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  • C22C33/00—Making ferrous alloys
  • C22C33/02—Making ferrous alloys by powder metallurgy
  • C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
  • C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
  • C22C33/0285—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5% with Cr, Co, or Ni having a minimum content higher than 5%
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  • 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
  • B22F3/1017—Multiple heating or additional steps
  • B22F3/1028—Controlled cooling
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  • 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
  • B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
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  • 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
  • B22F3/24—After-treatment of workpieces or articles
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  • B22F9/00—Making metallic powder or suspensions thereof
  • B22F9/02—Making metallic powder or suspensions thereof using physical processes
  • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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  • 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
  • B22F9/00—Making metallic powder or suspensions thereof
  • B22F9/02—Making metallic powder or suspensions thereof using physical processes
  • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
  • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
  • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C33/00—Making ferrous alloys
  • C22C33/02—Making ferrous alloys by powder metallurgy
  • C22C33/0207—Using a mixture of pre-alloyed powders or a master alloy
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  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C38/00—Ferrous alloys, e.g. steel alloys
  • C22C38/001—Ferrous alloys, e.g. steel alloys containing N
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  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C38/00—Ferrous alloys, e.g. steel alloys
  • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C38/00—Ferrous alloys, e.g. steel alloys
  • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C38/00—Ferrous alloys, e.g. steel alloys
  • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C38/00—Ferrous alloys, e.g. steel alloys
  • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C38/00—Ferrous alloys, e.g. steel alloys
  • C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
  • C22C38/105—Ferrous alloys, e.g. steel alloys containing cobalt containing Co and Ni
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C38/00—Ferrous alloys, e.g. steel alloys
  • C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C38/00—Ferrous alloys, e.g. steel alloys
  • C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
• • 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
  • B22F1/05—Metallic powder characterised by the size or surface area of the particles
  • B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
• • 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
  • B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
  • B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
• • 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
  • B22F3/24—After-treatment of workpieces or articles
  • B22F2003/248—Thermal after-treatment
• • 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
  • B22F9/00—Making metallic powder or suspensions thereof
  • B22F9/02—Making metallic powder or suspensions thereof using physical processes
  • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
  • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
• • 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
  • B22F9/00—Making metallic powder or suspensions thereof
  • B22F9/02—Making metallic powder or suspensions thereof using physical processes
  • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
  • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
  • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
  • B22F2009/0824—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid
• • 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
  • B22F2301/00—Metallic composition of the powder or its coating
  • B22F2301/35—Iron
• • 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
  • B22F2304/00—Physical aspects of the powder
  • B22F2304/10—Micron size particles, i.e. above 1 micrometer up to 500 micrometer
• • 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
  • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
  • B22F2998/10—Processes characterised by the sequence of their steps
• • 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
  • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

Definitions

• the subject of the invention is a steel with high mechanical characteristics and its method of manufacture.
• Known steels with high mechanical characteristics include in particular maraging steels.
• the name Maraging results from the contraction between the English words “martensitic” and “ageing” to signify that they are steels with a martensitic structure, therefore with a high Nickel content, which have been subjected to an aging treatment of the tempering type.
• Such treatments have the effect of causing intergranular precipitation which increases the tensile strength of the steel while maintaining a significant hardness.
• Maraging steels can thus have a tensile strength close to 2500 MegaPascals and their hardness is close to 500 Hv.
• Known maraging steels are most often produced by forging or casting. They are generally classified according to the American numbering Mxxx in which xxx gives the nominal stress at the maximum tensile stress that the material can undergo, stress expressed in the Anglo-Saxon unit ksi (kilo pound/square-inch) which converts in international units MegaPascals (MPa) by the expression:
• Maraging M200, M300, M400 steels are thus commercially available, which have maximum tensile stresses which are respectively 1379 MPa, 2069 MPa and 2758 MPa.
• This material is produced by casting followed by forging and homogenization heat treatment (1100°C for 24 hours), followed by quenching. This hot treatment is followed by a cold treatment by torsion at high pressure, itself followed by annealing.
• the subject of the invention is a steel with high mechanical characteristics which is characterized in that it has the following mass composition: 12% to 25% Nickel; 7.4% to 20% Cobalt; 3% to 11% Molybdenum; 0.2% to 2.21% of addition elements; and iron supplement.
• Such a composition makes it possible to obtain a steel with high mechanical characteristics (maraging type) whose maximum tensile stress varies from 1300 MPa to 2800 MPa.
• the structure of the material according to the invention also comprises a combination of fine grains and ultrafine grains, the so-called fine grains having a particle size between 1.2 micrometers and 3 micrometers and the so-called ultrafine grains having a particle size between 0.2 micrometers and 1 micrometers, the proportion of ultrafine grains being between 55% and 65% (range centered around 60%).
