EP0438338B1 - Procédé d'obtention d'un produit à partir de poudres préalliées et produit obtenu à partir dudit procédé - Google Patents

Procédé d'obtention d'un produit à partir de poudres préalliées et produit obtenu à partir dudit procédé Download PDF

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Publication number
EP0438338B1
EP0438338B1 EP91400064A EP91400064A EP0438338B1 EP 0438338 B1 EP0438338 B1 EP 0438338B1 EP 91400064 A EP91400064 A EP 91400064A EP 91400064 A EP91400064 A EP 91400064A EP 0438338 B1 EP0438338 B1 EP 0438338B1
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EP
European Patent Office
Prior art keywords
alloy
temperature
compaction
low pressure
treatment
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.)
Expired - Lifetime
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EP91400064A
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German (de)
English (en)
French (fr)
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EP0438338A1 (fr
Inventor
James Davidson
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TECPHY
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TECPHY
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0433—Nickel- or cobalt-based alloys
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14—Treatment of metallic powder
    • B22F1/142—Thermal or thermo-mechanical treatment

Definitions

  • the present invention relates to a process for obtaining a product from pre-alloyed powders, and more particularly to a process for obtaining in which the powders are subjected to a densification treatment.
  • the present invention also relates to the products obtained using said process.
  • powder metallurgy in development for several years, allows in particular the manufacture of parts, from metals, impossible or difficult to implement otherwise, for example in super-refractory alloys. As a result, powder metallurgy has, in particular, important applications in the field of aeronautical manufacturing (parts of turbines).
  • An object of the invention is to provide a process for obtaining products from pre-alloyed powders made of super-refractory alloy which overcomes these drawbacks.
  • the invention proposes a process for obtaining comprising treatments intended to increase the size of the grains, the size powder particles being nevertheless always initially limited by sieving, and the scale of segregations being reduced to dimensions which do not exceed the size of said particles.
  • the Applicant has observed that during the densification steps, for example by hot isostatic compaction or by spinning, the elements segregated on the surface of the powder particles (mainly carbon and oxygen ) precipitated there, thus forming stable networks which cannot be absorbed by further processing.
  • One consequence of this phenomenon is to promote interparticle ruptures and to make it impossible to magnify the grain.
  • the grain is limited to the size of the initial powder particles.
  • the invention proposes a process for obtaining one of which is a treatment making it possible to attenuate the "decoration" of the particles by precipitation of the segregated elements.
  • the solution adopted by the applicant consists in subjecting, before compaction, the powders of the alloy to heat treatments under low pressure (or without pressure) by which the segregated elements precipitate internally, in phases stable at temperature. compaction and no longer during compaction on the surface of the particles.
  • the Applicant has also observed that the grain enlargement treatments by temperature rise were limited by burning phenomena, that is to say the start of local melting, which prevented bring the powder alloy to the desired temperatures.
  • the invention proposes, in combination with the aforementioned non-pressure or low-pressure treatments, to subject the powders or alloys to homogenization treatments, intended to structurally standardize the materials, in order to ascend as much as possible the temperature where these burning phenomena appear.
  • the homogenization treatments according to the invention are heat treatments above the Solvus temperature of the alloy.
  • the subject of the invention is therefore a method of improving the behavior at high temperatures of a product obtained by a hot densification treatment of a pre-alloyed powder, said powder being subjected, in a manner known per se, to a heat treatment carried out, before the densification treatment, under low pressure (or without pressure), so as to allow the precipitation of elements segregated in stable phases.
  • the pre-alloyed powder consists of an alloy with structural hardening and the pretreatment under low pressure is carried out at a temperature allowing the precipitation of segregations in stable phases inside the powder particles and the densification treatment at high temperature and under pressure comprises at least one step of enlarging the metallurgical grains up to a size exceeding the limits of the particles.
  • the temperature at which the pretreatment is carried out under low pressure is between the Solvus temperature of the alloy reduced by approximately 100 ° C. and its melting temperature.
  • the powder is subjected to a heat treatment of homogenization at a temperature higher than the Solvus temperature of the alloy.
  • the densification treatment comprises a step of compaction at low pressure.
  • the densification treatment includes a consolidation step, in particular by hot isostatic compaction or by spinning.
  • Processing densification can include both a low pressure compaction step and a later consolidation step.
  • the heat treatment at a temperature above the Solvus temperature of the alloy is carried out after the densification treatment.
