US20160228948A1 - Metal powder for powder metallurgy, compound, granulated powder, and sintered body - Google Patents

Metal powder for powder metallurgy, compound, granulated powder, and sintered body Download PDF

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US20160228948A1
US20160228948A1 US15/002,818 US201615002818A US2016228948A1 US 20160228948 A1 US20160228948 A1 US 20160228948A1 US 201615002818 A US201615002818 A US 201615002818A US 2016228948 A1 US2016228948 A1 US 2016228948A1
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sintered body
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powder
metal powder
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Hidefumi Nakamura
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Seiko Epson Corp
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    • B—PERFORMING OPERATIONS; TRANSPORTING
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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
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • B22F3/15—Hot isostatic pressing
    • B22F1/0003—
    • 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
    • B22F1/0059—
    • 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
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
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    • 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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    • 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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    • C22C38/34—Ferrous alloys, e.g. steel alloys containing chromium with more than 1.5% by weight of silicon
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    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/36—Ferrous alloys, e.g. steel alloys containing chromium with more than 1.7% by weight of carbon
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    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/48—Ferrous alloys, e.g. steel alloys containing chromium with nickel with niobium or tantalum
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/50—Ferrous alloys, e.g. steel alloys containing chromium with nickel with titanium or zirconium
    • C—CHEMISTRY; METALLURGY
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/56—Ferrous alloys, e.g. steel alloys containing chromium with nickel with more than 1.7% by weight of carbon
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    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/60—Ferrous alloys, e.g. steel alloys containing lead, selenium, tellurium, or antimony, or more than 0.04% by weight of sulfur
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
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    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/35—Iron
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
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    • B22F2302/00—Metal Compound, non-Metallic compound or non-metal composition of the powder or its coating
    • B22F2302/45—Others, including non-metals
    • 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

Definitions

  • the present invention relates to a metal powder for powder metallurgy, a compound, a granulated powder, and a sintered body.
  • a composition containing a metal powder and a binder is molded into a desired shape to obtain a molded body, and the obtained molded body is degreased and sintered, whereby a sintered body is produced.
  • an atomic diffusion phenomenon occurs among particles of the metal powder, whereby the molded body is gradually densified, resulting in sintering.
  • JP-A-2012-87416 proposes a metal powder for powder metallurgy which contains Zr and Si, with the remainder including at least one element selected from the group consisting of Fe, Co, and Ni, and inevitable elements.
  • the sinterability is enhanced by the action of Zr, and a sintered body having a high density can be easily produced.
  • the thus obtained sintered body has recently become widely used for a variety of machine parts, structural parts, and the like.
  • a sintered body is further subjected to an additional treatment such as a hot isostatic pressing treatment (HIP treatment) to increase the density, however, the workload is significantly increased, and also an increase in the cost is inevitable.
  • HIP treatment hot isostatic pressing treatment
  • An advantage of some aspects of the invention is to provide a metal powder for powder metallurgy, a compound, and a granulated powder, each of which is capable of producing a sintered body having a high density, and a sintered body having a high density.
  • a metal powder for powder metallurgy includes particles, which contain Fe as a principal component, Cr in a proportion of 0.2% by mass or more and 35% by mass or less, Si in a proportion of 0.2% by mass or more and 3% by mass or less, and C in a proportion of 0.005% by mass or more and 2% by mass or less, and in which when one element selected from the group consisting of Ti, V, Y, Zr, Nb, Hf, and Ta is defined as a first element, and one element selected from the group consisting of Ti, V, Y, Zr, Nb, Hf, and Ta, and having a higher group number in the periodic table than that of the first element or having the same group number in the periodic table as that of the first element and a higher period number in the periodic table than that of the first element is defined as a second element, the first element is contained in a proportion of 0.01% by mass or more and 0.5% by mass or less and the second element is contained in a proportion of 0.01% by
  • the particles of the metal powder for powder metallurgy each have a passivation film derived from a Cr oxide whose thickness is small to some extent, and therefore, the decrease in the sinterability of the particles due to the passivation film can be suppressed.
  • the densification during sintering of the particles is achieved, and thus, a sintered body having a high density can be produced without performing an additional treatment.
  • the content of Si on the surface of each particle is 155% or more and 800% or less the content of Si at a depth of 60 nm from the surface of the particle.
  • Si is segregated on the surface of each particle, and this Si functions as a deoxidizing element which suppresses the oxidation of Fe or Cr, and therefore, when the particles are sintered, the generation of a large amount of iron oxide or chromium oxide can be suppressed. As a result, the particles have more excellent sinterability and a sintered body having a higher density can be produced.
  • the ratio of the content of 0 to the content of Si on the surface of each particle is 0.05 or more and 0.4 or less.
  • the ratio of Si present in the form of silicon oxide can be sufficiently decreased.
  • the deoxidizing effect of Si can be more reliably exhibited while suppressing the decrease in sinterability due to the presence of a large amount of silicon oxide.
  • the content of Cr on the surface of each particle is lower than the content of Cr in the whole particle.
  • the excessive increase in the thickness of the passivation film formed on the surface of each particle can be suppressed, and therefore, the sinterability of the particle can be particularly enhanced.
  • the ratio (X1/X2) of a value (X1) obtained by dividing the content (E1) of the first element by the mass number of the first element to a value (X2) obtained by dividing the content (E2) of the second element by the mass number of the second element is 0.3 or more and 3 or less.
  • the balance between the deposition amount of a carbide or the like of the first element and the deposition amount of a carbide or the like of the second element can be optimized.
  • pores remaining in a molded body can be eliminated as if they were swept out sequentially from the inside, and therefore, pores generated in the sintered body can be minimized.
  • a metal powder for powder metallurgy capable of producing a sintered body having a high density and excellent sintered body properties is obtained.
  • the sum of the content of the first element and the content of the second element is 0.05% by mass or more and 0.8% by mass or less.
  • the metal powder for powder metallurgy it is preferred that the metal powder has an average particle diameter of 0.5 ⁇ m or more and 30 ⁇ m or less.
  • pores remaining in a sintered body are extremely decreased, and therefore, a sintered body having a particularly high density and particularly excellent mechanical properties can be produced.
  • a compound according to an aspect of the invention includes the metal powder for powder metallurgy according to the aspect of the invention and a binder which binds the particles of the metal powder for powder metallurgy to one another.
  • a granulated powder according to an aspect of the invention is obtained by granulating the metal powder for powder metallurgy according to the aspect of the invention.
  • a sintered body according to an aspect of the invention is produced by sintering the metal powder for powder metallurgy according to the aspect of the invention.
  • FIG. 1 is a view schematically showing the cross sections of particles contained in an embodiment of a metal powder for powder metallurgy according to the invention.
  • FIG. 2 is an enlarged view of an area A of the cross section of the particle shown in FIG. 1 and is a view for illustrating a manner of performing an analysis in the depth direction by Auger electron spectroscopy in combination with sputtering of the surface of the particle.
  • FIG. 3 shows the Auger electron spectra obtained from a particle of a metal powder for powder metallurgy of sample No. 1.
  • FIG. 4 shows the Auger electron spectra obtained from a particle of a metal powder for powder metallurgy of sample No. 23.
  • a sintered body having a desired shape can be obtained by molding a composition containing a metal powder for powder metallurgy and a binder into a desired shape, followed by degreasing and firing. According to such a powder metallurgy technique, an advantage that a sintered body with a complicated and fine shape can be produced in a near-net shape (a shape close to a final shape) as compared with the other metallurgy techniques is obtained.
  • the present inventors have made intensive studies to find conditions for obtaining a sintered body having a high density without performing an additional treatment. As a result, they found that the density of a sintered body can be increased by optimizing the structure of each particle contained in a metal powder, and thus completed the invention.
  • the metal powder for powder metallurgy is a metal powder including particles, which contain Fe as a principal component, Cr in a proportion of 0.2% by mass or more and 35% by mass or less, Si in a proportion of 0.2% by mass or more and 3% by mass or less, C in a proportion of 0.005% by mass or more and 2% by mass or less, the below-mentioned first element in a proportion of 0.01% by mass or more and 0.5% by mass or less, and the below-mentioned second element in a proportion of 0.01% by mass or more and 0.5% by mass or less, wherein the content of Cr on the surface of each particle is 0.2% by atom or more and 15% by atom or less and is 70% or more and 170% or less the content of Cr at a depth of 60 nm from the surface of the particle.
  • the densification during sintering can be particularly enhanced.