• the fine grains give the material the stability of plastic deformation before the maximum tensile stress.
• the ultra-fine grains give the material its high mechanical resistance.
• the steel with high mechanical characteristics according to the invention may have the following mass composition: 12% to 25% Nickel; 7.4% to 20% Cobalt; 3% to 11% Molybdenum; 0.15% to 1.6% Titanium; 0.05% to 0.2% Aluminum; from 0% to 0.1% of Silicon and/or Manganese; from 0% to 0.08% Nitrogen and/or Oxygen; from 0% to 0.03% Carbon; from 0% to 0.01% Sulfur and/or Phosphorus; and iron supplement.
• the steel with high mechanical characteristics according to the invention may have the following mass composition: 15.7% Nickel; 7.4% Cobalt; 4.8% Molybdenum; 0.6% Titanium; 0.05% to 0.2% Aluminum; from 0% to 0.1% of Silicon and/or Manganese; from 0% to 0.08% Nitrogen and/or Oxygen; from 0% to 0.03% Carbon; from 0% to 0.01% Sulfur and/or Phosphorus; and iron supplement.
• the material according to the invention is produced in a preferred way by the metallurgy of alloyed steel powders, that is to say by a sintering process and in particular the process known under the name of SPS flash sintering (Spark Plasma Sintering).
• the process for manufacturing a steel with high mechanical characteristics is characterized in that it comprises the following steps: - production of a steel powder having the desired composition, for example by gas atomization, and having a particle size between 5 and 100 micrometers; - mechanical grinding by a planetary ball mill until a powder is obtained whose particle size combines fine grains (particle size between 1.2 and 3 micrometers) and ultrafine grains (particle size between 0.2 micrometers and 1 micrometer ), the proportion of ultrafine grains being between 55% and 65% (range centered around 60%); - mixing of the powders obtained; - sintering of the powder mixture by SPS flash sintering technology, so as to produce a steel block.
• the alloy powders having the desired composition are produced by a conventional process for producing powders.
• a process is also known in which the atomization is done by a rotating electrode spraying molten material by the action of centrifugal force in the form of droplets.
• the powders having the desired composition are then mechanically ground by a planetary ball mill until a powder is obtained whose particle size combines fine grains (particle size between 1.2 micrometers and 3 micrometers) and ultrafine grains (particle size between between 0.2 micrometers and 1 micrometer), with the proportion of fine grains being between 55% and 65% (range centered around 60%).
• Planetary ball mills are well known. It will be possible to implement a high-energy planetary mill of the P4 type marketed by the company Fritsch comprising a plate on which two bowls are fixed and rotate in opposite directions. Such planetary mills are for example described by utility models DE202005015896-U1 and DE202006006747-U1 and by patent EP2010329.
• the grinding powders are placed in bowls made of hardened steel and which contain balls, themselves of hardened steel.
• the bowls are rotated at a speed ⁇ which is of opposite sign to the speed of rotation ⁇ of the plate carrying the bowls.
• the planetary mill may have a plate having a diameter of the order of 800 mm, the rotation of the plate having a speed of between 50 revolutions/minute and 350 revolutions/minute, whereas the rotation of the bowls is between -50 revolutions/minute and -350 revolutions/minute, the ratio between the mass of the balls arranged in each bowl and the mass of powder in the said bowl being between 4 and 10.
• the volume of the bowls can be chosen between 30 milliliters and 1 litre.
• the number of bowls is two or four depending on the model of planetary mill used.
• the grinding can be carried out for a period of 2 to 4 hours.
• the grinding conditions obtained with planetary mills are friction type. They make it possible to obtain a powder combining fine grains and ultrafine grains with a proportion of the order of 60% (by mass) of ultrafine grains for 40% (by mass) of fine grains.
• the particle size of the fine grains being furthermore comprised between 1.2 micrometers and 3 micrometers and that of the ultrafine grains comprised between 0.2 micrometers and 1 micrometer.
• the proportions of ultrafine grains may vary between 55% and 65% (range centered around 60%).
• the powders are mixed, for example using a three-dimensional motion mixer, such as that marketed under the Turbula brand.
• the powders are sintered using flash sintering technology (of the Spark Plasma Sintering type).
• This well-known technique makes it possible to limit the enlargement of the grains and therefore to preserve the particle sizes of the fine and ultrafine structures of the powders obtained by grinding.
• the flash sintering cycle will include: - a rise to an austenitization temperature (greater than 820°C) with a rise rate of between 25°C/minute and 200°C/minute; - a plateau lasting 5 to 20 minutes at the austenitization temperature; - cooling to room temperature at a cooling rate of between 25°C/minute and 200°C/minute.
