WO2017056512A1 - Procédé de production d'une poudre d'acier allié destinée à la métallurgie des poudres - Google Patents

Procédé de production d'une poudre d'acier allié destinée à la métallurgie des poudres Download PDF

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WO2017056512A1
WO2017056512A1 PCT/JP2016/004441 JP2016004441W WO2017056512A1 WO 2017056512 A1 WO2017056512 A1 WO 2017056512A1 JP 2016004441 W JP2016004441 W JP 2016004441W WO 2017056512 A1 WO2017056512 A1 WO 2017056512A1
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powder
atomized iron
based powder
content
moving bed
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PCT/JP2016/004441
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English (en)
Japanese (ja)
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小林　聡雄
中村　尚道
伊都也 佐藤
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Ｊｆｅスチール株式会社
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Priority to JP2017500094A priority Critical patent/JP6112283B1/ja
Priority to KR1020187008471A priority patent/KR102090035B1/ko
Publication of WO2017056512A1 publication Critical patent/WO2017056512A1/fr

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    • 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
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • 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
    • 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
    • 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
    • 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
    • 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
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/24—Ferrous alloys, e.g. steel alloys containing chromium with vanadium
    • 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
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/38—Ferrous alloys, e.g. steel alloys containing chromium with more than 1.5% by weight of manganese
    • 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
    • B22F2201/00—Treatment under specific atmosphere
    • B22F2201/01—Reducing atmosphere
    • B22F2201/013—Hydrogen
    • 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
    • B22F2203/00—Controlling
    • B22F2203/11—Controlling temperature, temperature profile

Definitions

  • the present invention relates to a method for producing an alloy steel powder for powder metallurgy by reducing atomized iron base powder to produce an alloy steel powder for powder metallurgy, and in particular, the atomized iron base powder contains an easily oxidizable alloy element such as Cr.
  • the present invention relates to a method for producing alloy steel powder for powder metallurgy that can effectively reduce the C (carbon) content and the O (oxygen) content in the alloy steel powder even if contained.
  • Powder metallurgy technology allows parts with complex shapes to be manufactured in a shape very close to the product shape (so-called near net shape) and with high dimensional accuracy. Therefore, if a part is produced using powder metallurgy technology, the cutting cost can be greatly reduced. For this reason, powder metallurgy products to which powder metallurgy technology is applied are used in various fields as various machine parts. Recently, there has been a strong demand for improving the strength of powder metallurgy products in order to reduce the size and weight of parts. In particular, there is a demand for higher strength in iron-based powder metallurgy products (iron-based sintered bodies). Is strong.
  • an alloy element is added to the iron-based powder used in powder metallurgy.
  • the alloy element for example, Cr, Mn, and Mo are used because they have a high effect of improving hardenability and are relatively inexpensive.
  • V is used as an alloy element in order to improve high temperature strength and wear resistance.
  • Examples of the alloy powder for powder metallurgy containing the above alloy elements include Cr—Mo alloy steel powder (Patent Document 1), Cr—Mn—Mo alloy steel powder (Patent Document 2, Patent Document 3), Cr—Mn—Mo—V alloy steel powder (Patent Document 4) is known.
  • heat treatment is performed to reduce the C content and O content in the iron-based powder as a raw material.
  • the heat treatment is generally carried out continuously using a moving bed furnace (moving bed furnace).
  • the iron-based powder include a crude iron-based powder that has been atomized and a roughly reduced iron obtained by roughly reducing a mill scale.
  • a crude iron-based powder such as a base powder is used.
  • at least one treatment of decarburization, deoxidation, and denitrification is performed according to the use of the powder.
  • an apparatus described in Patent Document 5 As an apparatus for performing the above heat treatment, for example, an apparatus described in Patent Document 5 is known.
  • the space in the moving bed furnace is divided into a plurality of partitions by a partition wall provided so as to be perpendicular to the traveling direction of the raw material powder.
  • the flow path for flowing atmospheric gas is provided in the upper part of each divided
  • the heat treatment is continuously performed while flowing the atmospheric gas countercurrently, that is, in a direction opposite to the traveling direction of the raw material powder.
  • Patent Document 5 a heat treatment method as described in Patent Document 5 is used to reduce the C content and O content.
  • it contains elements such as Cr and Mn (hereinafter referred to as “easily oxidizable elements”) that are more easily oxidized than Fe. Therefore, when an iron-based powder containing Cr or Mn is produced by an atomizing method (particularly, a water atomizing method), the obtained iron-based powder contains an oxide formed by oxidation of Cr or Mn during atomization. It will be. The oxide remains without being sufficiently reduced even in the heat treatment.
  • Cr and Mn are further oxidized during the heat treatment, and the amount of oxide is increased.
  • the C content and the O content are large, the compressibility of the alloy steel powder at the time of pressure forming is lowered, so that a large amount of oxide remains is a problem.