  • a result a metal powder including particles, which contain Fe as a principal component, Cr in a proportion of 0.2% by mass or more and
  • Such a sintered body has excellent mechanical properties. Due to this, the sintered body can be widely applied also to, for example, machine parts, structural parts, and the like, to which an external force is applied.
  • metal powder for powder metallurgy is sometimes simply referred to as “metal powder”, and each of the multiple particles constituting the metal powder for powder metallurgy is sometimes simply referred to as “particle”.
  • FIG. 1 is a view schematically showing the cross sections of particles contained in the embodiment of a metal powder for powder metallurgy according to the invention
  • FIG. 2 is an enlarged view of an area A of the cross section of the particle shown in FIG. 1 and is a view for illustrating a manner of performing an analysis in the depth direction by Auger electron spectroscopy in combination with sputtering of the surface of the particle.
  • the particle 1 satisfying such conditions has a relatively fixed Cr content from the surface to the depth of 60 nm.
  • Such a particle 1 has a passivation film derived from a Cr oxide whose thickness is small to some extent, and therefore, the decrease in the sinterability of the particle 1 due to the passivation film can be suppressed.
  • the densification during sintering of the particles 1 is achieved, and therefore, a sintered body having a high density can be produced without performing an additional treatment.
  • the oxidation resistance on the surface of the particle 1 is deteriorated. If the oxidation resistance is deteriorated, the surface of the particle 1 is liable to be oxidized by the change in environment. At this time, the oxidation of the surface of the particle 1 is liable to occur unevenly among the particles 1, and therefore, the sinterability varies among the particles 1 resulting in deterioration of the densification of the sintered body.
  • the Cr(0) exceeds the above upper limit or the ratio of the Cr(0) to the Cr(60) exceeds the above upper limit, the thickness of the passivation film becomes too large. Therefore, the passivation film inhibits the sintering of the particles 1 resulting in deterioration of the densification of the sintered body.
  • the Cr(0) may be 70% or more and 170% or less the Cr(60), but is preferably set to 80% or more and 150% or less the Cr(60).
  • the content of Cr on the surface of the particle 1 (Cr(0)) preferably satisfies the following relationship: Cr(0) ⁇ Cr(w), more preferably satisfies the following relationship: Cr(0) ⁇ 0.8 ⁇ Cr(w).
  • the content of Cr on the surface of the particle 1 can be made lower than the content of Cr in the whole particle 1. According to this, as compared with the thickness of the passivation film converted from the chemical composition of the whole particle 1, the thickness of the passivation film formed on the surface of the particle 1 can be prevented from excessively increasing, and therefore, the sinterability of the particle 1 can be particularly enhanced.
  • the content of Cr in the whole particle 1 can be determined by an analytical method described below.
  • the Si(0) is preferably 155% or more and 800% or less, more preferably 200% or more and 500% or less the Si(60).
  • the content of Si on the surface is 1.55 times or more higher than the content of Si in the inside (at a depth of 60 nm). It can be said that in such a particle 1, Si is segregated on the surface. Si is considered to be present in the form of, for example, silicon oxide on the surface of the particle 1. Further, Si functions as a deoxidizing element which suppresses the oxidation of Fe or Cr, and therefore, the generation of iron oxide or chromium oxide on the surface of the particle 1 can be suppressed. Further, even in the case where oxygen is newly supplied when the particle 1 is sintered, the generation of a large amount of iron oxide or chromium oxide can be suppressed. As a result, the particle 1 has more excellent sinterability and a sintered body having a higher density can be produced.
  • Si present on the surface of the particle 1 functions to suppress the increase in the size of crystal grains when the metal powder is fired. Due to this, finer crystals are formed, and thus, a sintered body having excellent mechanical properties can be produced.
  • the Si(0) is preferably 15% by atom or more and 50% by atom or less, more preferably 25% by atom or more and 45% by atom or less.
  • the particle 1 satisfying such conditions can suppress the generation of a large amount of iron oxide or chromium oxide. Due to this, the particle 1 has more excellent sinterability and a sintered body having a higher density can be produced.
  • Si is segregated, however, if a large amount of Si in the form of silicon oxide is present, in the same manner as iron oxide or chromium oxide, firing of the metal powder may be inhibited.
  • the O(0) is preferably 0.05 times or more and 0.4 times or less, more preferably 0.1 times or more and 0.35 times or less the Si(0).
  • the ratio of O(0) to Si(0) falls within the above range, even if Si is segregated on the surface of the particle 1, the ratio of Si present in the form of silicon oxide is sufficiently decreased. Therefore, by making the ratio of O(0) to Si(0) fall within the above range, the deoxidizing effect of Si can be more reliably exhibited while suppressing the decrease in sinterability due to the presence of a large amount of silicon oxide. As a result, the particle 1 having particularly high sinterability is obtained, and by using the metal powder containing the particle 1, a sintered body having a high density can be produced.
  • Si(0), Si(60), and O(0) can be also obtained by an analysis in the depth direction by Auger electron spectroscopy in combination with sputtering in the same manner as the Cr(0) and Cr(60).
  • a sintered body having excellent mechanical properties is obtained.
  • Such a sintered body can be widely applied also to, for example, machine parts, structural parts, and the like, to which an external force is applied.
  • Fe is a component (principal component) whose content is the highest in the chemical composition of the particle 1 and has a great influence on the properties of the sintered body.
  • the content of Fe in the whole particle 1 is 50% by mass or more.
  • Cr chromium
  • the content of Cr in the particle 1 is set to 0.2% by mass or more and 35% by mass or less, but is set to preferably 2% by mass or more and 32% by mass or less, more preferably 6% by mass or more and 30% by mass or less.
  • the corrosion resistance of a sintered body to be produced may be insufficient depending on the overall composition.
  • the content of Cr exceeds the above upper limit, the sinterability is deteriorated depending on the overall composition so that it may become difficult to increase the density of the sintered body.
  • Ni nickel is an element which provides corrosion resistance and heat resistance to a sintered body to be produced as needed.
  • the content of Ni in the particle 1 is set to preferably 41% by mass or less, more preferably 10% by mass or more and 39% by mass or less, further more preferably 12% by mass or more and 27% by mass or less.
  • the corrosion resistance and the heat resistance of a sintered body to be produced may not be sufficiently enhanced depending on the overall composition.
  • the content of Ni exceeds the above upper limit, the corrosion resistance and the heat resistance may be deteriorated instead.
  • the content of Cr may be appropriately changed according to the content of Ni or Mo.
  • the content of Cr is more preferably 18% by mass or more and 20% by mass or less.
  • the content of Cr is more preferably 16% by mass or more and less than 18% by mass.
  • the content of Ni is 0.05% by mass or more and 0.6% by mass or less
  • the content of Cr is more preferably 10% by mass or more and 18% by mass or less.
  • the content of C is less than the above lower limit, it is difficult to generate sufficient amounts of a carbide or the like of the first element and a carbide or the like of the second element depending on the overall composition, and therefore, the densification of the sintered body may be insufficient.
  • the content of C exceeds the above upper limit, the amount of C with respect to the amounts of the first element and the second element is too large depending on the overall composition, and therefore, the sinterability of the particle 1 may be deteriorated instead.
  • the content of Ni is 0.05% by mass or more and 0.6% by mass or less
  • the content of C is more preferably 0.15% by mass or more and 1.2% by mass or less.
  • the content of Ni is preferably set to 0.05% by mass or more and 22% by mass or less.
  • the corrosion resistance and the heat resistance of a sintered body to be produced may not be sufficiently enhanced depending on the overall composition.
  • the content of Ni exceeds the above upper limit, the corrosion resistance and the heat resistance may be deteriorated instead.
  • the first element and the second element each deposit a carbide or an oxide (hereinafter also collectively referred to as “carbide or the like”). It is considered that this deposited carbide or the like inhibits the significant growth of crystal grains when the metal powder is sintered. As a result, as described above, it becomes difficult to generate pores in a sintered body, and also the increase in the size of crystal grains is prevented, and thus, a sintered body having a high density and excellent mechanical properties is obtained.
  • the deposited carbide or the like promotes the accumulation of silicon oxide at a crystal grain boundary, and as a result, the sintering is promoted and the density is increased while preventing the increase in the size of crystal grains.
  • the first element and the second element are two elements selected from the group consisting of the following seven elements: Ti, V, Y, Zr, Nb, Hf, and Ta, but preferably include an element belonging to group IIIA or group IVA in the long periodic table (Ti, Y, Zr, or Hf).
