bis auf ihre theoretisch mögliche Werkstoffdichte zu ver¬ dichten. Dabei hat sich herausgestellt, daß uner¬ wünschte Verunreinigungen des Sinterzwischenprodukts auftreten, wenn sich beim Sintern unter Vakuum von den Wänden, die den zu evakuierenden Raum umschlie¬ ßen, Desorbentien lösen, die sich auf den Pulver¬ teilchen des zu sinternden Materials niederschlagen. Es bilden sich Passivschichten aus, die die Sinter¬ vorgänge stören und eine Materialstruktur mit aus¬ schließlich geschlossener Porosität verhindern und die Produktqualität beeinträchtigen. Die geschlos¬ sene Porosität ist Voraussetzung für einen unmittel¬ bar nachfolgenden HIP-Schritt mit dem Ziel einer weiteren Verdichtung des Materials bis zu dessen theoretisch möglicher Dichte.Vacuum sintering followed by a HIP step is used to densify workpieces almost to their theoretically possible material density. It has been found that undesired contamination of the sintered intermediate product occurs if, during sintering under vacuum, desorbents dissolve from the walls which enclose the space to be evacuated, which are deposited on the powder particles of the material to be sintered. Passive layers are formed which disturb the sintering processes and prevent a material structure with exclusively closed porosity and impair the product quality. The closed porosity is a prerequisite for an immediately subsequent HIP step with the aim of further densifying the material up to its theoretically possible density.
Bisher wurde der Nachteil, daß sich nicht alle offe¬ nen Poren schließen, durch eine Kapselung des Sin- terzwischenprodukts gelöst. Es bedurfte also zwi¬ schen Sintern und HIP-Schritt eines weiteren Arbeits¬ ganges, nämlich einer Umhüllung des gesinterten Kör¬ pers mit einer gasdichten, druckfesteπ Kapsel.So far, the disadvantage that not all open pores close due to encapsulation of the sin intermediate product solved. A further operation was therefore required between sintering and the HIP step, namely a covering of the sintered body with a gastight, pressure-resistant capsule.
Aufgabe der Erfindung ist es, zum Herstellen dich¬ ter Sinterwerkstücke das Sintern von Grünkörpern aus pulverförmigem Material derart durchzuführen, daß beim Sintern Sinterzwischenprodukte mit nach außen geschlossener Porosität entstehen, damit der HIP-Schritt unmittelbar anschließbar ist.It is an object of the invention to carry out the sintering of green bodies made of powdery material in order to produce dense sintered workpieces in such a way that sintered intermediate products with porosity which are closed to the outside occur during sintering, so that the HIP step can be connected directly.
Diese Aufgabe der Erfindung wird bei einem Verfah¬ ren der eingangs genannten Art durch die in Patentan¬ spruch 1 angegebenen Maßnahmen gelöst. Danach wird während des Vakuumsinterns des oder der Grünkörper unter Beibehaltung niedrigen Druckes in die Druck¬ kammer in die Umgebung des zu sinternden Grünkör¬ pers ein Spülgas eingeführt, das sich zum Pulver¬ material chemisch inert verhält. Durch das Spülen mit Iπertgas werden chemische Reaktionen mit dem Material des zu sinternden Grünkörpers, Oxidation im wesentlichen aber Reduktion verhindert. Es ent¬ stehen beim Sintern Zwischenprodukte mit geschlos¬ sener Porosität, die direkt im Anschluß an das Va¬ kuumsintern heißisostatisch verdichtet werden kön¬ nen .This object of the invention is achieved in a method of the type mentioned at the outset by the measures specified in patent claim 1. A purging gas which is chemically inert to the powder material is then introduced into the pressure chamber in the vicinity of the green body to be sintered while the green body or bodies are vacuum-sintered while maintaining low pressure. Flushing with inert gas prevents chemical reactions with the material of the green body to be sintered, but essentially prevents oxidation. Intermediates with closed porosity are formed during sintering, which can be hot isostatically compressed directly after the vacuum sintering.