  • V used as an alloy element in Patent Document 4 has a property of being more easily oxidized than Cr and Mn. Therefore, V oxide contained in the atomized iron-based powder is removed by a normal heat treatment. It is difficult. Therefore, in Patent Document 4, costly vacuum reduction is performed.
  • Patent Document 6 and Patent Document 7 propose a method that enables decarburization and deoxidation in the production of alloy steel powder containing easily oxidizable elements such as Cr and Mn.
  • the method proposed in Patent Document 7 is a method in which heat treatment is continuously performed using a belt furnace, and thus is suitable for mass production.
  • it is essential to continuously measure the CO or CO 2 concentration or the oxygen potential (O 2 concentration or H 2 / H 2 O concentration ratio) in the atmospheric gas during the heat treatment, Furthermore, it is necessary to adjust the amount of water vapor injected into the furnace so that these measured values become target values.
  • the sensor part is soiled and the gas intake port is clogged, making it impossible to perform measurement normally. There's a problem. Therefore, when the method of Patent Document 7 is continuously performed, maintenance of the analyzer is a heavy burden.
  • the present invention has been made in view of the above circumstances, and is a method for producing alloy steel powder for powder metallurgy using a moving bed furnace, without requiring gas analysis that requires complicated maintenance management, To provide a method for producing an alloy steel powder for powder metallurgy that can heat-treat an iron-based powder containing an easily oxidizable element such as Cr, Mn, V, and stably reduce the C content and the O content. With the goal.
  • the gist of the present invention is as follows. 1. % By mass C: 0.8% or less, O: 1.0% or less, S: 0.3% or less, P: 0.03% or less, and as an alloy element, Mn: more than 0.08% and 1.0% or less, Cr: 0.3 to 3.5%, 1 or 2 or more selected from the group consisting of Mo: 0.1-2% and V: 0.1-0.5%, Prepare the remaining Fe and atomized iron-based powder which is an inevitable impurity, Supplying the atomized iron-based powder into a moving bed furnace so as to form a packed bed of thickness d (mm); In the moving bed furnace, an inert gas is supplied so as to have an average gas flow velocity v (mm / s), The atomized iron-based powder is reduced by heat treatment in the moving bed furnace to obtain an alloy steel powder for powder metallurgy, a method for producing an alloy steel powder for powder metallurgy, Said d and v satisfy
  • an alloy steel powder containing oxidizable elements such as Cr, Mn, and V is heat-treated using a moving bed furnace without performing gas analysis that requires complicated maintenance and management. , C content and O content can be stably reduced. As a result, it is possible to produce alloy steel powder that is low in cost and excellent in compressibility during pressure forming.
  • sintered parts produced using the alloy steel powder for powder metallurgy obtained by the production method of the present invention have excellent mechanical properties such as strength, toughness and fatigue properties. Applications of powders and sintered bodies can be expanded.
  • FIG. 1 It is side sectional drawing which shows the example of the heat processing apparatus which can be used in one Embodiment of this invention. It is a figure which shows the example of the temperature pattern in the heat processing apparatus described in patent document 5.
  • FIG. 1 It is side sectional drawing which shows the example of the heat processing apparatus which can be used in one Embodiment of this invention. It is a figure which shows the example of the temperature pattern in the heat processing apparatus described in patent document 5.
  • alloy steel powder for powder metallurgy (hereinafter sometimes simply referred to as “alloy steel powder”) is produced by heat-treating atomized iron-based powder as a raw material using a moving bed furnace.
  • the production method of the present invention includes the following treatments; (1) Prepare atomized iron-based powder. (2) supplying the atomized iron-based powder into a moving bed furnace so as to form a packed bed having a thickness of d (mm); (3) by supplying an inert gas in the moving bed furnace so as to have an average gas flow velocity v (mm / s); and (4) by heat-treating the atomized iron-based powder in the moving bed furnace. Reduce to alloy steel powder for powder metallurgy.
  • Each of the above processes can be performed independently at an arbitrary timing, and a plurality of processes can be performed simultaneously.
  • the thickness d of the packed bed and the average gas flow velocity v must satisfy the above-described conditions.
  • the atomized iron-based powder is further mixed with a carbon component according to the C content and O content of the atomized iron-based powder, and then the moving bed Supply to the furnace.
  • atomized iron-based powder is used as a raw material.
  • the manufacturing method of the atomized iron-based powder is not particularly limited, and can be manufactured according to a conventional method.
  • “Atomized iron-based powder” means an iron-based powder produced by the atomizing method.
  • the “iron-based powder” means a powder containing 50% by mass or more of Fe.
  • the atomized iron-based powder either a gas atomized iron-based powder obtained by a gas atomizing method or a water atomized iron-based powder obtained by a water atomizing method can be used.
  • the gas atomization method it is preferable to use an inert gas such as nitrogen or argon.