  • group IIIA or group IVA in the long periodic table (Ti, Y, Zr, or Hf).
  • the first element is only required to be one element selected from the group consisting of the following seven elements: Ti, V, Y, Zr, Nb, Hf, and Ta as described above, but is preferably an element belonging to group IIIA or group IVA in the long periodic table in the group consisting of the above-mentioned seven elements.
  • An element belonging to group IIIA or group IVA removes oxygen contained as an oxide in the metal powder (functions as a deoxidizing element) and therefore can particularly enhance the sinterability of the metal powder. According to this, the concentration of oxygen remaining in the crystal grains after sintering can be decreased. As a result, the content of oxygen in the sintered body can be decreased, and the density can be increased.
  • Zr is a ferrite forming element, and therefore deposits a body-centered cubic lattice phase.
  • This body-centered cubic lattice phase has more excellent sinterability than the other crystal lattice phases, and therefore contributes to the densification of a sintered body.
  • the atomic radius of Zr is slightly larger than that of Fe. Specifically, the atomic radius of Fe is about 0.117 nm, and the atomic radius of Zr is about 0.145 nm. Therefore, Zr is solid-dissolved in Fe, but is not completely solid-dissolved therein, and part of Zr is deposited as a carbide or the like. According to this, an appropriate amount of a carbide or the like is deposited, and therefore, the increase in the size of crystal grains can be effectively prevented while promoting the sintering and increasing the density.
  • the atomic radius of Nb is slightly larger than that of Fe, but slightly smaller than that of Zr. Specifically, the atomic radius of Fe is about 0.117 nm, and the atomic radius of Nb is about 0.134 nm. Therefore, Nb is solid-dissolved in Fe, but is not completely solid-dissolved therein, and part of Nb is deposited as a carbide or the like. According to this, an appropriate amount of a carbide or the like is deposited, and therefore, the increase in the size of crystal grains can be effectively prevented while promoting the sintering and increasing the density.
  • the content of the second element in the metal powder is set to 0.01% by mass or more and 0.5% by mass or less, but is set to preferably 0.03% by mass or more and 0.4% by mass or less, more preferably 0.05% by mass or more and 0.3% by mass or less. If the content of the second element is less than the above lower limit, the effect of the addition of the second element is weakened depending on the overall composition so that the density of a sintered body to be produced is not sufficiently increased. On the other hand, if the content of the second element exceeds the above upper limit, the amount of the second element is too large depending on the overall composition so that the ratio of the above-mentioned carbide or the like is too high, and therefore, the densification is deteriorated instead.
  • each of the first element and the second element deposits a carbide or the like, however, in the case where an element belonging to group III A or group IVA is selected as the first element as described above and an element belonging to group VA is selected as the second element as described above, it is presumed that when the metal powder is sintered, the timing when a carbide or the like of the first element is deposited and the timing when a carbide or the like of the second element is deposited differ moderately from each other. It is considered that due to the difference in timing when a carbide or the like is deposited in this manner, sintering gradually proceeds so that the generation of pores is prevented, and thus, a dense sintered body is obtained. That is, it is considered that by the presence of both of the carbide or the like of the first element and the carbide or the like of the second element, the increase in the size of crystal grains can be suppressed while increasing the density of the sintered body.
  • the carbide or the like of the first element and the carbide or the like of the second element are deposited apart from each other, an effect of preventing the increase in the size of crystal grains is uniformly exhibited in the particle 1. In view of this, the densification of the sintered body is particularly promoted.
  • a sintered body can be densified, and therefore, a sintered body having a high density can be produced without performing an additional treatment. It is considered that when the particles 1 are subjected to powder metallurgy, the carbide or the like moves to a metal crystal grain boundary in a sintered body. Then, the carbide or the like having moved to the triple point of a crystal grain boundary suppresses the crystal growth at this point (a flux pinning effect). As a result, the significant growth of crystal grains is suppressed, and thus, a sintered body having finer crystals is obtained. Such a sintered body has particularly high mechanical properties.
  • the ratio of the content of the first element to the content of the second element in consideration of the mass number of the first element and the mass number of the second element.
  • X1/X2 is preferably 0.3 or more and 3 or less, more preferably 0.5 or more and 2 or less, further more preferably 0.75 or more and 1.3 or less.
  • pores remaining in a molded body can be eliminated as if they were swept out sequentially from the inside, and therefore, pores generated in a sintered body can be minimized. Accordingly, a metal powder capable of producing a sintered body having a high density and excellent mechanical properties can be obtained by setting the ratio X1/X2 within the above range.
  • the ratio (E1/E2) of the content E1 of the first element to the content E2 of the second element is calculated.
  • E1/E2 is preferably 0.29 or more and 2.95 or less, more preferably 0.49 or more and 1.96 or less.
  • E1/E2 is preferably 0.58 or more and 5.76 or less, more preferably 0.96 or more and 3.84 or less.
  • E1/E2 is preferably 0.15 or more and 1.55 or less, more preferably 0.26 or more and 1.03 or less.
  • E1/E2 is preferably 0.15 or more and 1.54 or less, more preferably 0.26 or more and 1.03 or less.
  • E1/E2 is preferably 0.29 or more and 2.87 or less, more preferably 0.48 or more and 1.91 or less.
  • E1/E2 is preferably 0.16 or more and 1.64 or less, more preferably 0.27 or more and 1.10 or less.
  • E1/E2 is preferably 0.16 or more and 1.58 or less, more preferably 0.26 or more and 1.05 or less.
  • E1/E2 is preferably 0.15 or more and 1.51 or less, more preferably 0.25 or more and 1.01 or less.
  • E1/E2 is preferably 0.54 or more and 5.38 or less, more preferably 0.90 or more and 3.58 or less.
  • E1/E2 can be calculated in the same manner as described above.
  • the sum of the content E1 of the first element and the content E2 of the second element is preferably 0.05% by mass or more and 0.8% by mass or less, more preferably 0.10% by mass or more and 0.6% by mass or less, further more preferably 0.12% by mass or more and 0.24% by mass or less.
  • (E1+E2)/Si is preferably 0.1 or more and 0.7 or less, more preferably 0.15 or more and 0.6 or less, further more preferably 0.2 or more and 0.5 or less in terms of mass ratio.
  • the particle 1 in the particle 1, necessary and sufficient accumulation of silicon oxide occurs by using the carbide or the like of the first element and the carbide or the like of the second element as nuclei, and in the case where an element such as Ni is contained in the particle 1 other than Fe and Cr, an oxidation reaction of such an element is easily suppressed. Therefore, also from this viewpoint, the sinterability of the particle 1 is enhanced, and thus, a sintered body having a higher density, excellent mechanical properties, and excellent corrosion resistance can be obtained.
  • (E1+E2)/C is preferably 1 or more and 16 or less, more preferably 2 or more and 13 or less, further more preferably 3 or more and 10 or less.
  • the metal powder is only required to contain two elements selected from the group consisting of the above-mentioned seven elements, but may further contain an element which is selected from this group and is different from these two elements. That is, the metal powder may contain three or more elements selected from the group consisting of the above-mentioned seven elements. According to this, the above-mentioned effect can be further enhanced, which slightly varies depending on the combination of the elements to be contained.
  • the particle 1 may contain, other than the above-mentioned elements, at least one element of W, Co, Mn, Mo, Cu, N, and S as needed. These elements may be inevitably contained in some cases.
  • W is an element which enhances the heat resistance of a sintered body to be produced.
  • the content of W in the particle 1 is set to 0.5% by mass or more and 20% by mass or less, but is set to preferably 1% by mass or more and 10% by mass or less, more preferably 5% by mass or more and 7% by mass or less. If the content of W is less than the above lower limit, the heat resistance and the sintered body cannot be sufficiently enhanced depending on the overall composition, and for example, when a tool is produced by using the obtained sintered body, the hardness, softening resistance, and abrasion resistance of the tool at a high temperature may be deteriorated. On the other hand, if the content of W exceeds the above upper limit, the mechanical properties such as toughness of the sintered body may be deteriorated depending on the overall composition, and for example, a problem such as a chipping may occur in the tool.
  • Co is an element which enhances the heat resistance of a sintered body to be produced.
  • the content of Co in the particle 1 is not particularly limited, but is preferably 3% by mass or more and 12% by mass or less, more preferably 4.5% by mass or more and 10.5% by mass or less.
  • the heat resistance of a sintered body to be produced can be further enhanced without causing a large decrease in the density of the sintered body.