  • the heat treatment at a temperature higher than the Solvus temperature of the alloy is carried out during the pre-treatment without pressure or under low pressure and / or during the densification treatment.
  • the consolidation step can in particular comprise an isostatic compaction at a temperature higher than the Solvus temperature of the alloy.
  • the subject of the invention is also a product of structural hardening alloy obtained from such a process, and more particularly of product of nickel-based super-refractory alloy.
  • yet another object of the invention is the use of products obtained using said process, in critical parts operating at high temperatures, for example above 650 ° C., and more particularly the use of such products for the manufacture of critical parts in the field of aeronautical construction.
  • the process according to the invention was used to obtain a first alloy known under the trade name ASTROLOY® (registered trademark), the weight composition of which is as follows: 0.040% zirconium: 0.023% boron ; 0.020% carbon; 3.5% titanium; 4% aluminum; 5% molybdenum; 15% chromium; 17% cobalt; nickel balance.
  • ASTROLOY® registered trademark
  • This alloy has a Solvius temperature of 1140 ° C.
  • a classic process for obtaining a product based on pre-alloyed powders in the aforementioned weight proportions, consists of a densification treatment at high temperature and under pressure, for example a heat treatment under 100 MPa for six hours.
  • Table A gives, in ASTM standard, the grain sizes obtained as a function of the temperature of this heat treatment, this from powder particles having an average diameter less than 75 micrometers.
  • TABLE A ASTROLOY Treatment (s) Grain sizes in ASTM standard State of the art processes 1120 ° C 6h 100 MPa 10 1160 ° C 6h 100 MPa 7 1200 ° C 6h 100 MPa 6
  • An example of a process for obtaining according to the invention consists, for its part, of a preliminary heat treatment of the powders under low pressure (less than 1 atm) or without pressure for 24 hours, then in a densification heat treatment, a stage is a stage of hot isostatic compaction, under 100 MPa for six hours, at 1160 ° C., this stage of hot isostatic compactin being able to be followed by a treatment, for four hours at a temperature of 1200 ° C.
  • the results on the grain sizes are still very much improved when the obtaining process comprises a final treatment step at 1200 ° C., the metallurgical grain sizes produced being able to go up to a value of 1 in ASTM standard.
  • FIG. 1 represents a micrograph of an ASTROLOY alloy obtained from that of the methods according to the invention cited in table B, which comprises a final processing step at 1200 ° C, it can be seen that the metallurgical grains, the limits of which appear in solid lines, have developed beyond the initial limits of the powder particles, which can be seen in dotted lines on the micrograph, due to the persistence low decorations despite the implementation process.
  • the process according to the invention was also applied to obtain a second alloy known under the trade name N18, the weight composition of which is as follows: 0.030% zirconium; 0.015% boron; 0.015% carbon; 0.25% hafnium; 4.35% titanium; 4.35% aluminum; 6.5% molybdenum; 11.5% chromium; 15.7% cobalt; nickel balance.
  • This alloy has a Solvus temperature of 1195 ° C.
  • Table C gives the grain sizes obtained for this second alloy, from conventional production methods, that is to say by hot isostatic compaction at 100 MPa, for six hours, for different compaction temperatures, the initial powders with an average diameter of less than 75 ”m.
  • Table D gives, for its part, values of grain sizes of alloys produced for initial powders of similar dimensions, from production methods in accordance with the invention. These production methods each include thermal pretreatments under low pressure (less than 1 atm) or without pressure, followed by a densification treatment. Such densification treatment may include a consolidation step by conventional hot isostatic compaction, whether or not followed by a subsequent consolidation step. The densification treatment can also consist of an isostatic compaction step under low pressure, followed by a posterior compaction step.
  • Figures 3 and 4 respectively represent micrographs of an alloy N18 treated according to, on the one hand, the state of the art at 1160 ° C, for 6 hours, under 100 MPa, and, according to, on the other hand, a process in accordance with the invention consisting of a pretreatment at 1170 ° C for 24 hours, followed by isostatic compaction at low pressure at 1170 ° C, for 4 hours at 10 MPa, followed by further compaction after 1200 ° C, for 6 hours at 100 PMa, we see that l 'We clearly see in Figure 4, the limits of the metallurgical grains formed in the alloy by the process of obtaining according to the invention, while these same limits are difficult to distinguish on the micrograph shown in Figure 3, c 'is to say on the alloy obtained by a process according to the state of the art. The grains of the alloys obtained with the process according to the invention are very much higher than those obtained with the process according to the state of the art.
  • Figure 2 is a graph giving the grain size, in ASTM standard, of the alloys obtained using a process according to the invention, as a function of the pre-treatment temperature to which said alloys are subjected for 24 hours, this pretreatment having been followed by a step of hot isostatic compaction at 1120 ° C, for six hours, under 100 MPa, extended by a step of compaction after 1200 ° C for six hours, at 100 MPa, there is a significant increase in the value of the grain sizes when the temperature of the initial pretreatment is above the Solvus temperature of the alloy (1195 ° C.).