  • gas since gas is inferior in cooling capacity compared to water, it is necessary to use a large amount of gas when producing iron-based powder by the gas atomization method. Therefore, it is preferable to use the water atomization method from the viewpoint of mass productivity and manufacturing cost.
  • the water atomization method is normally performed in an atmosphere in which air is mixed, the iron-based powder is more easily oxidized in the production process than the gas atomization method. Therefore, the method of the present invention is particularly effective when a water atomized iron-based powder is used.
  • C and O are elements to be reduced by a heat treatment described later. And from the viewpoint of improving the compressibility of the finally obtained alloy steel powder for powder metallurgy, it is desirable to reduce the C content and O content of the alloy steel powder as much as possible, specifically, C: 0.1% or less, O: 0.28% or less are preferable. In order to achieve these appropriate amounts of C and O, the amount that can be reduced by the heat treatment according to the present invention is anticipated, and the appropriate ranges of the C content and O content of the atomized iron-based powder are determined as follows.
  • C 0.8% or less C is present in the atomized iron-based powder mainly as a precipitate such as cementite or in a solid solution state.
  • the C content in the atomized iron-based powder exceeds 0.8%, it becomes difficult to lower the C content to 0.1% or less in the heat treatment of the present invention, and an alloy powder having excellent compressibility is obtained. I can't. Therefore, the C content of the atomized iron-based powder is set to 0.8% or less.
  • the lower the C content the easier the reduction (decarburization) of the C content during heat treatment. Therefore, the lower limit of the C content is not particularly limited, and may be 0% or industrially greater than 0%.
  • O 1.0% or less O is mainly present on the surface of the iron-based powder as Cr oxide, Mn oxide, V oxide, and Fe oxide. If the O content in the atomized iron-based powder exceeds 1.0%, it becomes difficult to reduce the O content to 0.28% or less during heat treatment, and an alloy powder having excellent compressibility cannot be obtained. Therefore, the O content of the atomized iron-based powder is set to 1.0% or less. The O content is preferably 0.9% or less. On the other hand, the lower the O content, the easier the reduction (deoxidation) of the O content during heat treatment. Therefore, the lower limit of the O content is not particularly limited, but excessive reduction leads to an increase in manufacturing cost, so the O content is preferably 0.4% or more.
  • the contents of S, P, Cr, Mn, Mo, and V are not changed by the heat treatment of the present invention. Therefore, these elements contained in the atomized iron-based powder remain as they are in the alloy steel powder for powder metallurgy after the heat treatment. Based on this, the contents of these elements in the atomized iron-based powder are respectively defined as follows.
  • the S content in the alloy steel powder is 0.3% or less.
  • the S content in the atomized iron-based powder stage is made 0.3% or less.
  • the S content is preferably set to 0.25% or less.
  • the lower limit of the S content is not particularly limited and may be 0%, but industrially it may be more than 0%. From the viewpoint of improving the machinability after sintering, the S content is preferably 0.05% or more.
  • P 0.03% or less
  • P is an element contained as one of inevitable impurities.
  • the P content of the atomized iron-based powder is set to 0.03% or less.
  • the lower limit of the P content is not particularly limited and may be 0%, but industrially it may be more than 0%. However, excessive reduction leads to an increase in manufacturing cost, so the P content is preferably 0.0005% or more.
  • the atomized iron-based powder in the present invention contains one or more selected from the group consisting of Mn, Cr, Mo, and V in addition to the above components.
  • Mn more than 0.08% and not more than 1.0% Mn is an element having an action of improving the strength of the sintered body by improving hardenability and strengthening solid solution.
  • Mn content shall be over 0.08%.
  • the Mn content is preferably 0.10% or more.
  • the Mn content is higher than 1.0%, the amount of Mn oxide generated increases, and the compressibility of the alloy steel powder decreases. Further, the Mn oxide serves as a starting point for destruction inside the sintered body, and reduces fatigue strength and toughness. Therefore, the Mn content is 1.0% or less.
  • the Mn content is preferably 0.95% or less, and more preferably 0.80% or less.
  • Cr 0.3-3.5%
  • Cr is an element that has the effect of improving hardenability and improving the tensile strength and fatigue strength of the sintered body. Further, Cr has the effect of increasing the hardness after heat treatment such as quenching and tempering of the sintered body and improving the wear resistance. When adding Cr, in order to acquire these effects, Cr content shall be 0.3% or more. On the other hand, when the Cr content exceeds 3.5%, the amount of Cr oxide generated increases. Since the Cr oxide serves as a starting point for fatigue failure inside the sintered body, the fatigue strength of the sintered body is reduced. Therefore, the Cr content is 3.5% or less.
  • Mo 0.1-2%
  • Mo is an element having an action of improving the strength of the sintered body by improving hardenability, solid solution strengthening, precipitation strengthening, and the like.
  • Mo content shall be 0.1% or more.