  • the decrease in the hardness or the softness resistance at a high temperature can be suppressed, and therefore, for example, when a tool is produced by using the obtained sintered body, a high-speed tool which can be cut at a higher speed can be easily produced.
  • Mn is an element which provides corrosion resistance and high mechanical properties to a sintered body to be produced.
  • the content of Mn in the particle 1 is not particularly limited, but is preferably 0.01% by mass or more and 3% by mass or less, more preferably 0.05% by mass or more and 1% by mass or less. By setting the content of Mn within the above range, a sintered body having a higher density and excellent mechanical properties is obtained.
  • the corrosion resistance and the mechanical properties of a sintered body to be produced may not be sufficiently enhanced depending on the overall composition.
  • the content of Mn exceeds the above upper limit, the corrosion resistance and the mechanical properties may be deteriorated instead depending on the overall composition.
  • Mo is an element which enhances the corrosion resistance of a sintered body to be produced.
  • the content of Mo in the particle 1 is not particularly limited, but is preferably 1% by mass or more and 5% by mass or less, more preferably 1.2% by mass or more and 4% by mass or less, further more preferably 2% by mass or more and 3% by mass or less.
  • Cu is an element which enhances the corrosion resistance of a sintered body to be produced.
  • the content of Cu in the particle 1 is not particularly limited, but is preferably 5% by mass or less, more preferably 1% by mass or more and 4% by mass or less. By setting the content of Cu within the above range, the corrosion resistance of a sintered body to be produced can be further enhanced without causing a large decrease in the density of the sintered body.
  • the content of Ni is 0.05% by mass or more and 0.6% by mass or less
  • the content of Cu is preferably less than 1% by mass or less, more preferably less than 0.1% by mass or less. Further, in this case, it is more preferred that the particle 1 substantially contains no Cu (the content of Cu is set to less than 0.01% by mass) excluding the amount of Cu which is inevitably contained.
  • the detailed reasons therefor have not been known, however, this is due to the fear that by the incorporation of Cu, the effect brought about by the first element and the second element as described above may be weakened.
  • N is an element which enhances the mechanical properties such as proof stress of a sintered body to be produced.
  • the content of N in the particle 1 is not particularly limited, but is preferably 0.03% by mass or more and 1% by mass or less, more preferably 0.08% by mass or more and 0.3% by mass or less, further more preferably 0.1% by mass or more and 0.25% by mass or less.
  • a method using a nitrided starting material for example, a method of introducing nitrogen gas into a molten metal, a method of performing a nitriding treatment of a produced metal powder, or the like is used.
  • S is an element which enhances the machinability of a sintered body to be produced.
  • the content of S in the particle 1 is not particularly limited, but is preferably 0.5% by mass or less, more preferably 0.01% by mass or more and 0.3% by mass or less.
  • the machinability of a sintered body to be produced can be further enhanced without causing a large decrease in the density of the sintered body. Accordingly, the obtained sintered body can be cut out into a desired shape by performing a machining process.
  • B, Se, Te, Pd, Al, or the like may be added other than the above-mentioned elements.
  • the contents of these elements are not particularly limited, but the content of each element is preferably less than 0.1% by mass, and also the total content of these elements is preferably less than 0.2% by mass. These elements may be inevitably contained in some cases.
  • the particle 1 may contain impurities.
  • the impurities include all elements other than the above-mentioned elements, and examples thereof include Li, Be, Na, Mg, P, K, Ca, Sc, Zn, Ga, Ge, Ag, In, Sn, Sb, Os, Ir, Pt, Au, and Bi.
  • the incorporation amounts of these impurity elements are preferably such that the content of each of the impurity elements is less than the content of each of the above-mentioned constituent elements of the particle 1. Further, the incorporation amount of these impurity elements is preferably set such that the content of each of the impurity elements is less than 0.03% by mass, more preferably less than 0.02% by mass.
  • the total content of these impurity elements is set to preferably less than 0.3% by mass, more preferably less than 0.2% by mass. These elements do not inhibit the effect as described above as long as the contents thereof are within the above range, and therefore may be intentionally added to the particle 1.
  • O oxygen
  • the amount thereof is preferably about 0.8% by mass or less, more preferably about 0.5% by mass or less.
  • the lower limit thereof is not particularly set, but is preferably 0.03% by mass or more from the viewpoint of ease of mass production or the like.
  • the chemical composition of the particle 1 can be determined by, for example, Iron and steel—Atomic absorption spectrometric method specified in JIS G 1257 (2000), Iron and steel—ICP atomic emission spectrometric method specified in JIS G 1258 (2007), Iron and steel—Method for spark discharge atomic emission spectrometric analysis specified in JIS G 1253 (2002), Iron and steel—Method for X-ray fluorescence spectrometric analysis specified in JIS G 1256 (1997), gravimetric, titrimetric, and absorption spectrometric methods specified in JIS G 1211 to G 1237, or the like.
  • an optical emission spectrometer for solids (spark optical emission spectrometer, model: SPECTROLAB, type: LAVMB08A) manufactured by SPECTRO Analytical Instruments GmbH or an ICP device (model: CIROS-120) manufactured by Rigaku Corporation can be used.
  • JIS G 1211 to G 1237 are as follows.
  • JIS G 1214 Iron and steel—Methods for determination of phosphorus content
  • JIS G 1221 Iron and steel—Methods for determination of vanadium content
  • JIS G 1223 (1997): Iron and steel—Methods for determination of titanium content
  • C (carbon) and S (sulfur) are determined, particularly, an infrared absorption method after combustion in a current of oxygen (after combustion in a high-frequency induction heating furnace) specified in JIS G 1211 (2011) is also used.
  • a carbon-sulfur analyzer, CS-200 manufactured by LECO Corporation can be used.
  • N (nitrogen) and O (oxygen) are determined, particularly, a method for determination of nitrogen content in iron and steel specified in JIS G 1228 (2006) and a method for determination of oxygen content in metallic materials specified in JIS Z 2613 (2006) are also used.
  • an oxygen-nitrogen analyzer TC-300/EF-300 manufactured by LECO Corporation can be used.
  • the above-mentioned ratio can be obtained by arbitrarily extracting 20 or more particles in the metal powder for powder metallurgy and counting the particles 1 as described above.
  • the average particle diameter of the metal powder for powder metallurgy of the invention is preferably 0.5 ⁇ m or more and 30 ⁇ m or less, more preferably 1 ⁇ m or more and 20 ⁇ n or less, further more preferably 2 ⁇ n or more and 10 ⁇ n or less.
  • the average particle diameter can be obtained as a particle diameter when the cumulative amount obtained by cumulating the percentages of the particles from the smaller diameter side reaches 50% in a cumulative particle size distribution on amass basis obtained by laser diffractometry.
  • the average particle diameter of the metal powder for powder metallurgy is less than the above lower limit, the moldability is deteriorated in the case where the shape is difficult to mold, and therefore, the sintered density may be decreased.
  • the average particle diameter of the metal powder exceeds the above upper limit, spaces between the particles become larger during molding, and therefore, the sintered density may be decreased also in this case.
  • the average of the aspect ratio defined by S/L is preferably about 0.4 or more and 1 or less, more preferably about 0.7 or more and 1 or less.
  • the metal powder for powder metallurgy having an aspect ratio within this range has a shape relatively close to a spherical shape, and therefore, the packing factor when the metal powder is molded is increased. As a result, the density of the sintered body can be further increased.
  • the “major axis” is the maximum length in the projected image of the particle
  • the “minor axis” is the maximum length in the direction perpendicular to the major axis.
  • the average of the aspect ratio can be obtained as the average of the measured aspect ratios of 100 or more particles.
  • the tap density of the metal powder for powder metallurgy of the invention is preferably 3.5 g/cm 3 or more, more preferably 4 g/cm 3 or more. According to the metal powder for powder metallurgy having such a high tap density, when a molded body is obtained, the interparticle packing efficiency is particularly increased. Therefore, a particularly dense sintered body can be obtained in the end.
  • the method for producing a sintered body includes (A) a composition preparation step in which a composition for producing a sintered body is prepared, (B) a molding step in which a molded body is produced, (C) a degreasing step in which a degreasing treatment is performed, and (D) a firing step in which firing is performed.
  • A a composition preparation step in which a composition for producing a sintered body is prepared
  • B a molding step in which a molded body is produced
  • C a degreasing step in which a degreasing treatment is performed
  • D a firing step in which firing is performed.
  • the metal powder for powder metallurgy according to the invention and a binder are prepared, and these materials are kneaded using a kneader, whereby a kneaded material (composition) is obtained.