Nach Patentansprüchen 2 und 3 wird der Druck beim Vakuumsintern zweckmäßig nicht über 10 mbar einge¬ stellt. Bevorzugt beträgt der Druck zwischen 1 - 10 mbar.According to patent claims 2 and 3, the pressure during vacuum sintering is expediently not set above 10 mbar. The pressure is preferably between 1-10 mbar.
Gegenstand der Erfindung ist auch eine Druckkammer zur Durchführung des erfindungsgemäßen Verfahrens. Die Druckkammer weist eine an einer VakuumpumpeThe invention also relates to a pressure chamber for carrying out the method according to the invention. The pressure chamber has one on a vacuum pump
ERSATZBLATT angeschlossene Vakuumleitung sowie eine an einer Hochdruckpumpe angeschlossene Druckgasleitung auf. Innerhalb der Druckkammer befindet sich ein Proben¬ behalter zur Aufnahme zu sinternder Grünkörper, die der Form des späteren Sinterkörpers entsprechen. Der Probenbehalter ist auf Sinter-und HIP-Temperatur erhitzbar.REPLACEMENT LEAF connected vacuum line and a compressed gas line connected to a high pressure pump. A sample holder for receiving green bodies to be sintered, which correspond to the shape of the later sintered body, is located within the pressure chamber. The sample container can be heated to the sintering and HIP temperature.
In eine derart ausgebildete Druckkammer ist gemäß der Erfindung nach Patentanspruch 4 eine Spülgaslei¬ tung eingeführt, die am Probenbeh lter derart mündet, daß über die Spülgasleitung während des Sinterns in die Druckkammer bei niedrigem Druck ein Spülgas einströmen und das zu sinternde pulverförmige Ma¬ terial umgeben kann.In a pressure chamber designed in this way, a flushing gas line is introduced according to the invention according to claim 4, which opens at the sample container in such a way that a flushing gas flows in at low pressure via the flushing gas line during sintering into the pressure chamber and surrounds the powdery material to be sintered can.
Die Spülgasleitung mündet in weiterer Ausgestaltung der Druckkammer nach Patentanspruch 5 in einer am Probenbehalter vorhandenen Spülgaskammer. Aus dieser strömt das Spülgas zu den Grünkörpern.In a further embodiment of the pressure chamber, the purge gas line opens into a purge gas chamber provided on the sample container. The purge gas flows from this to the green bodies.
Die Erfindung wird nachfolgend anhand eines Ausfüh¬ rungsbeispiels näher erläutert. Die Zeichnung zeigt schematisch eine Druckkammer mit einem zum Sintern geeigneten Formbehälter.The invention is explained in more detail below on the basis of an exemplary embodiment. The drawing shows schematically a pressure chamber with a mold container suitable for sintering.
In der Zeichnung ist ein Druckbehälter 1 dargestellt, dessen Druckkammer 2 thermisch gegenüber der Umge¬ bung isoliert ist. Innerhalb der Druckkammer 2 sind elektrische Heizelemente 3, 4 angeordnet. Die Heiz¬ elemente 3 beheizen eine obere, die Heizelemente 4 eine vertikal darunter liegende Heizzone in der Druckkammer. Die Heizzonen sind in der Zeichnung mit Bezugsziffern 5 und 6 angegeben.A pressure vessel 1 is shown in the drawing, the pressure chamber 2 of which is thermally insulated from the environment. Electrical heating elements 3, 4 are arranged within the pressure chamber 2. The heating elements 3 heat an upper, the heating elements 4 a vertically below heating zone in the pressure chamber. The heating zones are indicated in the drawing with reference numbers 5 and 6.
ERSATZBLATT Die Isttemperatur In den Heizzonen wird durch Ther¬ moelemente 7 bis 9 ermittelt. Ein Regler 10 der das Ein- und Ausschalten der Heizele te 3, 4 steuert, regelt die Temperatur in der Druckkammer 2 über die Thermoelemente 7 bis 9 auf eine vorgegebene Solltem- peratur. Der Druck in der Druckkammer 2 wird außer¬ halb des Druckbehälters ermittelt.REPLACEMENT LEAF The actual temperature in the heating zones is determined by thermocouples 7 to 9. A controller 10 which controls the switching on and off of the heating elements 3, 4 regulates the temperature in the pressure chamber 2 via the thermocouples 7 to 9 to a predetermined target temperature. The pressure in the pressure chamber 2 is determined outside the pressure vessel.