  • the content of Mo exceeds 2%, the toughness of the sintered body decreases. Therefore, the Mo content is 2% or less.
  • V 0.1-0.5%
  • V is an element having an action of improving the strength of the sintered body by improving hardenability, solid solution strengthening, precipitation strengthening, and the like.
  • V content shall be 0.1% or more.
  • the V content exceeds 0.5%, the toughness of the sintered body decreases. Therefore, the V content is 0.5% or less.
  • the component composition of the atomized iron-based powder in the present invention is composed of the above elements, the remainder Fe and inevitable impurities.
  • the C content [C] (mass%) of the atomized iron base powder and the O content [O] (mass%) of the atomized iron base powder satisfy the following formula (2). There is a need. [O] ⁇ 4/3 [C] -2/15 (2)
  • the C content [C] (mass%) of the atomized iron-based powder and the O content [O] (mass%) of the atomized iron-based powder satisfy the following formula (2):
  • the amount of C in the powder can be reduced to a sufficiently low amount, for example, 0.1% by mass or less.
  • a carbon component is further mixed with the atomized iron-based powder as necessary.
  • the atomized iron base powder is used as it is in the moving bed furnace.
  • “Supply as it is” means that only the atomized iron-based powder is supplied to the moving bed furnace without being mixed with other components such as a carbon component. 4/3 [C] + 0.28 ⁇ [O] (3)
  • the method of adjusting C content and O content of atomized iron-based powder is not specifically limited, Arbitrary methods can be used. For example, what is necessary is just to adjust the component composition of the molten steel used for manufacture of an atomized iron base powder so that C content and O content of atomized iron base powder may satisfy the said conditions. Adjustment of the composition of the molten steel can be performed by a steel refining and steelmaking technique using a general converter.
  • the atomized iron-based powder if the atomized iron-based powder is as-atomized and satisfies the conditions of the above formulas (2) and (3), the atomized iron-based powder can be directly subjected to heat treatment. This is preferable because it is possible. However, if the C content in the atomized iron-based powder becomes excessive and the condition of the formula (2) is not satisfied, the adjustment before the heat treatment cannot be performed to satisfy the formula (2). Therefore, when producing atomized iron-based powder, it is necessary to satisfy the formula (2), and oxygen is allowed to be excessive for that purpose. This is because even if oxygen is excessive and the formula (3) is not satisfied, the amount of C and O in the final alloy steel powder can be reduced by adding the carbon component as described above.
  • the average particle size of the atomized iron-based powder is not particularly limited, and any particle size can be used as long as it is an iron-based powder obtained by the atomization method.
  • the average particle size of the atomized iron-based powder is less than 30 ⁇ m, the fluidity of the atomized iron-based powder is lowered, and it may be difficult to supply to the moving bed furnace using a hopper or the like.
  • the average particle size of the atomized iron-based powder is less than 30 ⁇ m, the fluidity of the alloy steel powder after heat treatment also decreases, so the work efficiency of filling the mold when the alloy steel powder is press-formed decreases. There is a case.
  • the average particle size of the atomized iron-based powder is preferably 30 ⁇ m or more, more preferably 40 ⁇ m or more, and even more preferably 50 ⁇ m or more.
  • the average particle size of the atomized iron-based powder is preferably 120 ⁇ m or less, more preferably 100 ⁇ m or less, and even more preferably 90 ⁇ m or less.
  • the average particle diameter means a median diameter (so-called d50, volume basis).
  • the apparent density of the atomized iron-based powder is not particularly limited, but is preferably 2.0 to 3.5 Mg / m 3 , more preferably 2.4 to 3.2 Mg / m 3 .
  • Atomized iron-based powder having the above component composition is supplied to a moving bed furnace, and a packed bed having a thickness d (mm) is formed on the moving bed of the moving bed furnace.
  • a moving bed furnace any one can be used as long as it can heat treat the atomized iron-based powder, but a moving bed furnace (hereinafter referred to as a “belt type moving bed furnace” or “ It is preferable to use a belt furnace).
  • a moving bed furnace hereinafter referred to as a “belt type moving bed furnace” or “ It is preferable to use a belt furnace).
  • an atomized iron-based powder can be supplied onto the belt to form a packed bed.
  • the atomized iron-based powder can be supplied by any method, but it is preferable to use a hopper.
  • the conveyance direction of the atomized iron-based powder in the moving bed furnace is not particularly limited, but it is generally conveyed linearly from the inlet side to the outlet side of the moving bed furnace. The thickness of the fill
  • the heating system of the moving bed furnace is not particularly limited, and any system can be used as long as it can heat the atomized iron-based powder.
  • the indirect heating system is used. It is preferable to use heating using a radiant tube.
  • a muffle furnace can also be suitably used as an indirect heating furnace.