• the axial force applied to the block throughout the duration of the cycle may be between 100 kilo Newtons and 1000 kilo Newtons.
• the current has a strong intensity, varying from 1000 to 30000 Amps, with a tension varying from 0 to 10 Volts.
• the desired granular structure is maintained in the block thus produced.
• the steel blocks thus obtained are said to be of "maraging type" because of their composition, but they have not yet undergone tempering treatment.
• This heat treatment may consist of bringing the steel block to a temperature of 480°C for 3 hours.
• This aging heat treatment (also called structural hardening) leads to the precipitation of intermetallic compounds of the Ni 3 Ti and/or Ni 3 Mo and/or Fe 2 Mo type.
• a block of Maraging steel with very high mechanical characteristics is thus obtained.
• the nominal stresses at the maximum tensile force then vary between 1500 MPa and 2900 MPa.
• This first example relates to a material which is produced from powders whose particle size distribution (before grinding) is centered around 37 ⁇ m.
• the chemical composition in mass percentages of these powders is as follows: 15.70 % nickel, 7.40% cobalt, 4.80% molybdenum, 0.60% titanium, 0.05 to 0.20% aluminum rate less than or equal to 0.10% silicon, less than or equal to 0.10% manganese, less than or equal to 0.01% phosphorus, less than or equal to 0.01% sulfur, carbon content less than or equal to 0.03%, rate less than or equal to 0.08% nitrogen, oxygen level less than or equal to 0.08%, balance for iron.
• the powders were ground by a planetary mill with friction type grinding conditions with rotational speeds ⁇ and ⁇ different from 250 rpm and ⁇ 250 rpm, respectively, for a grinding time of less than 4 hours.
• ground powders were then consolidated using flash sintering of the SPS type (Spark Plasma Sintering) under a uniaxial loading of at least 70 MPa (MegaPascals) with a sintering temperature below 950°C and with a temperature rise rate varying from 25°C/minute to 200°C/minute.
• SPS Spark Plasma Sintering
• Sintering is followed by a hold at the austenitization temperature, still under a uniaxial load of at least 70 MPa, the duration of which is between 5 and 20 minutes.
• the block is then gradually cooled to room temperature at a cooling rate varying from 25°C/minute to 200°C/minute.
• Curve 1 corresponds to the steel block according to the invention, curve 2 to the reference steel block.
• the microstructure is of the 100% martensitic type.
• the microstructure in the untreated state consists of the fine and ultrafine microstructures of the ground starting powders.
• the structure will be composed of approximately 40% of fine grains of size 1.8 ⁇ 0.3 micrometers ( ⁇ m) and of approximately 60% of ultrafine grains of size 0.6 ⁇ 0.2 ⁇ m.
• the material is composed of agglomerates of fine grains made up on average of 32 ⁇ 5 grains distributed in a homogeneous way.
• the spacing between the fine grain agglomerates is between 8 and 14 micrometers.
• the second example relates to a steel identical to that of the first example but having undergone, after its production, an aging treatment of the tempered type.
• This aging heat treatment (or structural hardening) of the tempering type was carried out by bringing the steel to a temperature of 480°C for 3 hours.
• Curve 3 corresponds to the steel block according to the invention, curve 4 to the reference steel block.
• the true plastic deformation up to the maximum tensile force ( ⁇ pEM ) is, for the steel according to the invention (curve 3), 300% greater than that of the reference steel (curve 4 ), which is a maraging steel made using the conventional foundry and forging approach.
• the microstructure is of the martensitic type with 10% reversion austenite.
• the microstructure in the treated state retains the fine and ultrafine microstructures of the starting ground powders.
• the structure will be composed of approximately 40% of fine grains of size 1.6 ⁇ 0.4 ⁇ m and of approximately 60% of ultrafine grains of size 0.8 ⁇ 0.2 ⁇ m.
• the material is composed of agglomerates of fine grains made up on average of 25 ⁇ 2 grains distributed in a homogeneous way.
• the spacing between the fine grain agglomerates is between 9 and 15 micrometers.

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• Chemical & Material Sciences (AREA)
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• Metallurgy (AREA)
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• Superconductors And Manufacturing Methods Therefor (AREA)

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• 2020
  • 2020-08-21 FR FR2008546A patent/FR3113495B1/fr active Active
• 2021
  • 2021-08-16 EP EP21777361.3A patent/EP4200455A1/de active Pending
  • 2021-08-16 US US18/021,692 patent/US12601037B2/en active Active
  • 2021-08-16 IL IL300639A patent/IL300639A/en unknown
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