  • the metal powder for powder metallurgy is uniformly dispersed.
  • the metal powder for powder metallurgy according to the invention is produced by, for example, any of a variety of powdering methods such as an atomization method (such as a water atomization method, a gas atomization method, or a spinning water atomization method), a reducing method, a carbonyl method, and a pulverization method.
  • an atomization method such as a water atomization method, a gas atomization method, or a spinning water atomization method
  • a reducing method such as a carbonyl method, and a pulverization method.
  • the metal powder for powder metallurgy according to the invention is preferably a metal powder produced by an atomization method, more preferably a metal powder produced by a water atomization method or a spinning water atomization method.
  • the atomization method is a method in which a molten metal (metal melt) is caused to collide with a fluid (liquid or gas) sprayed at a high speed to atomize the metal melt into a fine powder and also to cool the fine powder, whereby a metal powder is produced.
  • a molten metal metal melt
  • a fluid liquid or gas
  • the metal powder when the metal powder is molded, a molded body having a high packing factor is obtained. That is, a powder capable of producing a sintered body having a high density can be obtained.
  • the cooling rate of the metal melt is very high, and therefore, the particle 1 in which the second region P2 and the third region P3 are more uniformly distributed can be obtained.
  • the pressure of water (hereinafter referred to as “atomization water”) to be sprayed to the molten metal is not particularly limited, but is set to preferably about 75 MPa or more and 120 MPa or less (750 kgf/cm 2 or more and 1200 kgf/cm 2 or less), more preferably about 90 MPa or more and 120 MPa or less (900 kgf/cm 2 or more and 1200 kgf/cm 2 or less).
  • the temperature of the atomization water is also not particularly limited, but is preferably set to about 1° C. or higher and 20° C. or lower.
  • the atomization water is often sprayed in a cone shape such that it has a vertex on the falling path of the metal melt and the outer diameter gradually decreases downward.
  • the vertex angle ⁇ of the cone formed by the atomization water is preferably about 10° or more and 40° or less, more preferably about 15° or more and 35° or less. According to this, a metal powder for powder metallurgy having a composition as described above can be reliably produced.
  • the metal melt can be cooled particularly quickly. Due to this, a powder having high quality can be obtained in a wide alloy composition range.
  • the cooling rate when cooling the metal melt in the atomization method is preferably 1 ⁇ 10 4 ° C./s or more, more preferably 1 ⁇ 10 5 ° C./s or more.
  • the volume of an amorphous material or a metal glass tends to slightly increase
  • the cooling rate is decreased (for example, in the case of 1 ⁇ 10 4 ° C./s or more and less than 1 ⁇ 10 5 ° C./s)
  • the volume of a crystalline material tends to slightly increase.
  • the thus obtained metal powder for powder metallurgy may be classified as needed.
  • classification method include dry classification such as sieving classification, inertial classification, and centrifugal classification, and wet classification such as sedimentation classification.
  • binder examples include polyolefins such as polyethylene, polypropylene, and ethylene-vinyl acetate copolymers, acrylic resins such as polymethyl methacrylate and polybutyl methacrylate, styrenic resins such as polystyrene, polyesters such as polyvinyl chloride, polyvinylidene chloride, polyamide, polyethylene terephthalate, and polybutylene terephthalate, various resins such as polyether, polyvinyl alcohol, polyvinylpyrrolidone, and copolymers thereof, and various organic binders such as various waxes, paraffins, higher fatty acids (such as stearic acid), higher alcohols, higher fatty acid esters, and higher fatty acid amides. These can be used alone or by mixing two or more types thereof.
  • polyolefins such as polyethylene, polypropylene, and ethylene-vinyl acetate copolymers
  • acrylic resins such as polymethyl methacryl
  • the content of the binder is preferably about 2% by mass or more and 20% by mass or less, more preferably about 5% by mass or more and 10% by mass or less with respect to the total amount of the kneaded material.
  • a plasticizer may be added as needed.
  • the plasticizer include phthalate esters (such as DOP, DEP, and DBP), adipate esters, trimellitate esters, and sebacate esters. These can be used alone or by mixing two or more types thereof.
  • any of a variety of additives such as a lubricant, an antioxidant, a degreasing accelerator, and a surfactant can be added as needed.
  • the kneading conditions vary depending on the respective conditions such as the metal composition or the particle diameter of the metal powder for powder metallurgy to be used, the composition of the binder, and the blending amount thereof.
  • the kneading temperature can be set to about 50° C. or higher and 200° C. or lower, and the kneading time can be set to about 15 minutes or more and 210 minutes or less.
  • the kneaded material is formed into a pellet (small particle) as needed.
  • the particle diameter of the pellet is set to, for example, about 1 mm or more and 15 mm or less.
  • a granulated powder may be produced.
  • the kneaded material, the granulated powder, and the like are examples of the composition to be subjected to the molding step described below.
  • the embodiment of the granulated powder according to the invention is directed to a granulated powder obtained by binding a plurality of metal particles to one another with a binder by subjecting the metal powder for powder metallurgy according to the invention to a granulation treatment.
  • binder to be used for producing the granulated powder examples include polyolefins such as polyethylene, polypropylene, and ethylene-vinyl acetate copolymers, acrylic resins such as polymethyl methacrylate and polybutyl methacrylate, styrenic resins such as polystyrene, polyesters such as polyvinyl chloride, polyvinylidene chloride, polyamide, polyethylene terephthalate, and polybutylene terephthalate, various resins such as polyether, polyvinyl alcohol, polyvinylpyrrolidone, and copolymers thereof, and various organic binders such as various waxes, paraffins, higher fatty acids (such as stearic acid), higher alcohols, higher fatty acid esters, and higher fatty acid amides. These can be used alone or by mixing two or more types thereof.
  • a binder containing a polyvinyl alcohol or polyvinylpyrrolidone is preferred.
  • These binder components have a high binding ability, and therefore can efficiently form the granulated powder even in a relatively small amount. Further, the thermal decomposability thereof is also high, and therefore, the binder can be reliably decomposed and removed in a short time during degreasing and firing.
  • the content of the binder is preferably about 0.2% by mass or more and 10% by mass or less, more preferably about 0.3% by mass or more and 5% by mass or less, further more preferably about 0.3% by mass or more and 2% by mass or less with respect to the total amount of the granulated powder.
  • a difference in size between the molded body and the degreased body, that is, so-called a shrinkage ratio is optimized, whereby a decrease in the dimensional accuracy of the finally obtained sintered body can be prevented.
  • any of a variety of additives such as a plasticizer, a lubricant, an antioxidant, a degreasing accelerator, and a surfactant may be added as needed.
  • Examples of the granulation treatment include a spray drying method, a tumbling granulation method, a fluidized bed granulation method, and a tumbling fluidized bed granulation method.
  • a solvent which dissolves the binder is used as needed.
  • the solvent include inorganic solvents such as water and carbon tetrachloride, and organic solvents such as ketone-based solvents, alcohol-based solvents, ether-based solvents, cellosolve-based solvents, aliphatic hydrocarbon-based solvents, aromatic hydrocarbon-based solvents, aromatic heterocyclic compound-based solvents, amide-based solvents, halogen compound-based solvents, ester-based solvents, amine-based solvents, nitrile-based solvents, nitro-based solvents, and aldehyde-based solvents, and one type or a mixture of two or more types selected from these solvents is used.
  • the average particle diameter of the granulated powder is not particularly limited, but is preferably about 10 ⁇ m or more and 200 ⁇ m or less, more preferably about 20 ⁇ m or more and 100 ⁇ m or less, further more preferably about 25 ⁇ m or more and 60 ⁇ m or less.
  • the granulated powder having such a particle diameter has favorable fluidity, and can more faithfully reflect the shape of a molding die.
  • the average particle diameter can be obtained as a particle diameter when the cumulative amount obtained by cumulating the percentages of the particles from the smaller diameter side reaches 50% in a cumulative particle size distribution on amass basis obtained by laser diffractometry.
  • the kneaded material or the granulated powder is molded, whereby a molded body having the same shape as that of a target sintered body is produced.
  • the method for producing a molded body is not particularly limited, and for example, any of a variety of molding methods such as a powder compacting (compression molding) method, a metal injection molding (MIM) method, and an extrusion molding method can be used.
  • the molding conditions in the case of a powder compacting method among these methods are preferably such that the molding pressure is about 200 MPa or more and 1000 MPa or less (2 t/cm 2 or more and 10 t/cm 2 or less), which vary depending on the respective conditions such as the composition and the particle diameter of the metal powder for powder metallurgy to be used, the composition of the binder, and the blending amount thereof.