  • Patent Document 5 As the moving bed furnace, a moving bed furnace as described in Patent Document 5 can be used. Therefore, the moving bed furnace in Patent Document 5 will be described below for reference. However, the atomized iron-based powder and the atmospheric gas used in the present invention are different from the processing in Patent Document 5 described below. The atomized iron-based powder and atmospheric gas used in the present invention will be described later.
  • Patent Document 5 it is assumed that one or more processes of decarburization, deoxidation, or denitrification are continuously performed by using a continuous moving bed furnace to heat-treat the iron-based powder. Further, in the description of Patent Document 5, each of the decarburization, deoxidation, and denitrification treatment steps is made independent using the divided space of the moving bed furnace, and the decarburization step is performed at 600 to 1100 ° C. In the denitrification process, the iron-base powder is heat-treated by controlling the temperature independently at 450 to 750 ° C.
  • Patent Document 5 as an atmospheric gas, a reducing gas such as H 2 or AX gas at decarburization zone or an inert gas such as N 2 or Ar, reduction such as H 2 or AX gas in deoxidation zone It is said that gas mainly composed of H 2 is used in the denitrification zone.
  • FIG. 1 A heat treatment apparatus 100 shown in FIG. 1 is provided on a furnace body 30 divided into a plurality of zones by a partition wall 1, that is, a decarburization zone 2, a deoxidation zone 3, and a denitrification zone 4, and an entrance side of the furnace body 30.
  • the hopper 8 is provided, a wheel 10 provided on the entrance / exit side of the furnace body 30, a belt 9 that continuously rotates by the wheel 10 and circulates in each zone in the furnace body 30, and a radiant tube 11.
  • the product powder 13 is stored in the product tank 14.
  • the reaction in each zone is considered as follows.
  • the ambient temperature is controlled to 600 to 1100 ° C. by the radiant tube 11, and water vapor (H 2 O gas) introduced from the water vapor inlet 12 provided on the downstream side of the decarburization zone 2
  • water vapor H 2 O gas
  • decarburization is performed from the crude iron-based powder while adjusting the atmospheric gas in the deoxidation zone 3 as the next zone to a dew point of 30 to 60 ° C.
  • an atmospheric gas discharge port 6 is provided to discharge the atmospheric gas to the outside of the apparatus.
  • the decarburization reaction formula is represented by the following formula (I).
  • C (in Fe) + H 2 O (g) CO (g) + H 2 (g) (I)
  • the ambient temperature is controlled to 700 to 1100 ° C. by the radiant tube 11, and deoxidation is performed from the crude iron-based powder using the atmospheric gas from the denitrification zone 4 (dew point: hydrogen gas of 40 ° C. or less). Is going to do.
  • the ambient temperature is controlled to 450 to 750 ° C. by the radiant tube 11, and hydrogen gas (dew point: 40 ° C.) as a reaction gas is supplied from the atmosphere gas inlet 5 provided on the downstream side of the denitrification zone 4.
  • hydrogen gas dew point: 40 ° C.
  • the following is introduced to denitrify the crude iron-based powder.
  • the water sealing tank 15 functions to block the mixing of the outside gas into the furnace gas and the leakage of the inside gas to the outside of the furnace.
  • FIG. 5 a typical example of a heat treatment temperature pattern by a belt furnace type heat treatment apparatus described in Patent Document 5 is shown in FIG.
  • the iron-based powder to be treated is first heated in the decarburization zone, then soaked in the deoxidation zone, and finally in the denitrification zone.
  • the hydrogen gas introduced in the direction opposite to the flow of the iron-based powder first enters the denitrification zone, denitrifies the iron-based powder while being heated, and then enters the deoxidation zone and is kept at a constant temperature.
  • the iron-base powder is deoxidized while finally entering the decarburization zone together with a predetermined amount of water vapor, and the iron-base powder is decarburized while being cooled.
  • the inert gas is not particularly limited, and any inert gas can be used.
  • the inert gas that can be suitably used include argon (Ar) gas, nitrogen (N 2 ) gas, and a mixed gas thereof.
  • the inert gas is supplied into the moving bed furnace so as to have an average gas flow velocity v (mm / s) during the heat treatment of the atomized iron-based powder in the moving bed furnace.
  • the inert gas is preferably flowed in the moving bed furnace in a direction opposite to the moving direction of the raw material powder.
  • a conveying means such as a belt
  • the inert gas is introduced from the other end (downstream side) and exhausted from the one end (upstream side). Therefore, it is preferable that the moving bed furnace is provided with an atomized iron-based powder supply port and an atmosphere gas discharge port at one end, and a discharge port and an inert gas supply port for treated powder (alloy steel powder) at the other end.
  • the alloy steel powder for powder metallurgy can be obtained by heat-treating the atomized iron-based powder in the moving bed furnace with the inert gas supplied as described above. By the heat treatment, C and O contained in the atomized iron-based powder are removed by a decarburization and deoxidation (reduction) reaction described later.
  • both the thickness d (mm) of the packed bed and the average gas flow velocity v (mm / s) are controlled so as to satisfy the following expression (1).