Die Druckkammer 2 ist einerseits an einer Vakuumlei- tuπg 11 mit Vakuumventil 12 angeschlossen, anderer¬ seits mit einer Druckgasleitung 13 mit DruckventilThe pressure chamber 2 is connected on the one hand to a vacuum line 11 with a vacuum valve 12, and on the other hand to a pressure gas line 13 with a pressure valve
14 verbunden. Es lassen sich in der Druckkammer Vakua14 connected. It can be vacuumed in the pressure chamber
_3 bis unter 10 mbar und Drücke bis zu 400 MPa ein¬ stellen ._3 to below 10 mbar and pressures up to 400 MPa.
Innerhalb der Heizzonen 5, 6 befindet sich ein ver¬ schiebbarer Ladetisch 15 mit einem Probenbehalter 16 zur Aufnahme von Grünkörpern 17 aus zu sintern¬ dem pulverförmigen Material. Die Grünkörper 17 wei¬ sen die Vorform des zu fertigenden Sinterkörpers auf, sie sind offenporig.Within the heating zones 5, 6 there is a sliding loading table 15 with a sample holder 16 for receiving green bodies 17 made of powdered material to be sintered. The green bodies 17 have the preform of the sintered body to be produced, they are open-pore.
In den Probenbehalter 16 führt eine Spülgasleitung 18 zur Spülung des Probeπbehälters mit Argon. Das Spülgas strömt in eine Spülgaskammer 19 ein und wird aus dieser zu den Grünkörpern 17 geführt. Nach Umströmen der Grünkörper wird das Spülgas über eine Absaugleitung 20 aus dem Proben behälter 16 wieder abgezogen. Die Temperatur des Spülgases nach Durch¬ tritt des pulverförmigen Materials wird von einem Thermoelement 21 gemessen. Das abgezogene Spülgas strömt über die Absaugleitung 20 zu einem Gasanaly- sator 22 und wird dort auf seine Verunreinigungen hin untersucht.A purge gas line 18 leads to the sample container 16 for purging the sample container with argon. The purging gas flows into a purging gas chamber 19 and is guided out of this to the green bodies 17. After flowing around the green body, the purge gas is withdrawn from the sample container 16 via a suction line 20. The temperature of the purge gas after passage of the powdery material is measured by a thermocouple 21. The purge gas drawn off flows via the suction line 20 to a gas analyzer 22 and is examined there for its impurities.
ERSATZBLÄΓT Der Druckbehälter 1 weist thermische Isolierbleche 23 auf, die die Druckkammer 2 nach außen gegen Wär¬ meverluste schützen.SPARE BLADE The pressure vessel 1 has thermal insulating plates 23 which protect the pressure chamber 2 against heat losses to the outside.
Im Ausführungsbeispiel wurden Grünkörper aus U 700 (UDIMET 700) hergestellt. Das pulverförmige Material für die Grünkörper wies eine mittleren Pulverkorn¬ größe von < 45 μm auf. Es wurden zylindrisch geform¬ te Grünkörper zur Herstellung von ringförmigen Sin¬ terstücken eingesetzt. Die Grünkörper wurden im Pro¬ benbeh lter 16 aufeinandergeschichtet und unter Ein¬ leitung von Argon unter Vakuum bei einem Druck von 10 mbar und einer Temperatur von 1270°C eine halbe Stunde gesintert.In the exemplary embodiment, green bodies were produced from U 700 (UDIMET 700). The powdery material for the green bodies had an average powder grain size of <45 μm. Cylindrical green bodies were used to produce ring-shaped sintered pieces. The green bodies were stacked on top of one another in the sample container 16 and sintered for half an hour while introducing argon under vacuum at a pressure of 10 mbar and a temperature of 1270 ° C.