  • the molding conditions in the case of a metal injection molding method are preferably such that the material temperature is about 80° C. or higher and 210° C. or lower, and the injection pressure is about 50 MPa or more and 500 MPa or less (0.5 t/cm 2 or more and 5 t/cm 2 or less), which vary depending on the respective conditions.
  • the molding conditions in the case of an extrusion molding method are preferably such that the material temperature is about 80° C. or higher and 210° C. or lower, and the extrusion pressure is about 50 MPa or more and 500 MPa or less (0.5 t/cm 2 or more and 5 t/cm 2 or less), which vary depending on the respective conditions.
  • the thus obtained molded body is in a state where the binder is uniformly distributed in spaces between the particles of the metal powder.
  • the shape and size of the molded body to be produced are determined in anticipation of shrinkage of the molded body in the subsequent degreasing step and firing step.
  • the binder is decomposed by heating the molded body, whereby the binder is removed from the molded body. In this manner, the degreasing treatment is performed.
  • Examples of the degreasing treatment include a method of heating the molded body and a method of exposing the molded body to a gas capable of decomposing the binder.
  • the conditions for heating the molded body are preferably such that the temperature is about 100° C. or higher and 750° C. or lower and the time is about 0.1 hours or more and 20 hours or less, and more preferably such that the temperature is about 150° C. or higher and 600° C. or lower and the time is about 0.5 hours or more and 15 hours or less, which slightly vary depending on the composition and the blending amount of the binder.
  • the degreasing of the molded body can be necessarily and sufficiently performed without sintering the molded body. As a result, it is possible to reliably prevent the binder component from remaining inside the degreased body in a large amount.
  • the atmosphere when the molded body is heated is not particularly limited, and an atmosphere of a reducing gas such as hydrogen, an atmosphere of an inert gas such as nitrogen or argon, an atmosphere of an oxidative gas such as air, a reduced pressure atmosphere obtained by reducing the pressure of such an atmosphere, or the like can be used.
  • a reducing gas such as hydrogen
  • an atmosphere of an inert gas such as nitrogen or argon
  • an atmosphere of an oxidative gas such as air
  • a reduced pressure atmosphere obtained by reducing the pressure of such an atmosphere, or the like can be used.
  • Examples of the gas capable of decomposing the binder include ozone gas.
  • this degreasing step into a plurality of steps in which the degreasing conditions are different, and performing the plurality of steps, the binder in the molded body can be more rapidly decomposed and removed so that the binder does not remain in the molded body.
  • the degreased body may be subjected to a machining process such as grinding, polishing, or cutting.
  • the degreased body has a relatively low hardness and relatively high plasticity, and therefore, the machining process can be easily performed while preventing the degreased body from losing its shape. According to such a machining process, a sintered body having high dimensional accuracy can be easily obtained in the end.
  • the degreased body obtained in the above step (C) is fired in a firing furnace, whereby a sintered body is obtained.
  • the firing temperature varies depending on the composition, the particle diameter, and the like of the metal powder for powder metallurgy used in the production of the molded body and the degreased body, but is set to, for example, about 980° C. or higher and 1330° C. or lower, and preferably set to about 1050° C. or higher and 1260° C. or lower.
  • the firing time is set to 0.2 hours or more and 7 hours or less, but is preferably set to about 1 hour or more and 6 hours or less.
  • the firing temperature or the below-described firing atmosphere may be changed in the middle of the step.
  • the firing temperature is a relatively low temperature, it is easy to control the heating temperature in the firing furnace to be a fixed temperature, and therefore, it is also easy to maintain the temperature of the degreased body at a fixed temperature. As a result, a more homogeneous sintered body can be produced.
  • the firing temperature as described above is a temperature which can be sufficiently realized using a common firing furnace, and therefore, an inexpensive firing furnace can be used, and also the running cost can be kept low. In other words, in the case where the temperature exceeds the above-mentioned firing temperature, it is necessary to employ an expensive firing furnace using a special heat resistant material, and also the running cost may be increased.
  • the atmosphere when performing firing is not particularly limited, however, in consideration of prevention of significant oxidation of the metal powder, an atmosphere of a reducing gas such as hydrogen, an atmosphere of an inert gas such as argon, a reduced pressure atmosphere obtained by reducing the pressure of such an atmosphere, or the like is preferably used.
  • the thus obtained sintered body has a high density and excellent mechanical properties. That is, a sintered body produced by molding a composition containing the metal powder for powder metallurgy according to the invention and a binder, followed by degreasing and sintering has a higher relative density than a sintered body obtained by sintering a metal powder in the related art. Therefore, according to the invention, a sintered body having a high density which could not be obtained unless an additional treatment such as an HIP treatment is performed can be realized without performing an additional treatment.
  • the relative density can be expected to be increased by 2% or more as compared with the related art, which slightly varies depending on the composition of the metal powder for powder metallurgy.
  • the relative density of the obtained sintered body can be expected to be, for example, 97% or more (preferably 98% or more, more preferably 98.5% or more).
  • the sintered body having a relative density within such a range has excellent mechanical properties comparable to those of ingot materials although it has a shape as close as possible to a desired shape by using a powder metallurgy technique, and therefore, the sintered body can be applied to a variety of machine parts, structural parts, and the like with virtually no post-processing.
  • the tensile strength and the 0.2% proof stress of a sintered body produced by molding a composition containing the metal powder for powder metallurgy according to the invention and a binder, followed by degreasing and sintering are higher than those of a sintered body obtained by performing sintering in the same manner using a metal powder in the related art. This is considered to be because by optimizing the alloy composition and the particle structure, the sinterability of the metal powder is enhanced, and thus, the mechanical properties of a sintered body to be produced using the metal powder are enhanced.
  • the sintered body produced as described above has a high surface hardness.
  • the Vickers hardness of the surface of the sintered body is expected to be 140 or more and 500 or less, also preferably expected to be 150 or more and 400 or less, which slightly varies depending on the composition of the metal powder for powder metallurgy.
  • the Vickers hardness of the surface of the sintered body is expected to be 570 or more and 1200 or less, also preferably expected to be 600 or more and 1000 or less.
  • the sintered body having such a hardness has particularly high durability.
  • the sintered body has a sufficiently high density and excellent mechanical properties even without performing an additional treatment, however, in order to further increase the density and enhance the mechanical properties, a variety of additional treatments may be performed.
  • the content of C in the final sintered body may change within the range of 5% or more and 100% or less (preferably within the range of 30% or more and 100% or less) of the content of C in the metal powder for powder metallurgy, which varies depending on the conditions for the step or the conditions for the treatment.
  • the content of 0 in the final sintered body may change within the range of 1% or more and 50% or less (preferably within the range of 3% or more and 50% or less) of the content of 0 in the metal powder for powder metallurgy, which varies depending on the conditions for the step or the conditions for the treatment.
  • the produced sintered body may be subjected to an HIP treatment as part of the additional treatments to be performed as needed, however, even if the HIP treatment is performed, a sufficient effect is not exhibited in many cases.
  • the density of the sintered body can be further increased, however, in the first place, the density of the sintered body obtained according to the invention has already been sufficiently increased at the end of the firing step. Therefore, even if the HIP treatment is further performed, densification hardly proceeds any further.
  • the material to be treated may be contaminated, the composition or the physical properties of the material to be treated may unintentionally change accompanying the contamination, or the color of the material to be treated may change accompanying the contamination.
  • residual stress is generated or increased in the material to be treated, and a problem such as a change in the shape or a decrease in the dimensional accuracy may occur as the residual stress is released over time.
  • a sintered body having a sufficiently high density can be produced without performing such an HIP treatment, and therefore, a sintered body having an increased density and also an increased strength can be obtained in the same manner as in the case of performing an HIP treatment.
  • Such a sintered body is less contaminated and discolored, and also an unintended change in the composition or physical properties, or the like occurs less, and also a problem such as a change in the shape or a decrease in the dimensional accuracy occurs less. Therefore, according to the invention, a sintered body having high mechanical strength and dimensional accuracy, and excellent durability can be efficiently produced.
  • the sintered body produced according to the invention requires almost no additional treatments for enhancing the mechanical properties, and therefore, the composition and the crystal structure tend to become uniform in the entire sintered body. Due to this, the sintered body has high structural anisotropy and therefore has excellent durability against a load from every direction regardless of its shape.