  • the heat treatment By performing the heat treatment under the above conditions, it is possible to stably reduce C and O contained in the atomized iron-based powder in spite of the fact that the atomized iron-based powder contains oxidizable elements such as Cr, Mn, and V. it can. As a result, the C content and the O content in the alloy steel powder after the heat treatment can be set to extremely low values such as C ⁇ 0.1% and O ⁇ 0.28%. The reason will be described below.
  • the thickness d of the packed bed and the average gas flow velocity v in the furnace when the inert gas is introduced into the furnace are controlled so as to satisfy the above formula (1).
  • a velocity boundary layer of the flowing inert gas is formed in the space above the surface of the packed bed. It is derived from the theory regarding the boundary layer that the thickness of the velocity boundary layer is inversely proportional to ⁇ v. Further, since the diffusion rate of CO generated by the reduction reaction is considered to be constant regardless of the thickness of the velocity boundary layer, the diffusion time is proportional to the thickness of the velocity boundary layer. Therefore, if the velocity boundary layer thickness is halved and the same diffusion time is given, it is considered that the concentration of CO on the surface of the packed layer is halved. Then, even if the thickness of the packed layer is doubled, It is estimated that the CO concentration in the lowermost layer can be made the same.
  • the packed layer thickness and the velocity boundary layer thickness are inversely proportional, that is, it is estimated that the packed layer thickness and ⁇ v are in a proportional relationship. Therefore, as in the present invention, in the heat treatment, if the packed layer thickness and the gas flow rate are adjusted so that the condition of d / ⁇ v ⁇ 3.0 is satisfied, a gas analyzer that requires complicated maintenance management is required. Even if it is not used, the state in which the CO partial pressure in the furnace atmosphere is lower than the equilibrium CO partial pressure determined by the reactions of the above formulas (a) to (d) is maintained.
  • the lower limit of d / ⁇ v is not particularly limited. The lower the better, the lower the better. However, if d is excessively decreased, the production efficiency decreases, and if v is excessively increased, the cost increases. It is preferable to set it as the above, and it is more preferable to set it as 0.3 or more.
  • the atomized iron-based powder reduced by the heat treatment is further cooled using hydrogen gas or a hydrogen-containing gas.
  • the reason is as follows.
  • the reduced atomized iron-based powder may contain N as an impurity.
  • the N content of the finally obtained alloy steel powder for powder metallurgy may be as high as exceeding 0.005% by mass. .
  • the alloy steel powder contains N, the compressibility is lowered. Therefore, it is preferable to reduce the N content of the alloy steel powder as much as possible. Therefore, if the reduced atomized iron-based powder is cooled using hydrogen gas or a hydrogen-containing gas, N contained in the powder can be removed by the reaction of the following formula (e).
  • N content of the alloy steel powder for powder metallurgy finally obtained shall be 0.005 mass% or less.
  • the gas used for the cooling may be supplied by any method.
  • the inert gas in the moving bed furnace is exhausted at the position where the reduction of the iron-based powder in the moving bed furnace is completed, or at the downstream side in the transport direction from the position, and the cooling gas is transferred to the moving bed furnace. It can be introduced into the furnace.
  • the timing exhaust and introduction position in the moving bed furnace
  • the atmosphere gas can be replaced.
  • C that should be used for reduction of Cr 2 O 3 and MnO reacts with water vapor in the atmosphere and is consumed, or once reduced Cr and Mn are in the atmosphere This is because it is reoxidized by water vapor. In order to efficiently advance the reduction reaction in the heat treatment, it is necessary to suppress such wasteful consumption of C and reoxidation of Cr and Mn.
  • the dew point of the inert gas is set to 5 ° C. or less.
  • the dew point of the inert gas is preferably 5 ° C. or less, more preferably ⁇ 10 ° C. or less as described above.
  • the dew point of the inert gas The lower the dew point of the inert gas, the better the deoxidation reaction will proceed.
  • a gas with a low dew point is expensive, and the use of a gas with an excessively low dew point causes an increase in production cost. Therefore, it is usually preferable to set the dew point to ⁇ 40 ° C. or higher.
  • the moving bed furnace includes a sealing unit for preventing gas leakage and intrusion.
  • a sealing unit for example, a water-sealed tank (15 in FIG. 1) as described in Patent Document 5 can be used, but it is more preferable to use a system that does not use water such as a seal roll.
  • the sealing means is preferably provided at both ends on the upstream side and the downstream side in the transport direction.
  • the atmospheric temperature is preferably set to 1080 ° C. or higher.
  • the upper limit of the ambient temperature is not particularly limited, but is preferably about 1200 ° C. in consideration of the heat resistance performance of the apparatus, the manufacturing cost, and the like.
  • the “atmosphere temperature” is a temperature measured by a thermocouple at a position 20 mm immediately above the surface of the iron-based powder (packed bed) in the moving bed furnace.