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)
EP91400064A 1990-01-16 1991-01-11 Procédé d'obtention d'un produit à partir de poudres préalliées et produit obtenu à partir dudit procédé Expired - Lifetime EP0438338B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9000454A FR2657032A1 (fr) 1990-01-16 1990-01-16 Procede d'obtention d'un produit a partir de poudres prealliees et produit obtenu a partir dudit procede.
FR9000454 1990-01-16

Publications (2)

Publication Number Publication Date
EP0438338A1 EP0438338A1 (fr) 1991-07-24
EP0438338B1 true EP0438338B1 (fr) 1995-06-07

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP91400064A Expired - Lifetime EP0438338B1 (fr) 1990-01-16 1991-01-11 Procédé d'obtention d'un produit à partir de poudres préalliées et produit obtenu à partir dudit procédé

Country Status (4)

Country Link
US (1) US5395464A (enrdf_load_stackoverflow)
EP (1) EP0438338B1 (enrdf_load_stackoverflow)
DE (1) DE69110139T2 (enrdf_load_stackoverflow)
FR (1) FR2657032A1 (enrdf_load_stackoverflow)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5462808A (en) * 1993-09-03 1995-10-31 Sumitomo Metal Industries, Ltd. Highly rigid composite material and process for its manufacture
FR2935396B1 (fr) * 2008-08-26 2010-09-24 Aubert & Duval Sa Procede de preparation d'une piece en superalliage base nickel et piece ainsi obtenue.
US10245639B2 (en) 2012-07-31 2019-04-02 United Technologies Corporation Powder metallurgy method for making components
US10247480B2 (en) 2017-04-28 2019-04-02 General Electric Company High temperature furnace

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3702791A (en) * 1970-04-20 1972-11-14 Nasa Method of forming superalloys
JPS55161002A (en) * 1979-06-01 1980-12-15 Kobe Steel Ltd Steel powder for powder metallurgy
US4732622A (en) * 1985-10-10 1988-03-22 United Kingdom Atomic Energy Authority Processing of high temperature alloys
US5009704A (en) * 1989-06-28 1991-04-23 Allied-Signal Inc. Processing nickel-base superalloy powders for improved thermomechanical working

Also Published As

Publication number Publication date
US5395464A (en) 1995-03-07
FR2657032B1 (enrdf_load_stackoverflow) 1995-01-27
FR2657032A1 (fr) 1991-07-19
DE69110139T2 (de) 1996-01-04
EP0438338A1 (fr) 1991-07-24
DE69110139D1 (de) 1995-07-13

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