  • the porosity near the surface thereof is often relatively lower than inside the sintered body.
  • the reason therefor is not clear, however, one of the reasons is that by the addition of the first element and the second element, the sintering reaction more easily proceeds near the surface of the molded body than inside the molded body.
  • A2 ⁇ A1 is preferably 0.1% or more and 3% or less, more preferably 0.2% or more and 2% or less.
  • the sintered body showing the value of A2 ⁇ A1 within the above range not only has necessary and sufficient mechanical strength, but also can easily flatten the surface. That is, by polishing the surface of such a sintered body, a surface having high specularity can be obtained.
  • Such a sintered body having high specularity not only has high mechanical strength, but also has excellent aesthetic properties. Therefore, such a sintered body is favorably used also for application requiring excellent aesthetic appearance.
  • the porosity A1 near the surface of the sintered body refers to a porosity in a 25- ⁇ m radius region centered on the position at a depth of 50 ⁇ m from the surface of the cross section of the sintered body.
  • the porosity A2 inside the sintered body refers to a porosity in a 25- ⁇ m radius region centered on the position at a depth of 300 ⁇ m from the surface of the cross section of the sintered body.
  • the metal powder for powder metallurgy, the compound, the granulated powder, and the sintered body according to the invention have been described with reference to preferred embodiments, however, the invention is not limited thereto.
  • the sintered body according to the invention is used for, for example, parts for transport machinery such as parts for automobiles, parts for bicycles, parts for railroad cars, parts for ships, parts for airplanes, and parts for space transport machinery (such as rockets); parts for electronic devices such as parts for personal computers and parts for mobile phone terminals; parts for electrical devices such as refrigerators, washing machines, and cooling and heating machines; parts for machines such as machine tools and semiconductor production devices; parts for plants such as atomic power plants, thermal power plants, hydroelectric power plants, oil refinery plants, and chemical complexes; parts for timepieces, metallic tableware, jewels, ornaments such as frames for glasses, and all other sorts of structural parts.
  • parts for transport machinery such as parts for automobiles, parts for bicycles, parts for railroad cars, parts for ships, parts for airplanes, and parts for space transport machinery (such as rockets); parts for electronic devices such as parts for personal computers and parts for mobile phone terminals; parts for electrical devices such as refrigerators, washing machines, and cooling and heating machines; parts for machines such as machine tools and semiconductor production
  • a metal powder having a composition shown in Table 1 produced by a water atomization method was prepared.
  • This metal powder had an average particle diameter of 4.05 ⁇ m, a tap density of 4.15 g/cm 3 , and a specific surface area of 0.21 m 2 /g.
  • this mixed starting material was kneaded using a kneader, whereby a compound was obtained.
  • this compound was molded using an injection molding device under the following molding conditions, whereby a molded body was produced.
  • the obtained degreased body was fired under the following firing conditions, whereby a sintered body was obtained.
  • the shape of the sintered body was determined to be a cylinder with a diameter of 10 mm and a thickness of 5 mm.
  • Sintered bodies were obtained in the same manner as the method for producing the sintered body of sample No. 1 except that the composition and the like of the metal powder for powder metallurgy were changed as shown in Table 1, respectively.
  • the sintered body of sample No. 30 was obtained by performing an HIP treatment under the following conditions after firing. Further, the sintered bodies of sample Nos. 18 to 20 were obtained by using the metal powder produced by a gas atomization method, respectively, and indicated by “gas” in the column of Remarks in Table 1.
  • Each sintered body contained very small amounts of impurities, but the description thereof in Table 1 is omitted.
  • Sintered bodies were obtained in the same manner as the method for producing the sintered body of sample No. 1 except that the composition and the like of the metal powder for powder metallurgy were changed as shown in Table 2, respectively.
  • the sintered body of sample No. 48 was obtained by performing an HIP treatment under the following conditions after firing. Further, the sintered bodies of sample Nos. 41 to 43 were obtained by using the metal powder produced by a gas atomization method, respectively, and indicated by “gas” in the column of Remarks in Table 2.
  • Each sintered body contained very small amounts of impurities, but the description thereof in Table 2 is omitted.
  • Sintered bodies were obtained in the same manner as the method for producing the sintered body of sample No. 1 except that the composition and the like of the metal powder for powder metallurgy were changed as shown in Table 3, respectively.
  • the sintered body of sample No. 66 was obtained by performing an HIP treatment under the following conditions after firing. Further, the sintered bodies of sample Nos. 59 to 61 were obtained by using the metal powder produced by a gas atomization method, respectively, and indicated by “gas” in the column of Remarks in Table 3.
  • Example 16.58 7.45 0.56 0.128 0.06 0.08 0.05 0.48 0.25 remainder 0.75 0.14 0.25 1.09
  • Example 15.72 10.25 0.36 0.058 0.04 0.09 2.54 0.07 0.21 remainder 0.44 0.13 0.36 2.24 No.
  • Example 19.11 8.43 0.64 0.045 0.07 0.07 0.00 0.23 0.12 remainder 1.00 0.14 0.22 3.11 gas No.
  • Example 19.72 9.65 0.85 0.048 0.06 0.11 0.09 0.05 0.14 remainder 0.55 0.17 0.20 3.54 gas No.
  • Example 18.25 10.21 0.46 0.015 0.12 0.12 0.06 0.09 0.18 remainder 1.00 0.24 0.52 16.00 gas No.
  • Each sintered body contained very small amounts of impurities, but the description thereof in Table 3 is omitted.
  • the metal powder was granulated by a spray drying method.
  • the binder used at this time was polyvinyl alcohol, which was used in an amount of 1 part by mass with respect to 100 parts by mass of the metal powder. Further, a solvent (ion exchanged water) was used in an amount of 50 parts by mass with respect to 1 part by mass of polyvinyl alcohol. In this manner, a granulated powder having an average particle diameter of 50 ⁇ m was obtained.
  • this granulated powder was subjected to powder compacting under the following molding conditions.
  • a press molding machine was used.
  • the shape of the molded body to be produced was determined to be a cube with a side length of 20 mm.
  • Sintered bodies were obtained in the same manner as in the case of sample No. 67 except that the composition and the like of the metal powder for powder metallurgy were changed as shown in Table 4, respectively.
  • the sintered body of sample No. 85 was obtained by performing an HIP treatment under the following conditions after firing.
  • Each sintered body contained very small amounts of impurities, but the description thereof in Table 4 is omitted.
  • Sintered bodies were obtained in the same manner as in the case of sample No. 1 except that the composition and the like of the metal powder for powder metallurgy were changed as shown in Table 5, respectively.
  • Example No. 90 Example 1.06 0.02 0.73 0.724 0.08 0.08 0.19 0.78 0.25 remainder 1.00 0.16 0.22 0.22 No. 91
  • Each sintered body contained very small amounts of impurities, but the description thereof in Table 5 is omitted.
  • the time of execution of sputtering was converted into a depth from the surface of the particle (sputter depth) and shown on the horizontal axis, and also the content of an atom (atomic concentration) determined by the Auger electron spectroscopy was shown on the vertical axis, and the analytical results were plotted, whereby Auger electron spectra were obtained.
  • the Auger electron spectra obtained from the particle of the metal powder for powder metallurgy of sample No. 1 are shown in FIG. 3 .
  • the four horizontal straight lines drawn overlapping the spectra indicate the contents of Fe, Cr, Si, and O in the whole particle of sample No. 1, respectively.
  • the content of Cr little fluctuates in a region from the surface (at a depth of 0 nm) to a depth of 60 nm. Accordingly, it is confirmed that the content of Cr on the surface of the particle (Cr(0)) falls within the range of 70% or more and 170% or less the content of Cr at a depth of 60 nm from the surface of the particle (Cr(60)).
  • the content of Cr on the surface of the particle (Cr(0)) falls within the range of 0.2% by atom or more and 15% by atom or less.
  • the Auger electron spectra obtained from the particle of the metal powder for powder metallurgy of sample No. 23 are shown in FIG. 4 .
  • the four horizontal straight lines drawn overlapping the spectra indicate the contents of Fe, Cr, Si, and O in the whole particle of sample No. 23, respectively.
  • the content of Si on the surface of the particle (Si(0)), the content of Si at a depth of 60 nm from the surface of the particle (Si(60)), and the content of O on the surface of the particle (O(0)) were determined.
  • the sintered density was measured in accordance with the method for measuring the density of sintered metal materials specified in JIS Z 2501 (2000), and also the relative density of each sintered body was calculated with reference to the true density of the metal powder for powder metallurgy used for producing each sintered body.