  • Holding time t 10 4 -0.0037 ⁇ T (h) or more If the holding time t is 10 4 -0.0037 ⁇ T (h) or more according to the ambient temperature T (° C.), O Since it can reduce more, it is preferable.
  • the relationship between the said t and T was determined from the result of having conducted the experiment which manufactures alloy steel powder with various T and t. Specifically, the O content of the obtained alloy steel powder was plotted on a Tt diagram, and a curve (contour line) connecting the same oxygen content was determined as an approximate expression.
  • the upper limit of the retention time is not particularly limited, but the retention time is preferably 4 hours or less because the production cost only increases even if the retention time is longer than the time required for completion of the deoxidation reaction.
  • Example 1 An atomized iron-based powder having the component composition shown in Table 1 was produced by the water atomization method. Atomized iron-based powder symbols: A, B, F, I, and M satisfy [O] ⁇ 4/3 [C] ⁇ 2/15, but 4/3 [C] + 0.28 ⁇ [ O] is not satisfied, and O is excessive. Therefore, in order to adjust the C amount and O amount after heat treatment to an appropriate range, an appropriate amount of carbon component, for example, carbon powder such as graphite powder is adjusted before heat treatment. Mixing is necessary.
  • Atomized iron-based powder symbols C to E, G, H, and J satisfy both [O] ⁇ 4/3 [C] ⁇ 2/15 and 4/3 [C] + 0.28 ⁇ [O] It is not necessary to mix carbon powder before heat treatment.
  • the atomized iron-based powder is supplied into the moving bed furnace so as to have the packed bed thickness d shown in Tables 2 and 3, and the average gas flow velocity v shown in Tables 2 and 3 is obtained.
  • the heat treatment was continuously performed while supplying the inert gas.
  • the component composition of the obtained alloy steel powder for powder metallurgy was as shown in Tables 2 and 3.
  • surface and the following description means vol%.
  • Table 2 is an example at the time of using Ar containing gas as an inert gas.
  • powder symbols: A and I that are not mixed with carbon powder (powder symbols: A10, I10), the atomized iron-based powder is O-excess, so these can be obtained even after the heat treatment conditions are adjusted appropriately. The amount of O after heat-treating is out of the proper value. Therefore, for the atomized iron-based powder symbols: A and I, it is necessary to mix an appropriate amount of carbon powder that satisfies 4/3 ([C] + [MXC]) + 0.28 ⁇ [O].
  • the inert gas is 100% Ar and d / ⁇ v ⁇ 2.6 (powder symbols: A11 to A13, A16, B13 to B15, C11 to C14, D11 to D14, E11 to E13, F11, G11, For H11, I11, J11), the C content is 0.1% by mass or less and the O content is 0.23% by mass or less. Since the O content is further reduced, d / ⁇ v ⁇ 2.6. It is preferable that
  • the introduced gas was changed from 100% Ar to 50% Ar-50% N 2 , and in each case, the O amount was 0.28% by mass or less.
  • powder symbols: C11 to C14 good values were obtained with a dew point of 5 ° C. or less (powder symbols: C12 to C14) and an O amount of 0.20 mass% or less. Further, when the dew point is ⁇ 10 ° C. or lower (powder symbol: C14), the amount of O is 0.15% by mass or lower, which is a much better value. Further, for powder symbols D11 to D13 and E11 to E13, the soaking temperature is 1080 ° C. or higher and t ⁇ 10 4 ⁇ 0.0037 ⁇ T is satisfied (powder symbols: D13 to D14, E13) and the amount of O is An even better value of 0.20% by mass or less is obtained.
  • the amount of C and O in the atomized iron-based powder is [O] ⁇ 4/3 [C] ⁇ 2 / Since both 15 and 4/3 [C] + 0.28 ⁇ [O] are satisfied, the heat treatment can be performed by treating in an inert gas atmosphere using appropriate heat treatment conditions without mixing the carbon powder before the heat treatment. It shows that appropriate values are obtained for the subsequent C and O amounts.
  • the amount of C and O in the atomized iron-based powder does not satisfy [O] ⁇ 4/3 [C] ⁇ 2/15 and is excessive C. This shows that the amount of C after the heat treatment is out of the proper range even if the treatment is performed under the conditions.
  • the C amount or O amount of the atomized iron-based powder is too high, and therefore the C amount or O amount cannot be reduced to the specified amount even by heat treatment.
  • ⁇ N 2 containing case Table 3 using the gas is an example of a case of performing heat treatment in an N 2 containing atmosphere.
  • Atomized iron-based powder symbol: A, B, F and I are O-excessive, so an appropriate amount of carbon powder satisfying 4/3 ([C] + [MXC]) + 0.28 ⁇ [O] Mixing is necessary.