Nach Beendigung des Sintervorgangs wurden die Sinter¬ zwischenprodukte ohne vorhergehende Entnahme aus der Druckkammer 2 und ohne Zwischenkühlung bei einer Temperatur von 1150°C und einem Druck von 150 MPa heißisostatisch gepreßt. Der HIP-Vorgang dauerte 3 Stunden.After the sintering process had ended, the sintered intermediate products were hot isostatically pressed without prior removal from the pressure chamber 2 and without intermediate cooling at a temperature of 1150 ° C. and a pressure of 150 MPa. The HIP process took 3 hours.
Die gefertigten Werkstückringe wiesen theoretische Dichte auf .The manufactured workpiece rings had a theoretical density.
ERSATZBLATT REPLACEMENT LEAF
Claims
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE59107394T DE59107394D1 (en) | 1990-12-22 | 1991-12-17 | METHOD AND DEVICE FOR PRODUCING HIGH DENSITY SINTER WORKPIECES |
| EP92901336A EP0563140B1 (en) | 1990-12-22 | 1991-12-17 | Process and device for manufacturing high-density sintered products |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEP4041514.7 | 1990-12-22 | ||
| DE4041514A DE4041514C2 (en) | 1990-12-22 | 1990-12-22 | Process for producing dense sintered workpieces |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO1992011106A1 true WO1992011106A1 (en) | 1992-07-09 |
Family
ID=6421243
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/DE1991/000983 Ceased WO1992011106A1 (en) | 1990-12-22 | 1991-12-17 | Process and device for manufacturing high-density sintered products |
Country Status (3)
| Country | Link |
|---|---|
| EP (1) | EP0563140B1 (en) |
| DE (2) | DE4041514C2 (en) |
| WO (1) | WO1992011106A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013167289A1 (en) * | 2012-05-05 | 2013-11-14 | Wdt-Wolz-Dental-Technik Gmbh | Sintered insert for a sintering furnace for the oxygen-free sintering of metal or ceramic material |
| EP2868407A3 (en) * | 2013-11-04 | 2015-11-25 | Thermo-Star GmbH | Sintering device |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1590953A (en) * | 1977-10-04 | 1981-06-10 | Powdrex Ltd | Making articles from metallic powder |
| DE3808123A1 (en) * | 1988-03-11 | 1988-07-07 | Krupp Gmbh | Process for producing sintered parts of finely particulate metal or ceramic powders |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS526716A (en) * | 1975-06-30 | 1977-01-19 | Gen Electric | Silicon carbide sintered articles |
| SE447610B (en) * | 1985-04-02 | 1986-11-24 | Asea Atom Ab | SET TO MANUFACTURE SINTERED NUCLEAR FUEL BODIES |
-
1990
- 1990-12-22 DE DE4041514A patent/DE4041514C2/en not_active Expired - Fee Related
-
1991
- 1991-12-17 EP EP92901336A patent/EP0563140B1/en not_active Expired - Lifetime
- 1991-12-17 DE DE59107394T patent/DE59107394D1/en not_active Expired - Fee Related
- 1991-12-17 WO PCT/DE1991/000983 patent/WO1992011106A1/en not_active Ceased
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1590953A (en) * | 1977-10-04 | 1981-06-10 | Powdrex Ltd | Making articles from metallic powder |
| DE3808123A1 (en) * | 1988-03-11 | 1988-07-07 | Krupp Gmbh | Process for producing sintered parts of finely particulate metal or ceramic powders |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013167289A1 (en) * | 2012-05-05 | 2013-11-14 | Wdt-Wolz-Dental-Technik Gmbh | Sintered insert for a sintering furnace for the oxygen-free sintering of metal or ceramic material |
| EP2868407A3 (en) * | 2013-11-04 | 2015-11-25 | Thermo-Star GmbH | Sintering device |
Also Published As
| Publication number | Publication date |
|---|---|
| DE59107394D1 (en) | 1996-03-21 |
| DE4041514A1 (en) | 1992-07-02 |
| EP0563140A1 (en) | 1993-10-06 |
| DE4041514C2 (en) | 1995-05-24 |
| EP0563140B1 (en) | 1996-02-07 |
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