  • examples of mixing graphite powder as shown in Table 3 and treating under various heat treatment conditions are powder symbols: A21 to A28, B21 to B25, C21 to C24, D21 to D24, E21 to E23, F21. , G21, H21, I21, J21.
  • the relationship between the packed bed thickness d (mm) of the iron powder and the flow velocity v (mm / s) of the inert gas satisfies d / ⁇ v ⁇ 3.0 (powder symbol: A21 -A24, A26-A28, B22-B25, C21-C24, D21-D24, E21-E23, F21, G21, H21, I21, J21), the amount of O is 0.28% by mass or less. In addition, for those not satisfying d / ⁇ v ⁇ 3.0 (powder symbols: A25, B21), the amount of O exceeds 0.28% by mass.
  • the introduced gas is 100% N 2 and d / ⁇ v ⁇ 2.6 (powder symbols: A21 to A23, A26, B23 to B25, C21 to C24, D21 to D24, E21 to E23, F21, G21, For H21, I21, J21), the C amount is 0.1% by mass or less, the O amount is 0.23% by mass or less, and the O amount is further reduced. It can be seen that the relationship with the flow velocity v (mm / s) of the inert gas is preferably d / ⁇ v ⁇ 2.6.
  • the introduced gas was changed from 100% N 2 to 90% N 2 -10% He, and in each case, the O amount was 0.28% by mass or less. .
  • powder symbols: C21 to C24 those having a dew point of 5 ° C. or less (powder symbols: C22 to C24) and an O amount of 0.20% by mass or less are good values. Further, when the dew point is ⁇ 10 ° C. or less (powder symbol: C24), the amount of O is 0.15% by mass or less, which is a much better value. Furthermore, powder symbols: D21 to D24 and E21 to E23 satisfy the condition of t ⁇ 10 4 ⁇ 0.0037 ⁇ T when the soaking temperature is 1080 ° C. or more (powder symbols: D23 to D24, E23). An even better value of 0.20% by mass or less is obtained.
  • the amount of C and O in the atomized iron-based powder is [O] ⁇ 4/3 [C] -2 / Since both 15 and 4/3 [C] + 0.28 ⁇ [O] are satisfied, it is possible to reduce the C amount and O after the heat treatment by reducing the carbon powder before the heat treatment under appropriate heat treatment conditions. It shows that an appropriate value is obtained for the amount.
  • Example 2 Of the atomized iron-based powders in Table 1, A and J were reduced by heat treatment using N 2 as an inert gas. Table 4 shows the processing conditions. At that time, the atomized iron-based powder A was mixed with the amount of graphite powder shown in Table 4 and then supplied to the moving bed furnace. On the other hand, the atomized iron-based powder J was supplied as it was (only the atomized iron-based powder J) to the moving bed furnace without being mixed with the graphite powder.
  • the inert gas in the moving bed furnace was exhausted and H 2 gas was supplied, and the reduced powder was cooled in the H 2 gas atmosphere (A31, J31). After cooling, the obtained powder was crushed to obtain alloy steel powder for powder metallurgy.
  • the component composition of the obtained alloy steel powder is shown in Table 4.
  • the heat treatment conditions of A23 and J21 in Example 1 and the component composition of the alloy steel powder are also shown in Table 4. In A23 and J21, the cooling after the reduction is performed in an N 2 atmosphere.
  • N as an impurity contained in the alloy steel powder can be further reduced by cooling the reduced atomized iron-based powder using hydrogen gas or a hydrogen-containing gas.

Abstract

La présente invention concerne un procédé de production d'une poudre d'acier allié destinée à la métallurgie des poudres. Le procédé utilise un four à lit mobile et, sans recourir à une analyse de gaz, qui rend nécessaire une maintenance fastidieuse, permet de traiter thermiquement une poudre à base de fer qui contient des éléments pouvant facilement s'oxyder, tels Cr, Mn et V, et de réduire de façon stable la teneur en C et la teneur en O. Un procédé de production d'une poudre d'acier allié destinée à la métallurgie des poudres d'après la présente invention comprend les étapes consistant à : préparer une poudre atomisée à base de fer ayant une composition spécifique ; après l'avoir mélangée, si nécessaire, à un composant carboné, introduire la poudre atomisée à base de fer dans un four à lit mobile de manière à former une couche de remplissage ayant une épaisseur de d (mm) ; introduire un gaz inerte dans le four à lit mobile d'une manière telle que le gaz inerte présente une vitesse moyenne de flux de gaz telle que v (mm/s) ; réduire la poudre atomisée à base de fer en la traitant thermiquement dans le four à lit mobile ; et produire une poudre d'acier allié destinée à la métallurgie des poudres, d et v satisfaisant l'expression d/√v ≤ 3,0 (mm1/2∙s1/2).
PCT/JP2016/004441 2015-09-30 2016-09-30 Procédé de production d'une poudre d'acier allié destinée à la métallurgie des poudres WO2017056512A1 (fr)

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