  • the Vickers hardness was measured in accordance with the Vickers hardness test method specified in JIS Z 2244 (2009).
  • the tensile strength of the sintered body is 520 MPa or more.
  • the tensile strength of the sintered body is 510 MPa or more and less than 520 MPa.
  • the tensile strength of the sintered body is 500 MPa or more and less than 510 MPa.
  • the tensile strength of the sintered body is 490 MPa or more and less than 500 MPa.
  • the tensile strength of the sintered body is 480 MPa or more and less than 490 MPa.
  • the tensile strength of the sintered body is less than 480 MPa.
  • the tensile strength of the sintered body is 560 MPa or more.
  • the tensile strength of the sintered body is 550 MPa or more and less than 560 MPa.
  • the tensile strength of the sintered body is 540 MPa or more and less than 550 MPa.
  • the tensile strength of the sintered body is 530 MPa or more and less than 540 MPa.
  • the tensile strength of the sintered body is 520 MPa or more and less than 530 MPa.
  • the tensile strength of the sintered body is less than 520 MPa.
  • the 0.2% proof stress of the sintered body is 195 MPa or more.
  • the 0.2% proof stress of the sintered body is 190 MPa or more and less than 195 MPa.
  • the 0.2% proof stress of the sintered body is 185 MPa or more and less than 190 MPa.
  • the 0.2% proof stress of the sintered body is 175 MPa or more and less than 180 MPa.
  • the 0.2% proof stress of the sintered body is 225 MPa or more.
  • the 0.2% proof stress of the sintered body is 215 MPa or more and less than 220 MPa.
  • the 0.2% proof stress of the sintered body is 210 MPa or more and less than 215 MPa.
  • the 0.2% proof stress of the sintered body is 205 MPa or more and less than 210 MPa.
  • the 0.2% proof stress of the sintered body is less than 205 MPa.
  • the elongation of the sintered body is 48% or more.
  • the elongation of the sintered body is 44% or more and less than 46%.
  • the elongation of the sintered body is 42% or more and less than 44%.
  • the elongation of the sintered body is less than 40%.
  • the fatigue strength was measured in accordance with the test method specified in JIS Z 2273 (1978).
  • the waveform of an applied load corresponding to a repeated stress was set to an alternating sine wave, and the minimum/maximum stress ratio (minimum stress/maximum stress) was set to 0.1. Further, the repeated frequency was set to 30 Hz, and the repeat count was set to 1 ⁇ 10 7 .
  • the measured fatigue strength was evaluated according to the following evaluation criteria.
  • the fatigue strength of the sintered body is 260 MPa or more.
  • the fatigue strength of the sintered body is 240 MPa or more and less than 260 MPa.
  • the fatigue strength of the sintered body is 200 MPa or more and less than 220 MPa.
  • the fatigue strength of the sintered body is 180 MPa or more and less than 200 MPa.
  • the fatigue strength of the sintered body is less than 180 MPa.
  • Example 7.25 — — — — — — — — — No. 21 Compar- 3.77 20.4 9.5 214.7 22.6 15.2 148.7 10.1 0.45 ative Example No.
  • Example 98.8 156 B B A B No. 8 Example 98.3 149 B B A B No. 9
  • Example 98.1 148 B B B B No. 10 Example 98.5 152 B B A B No. 11
  • Example 98.1 146 B B B B No. 12 Example 97.8 144 B B C B No. 13
  • Example 97.6 142 C C C C No. 14 Example 97.5 144 B C C C No. 15
  • Example 97.8 141 B B B B B No. 17 Example 97.3 163 B B C B No. 18
  • Example 99.3 161 A A A A No. 19 Example 99.4 171 A A A A No. 20
  • Example 99.1 164 A A A A No.
  • the sintered bodies corresponding to Example each have a higher relative density than the sintered bodies corresponding to Comparative Example (excluding the sintered bodies having undergone the HIP treatment). Further, it was also confirmed that there is a significant difference in properties such as tensile strength, 0.2% proof stress, elongation, and fatigue strength between the sintered bodies corresponding to Example and the sintered bodies corresponding to Comparative Example (excluding the sintered bodies having undergone the HIP treatment).
  • Sintered bodies were obtained in the same manner as the method for producing the sintered body of sample No. 1 except that the composition and the like of the metal powder for powder metallurgy were changed as shown in Tables 11 to 14, respectively.
  • Each sintered body contained very small amounts of impurities, but the description thereof in Tables 11 to 14 is omitted.
  • the content of Cr on the surface of the particle (Cr(0)), the content of Cr at a depth of 60 nm from the surface of the particle (Cr(60)), the content of Si on the surface of the particle (Si(0)), the content of Si at a depth of 60 nm from the surface of the particle (Si(60)), and the content of O on the surface of the particle (O(0)) were determined.
  • the content of Cr on the surface (Cr(0)) falls within the range of 70% or more and 170% or less the content of Cr at a depth of 60 nm from the surface of the particle (Cr(60)).
  • the content of Cr on the surface of the particle 1 (Cr(0)) falls within the range of 0.2% by atom or more and 15% by atom or less.
  • the sintered density was measured in accordance with the method for measuring the density of sintered metal materials specified in JIS Z 2501 (2000), and also the relative density of each sintered body was calculated with reference to the true density of the metal powder for powder metallurgy used for producing each sintered body.
  • the Vickers hardness was measured in accordance with the Vickers hardness test method specified in JIS Z 2244 (2009).
  • the sintered bodies corresponding to Example each have a higher relative density than the sintered bodies corresponding to Comparative Example. It was also confirmed that there is a significant difference in properties such as tensile strength, 0.2% proof stress, and elongation between the sintered bodies corresponding to Example and the sintered bodies corresponding to Comparative Example.
  • Sintered bodies were obtained in the same manner as the method for producing the sintered body of sample No. 1 except that the composition and the like of the metal powder for powder metallurgy were changed as shown in Table 19, respectively.
  • a metal powder having an average particle diameter of 4.62 ⁇ m, a Ti powder having an average particle diameter of 40 ⁇ m, and a Nb powder having an average particle diameter of 25 ⁇ m were mixed, whereby a mixed powder was prepared.
  • each of the mixing amounts of the metal powder, the Ti powder, and the Nb powder was adjusted so that the composition of the mixed powder was as shown in Table 19.
  • Example No. 153 Compar- 17.56 14.51 0.78 0.032 0.12 0.00 2.68 0.11 0.33 remainder — 0.12 0.15 3.75 ative Example No.
  • Each sintered body contained very small amounts of impurities, but the description thereof in Table 19 is omitted.
  • the content of Cr on the surface of the particle (Cr(0)), the content of Cr at a depth of 60 nm from the surface of the particle (Cr(60)), the content of Si on the surface of the particle (Si(0)), the content of Si at a depth of 60 nm from the surface of the particle (Si(60)), and the content of O on the surface of the particle (O(0)) were determined.
  • the content of Cr on the surface (Cr(0)) fell within the range of 70% or more and 170% or less the content of Cr at a depth of 60 nm from the surface of the particle (Cr(60)).
  • the content of Cr on the surface of the particle (Cr(0)) fell within the range of 0.2% by atom or more and 15% by atom or less.
  • the sintered density was measured in accordance with the method for measuring the density of sintered metal materials specified in JIS Z 2501 (2000), and also the relative density of each sintered body was calculated with reference to the true density of the metal powder for powder metallurgy used for producing each sintered body.
  • the Vickers hardness was measured in accordance with the Vickers hardness test method specified in JIS Z 2244 (2009).
  • the sintered bodies corresponding to Example each have a higher relative density than the sintered bodies corresponding to Comparative Example. It was also confirmed that there is a significant difference in properties such as tensile strength, 0.2% proof stress, and elongation between the sintered bodies corresponding to Example and the sintered bodies corresponding to Comparative Example.
  • Sintered bodies were obtained in the same manner as the method for producing the sintered body of sample No. 1 except that the composition and the like of the metal powder for powder metallurgy were changed as shown in Table 21, respectively.
  • No. 163 Compar- 17.11 12.29 0.74 0.064 0.00 0.05 2.18 0.15 0.29 remainder 0.00 0.05 0.07 0.78 ative
  • Each sintered body contained very small amounts of impurities, but the description thereof in Table 21 is omitted.
  • the content of Cr on the surface of the particle (Cr(0)), the content of Cr at a depth of 60 nm from the surface of the particle (Cr(60)), the content of Si on the surface of the particle (Si(0)), the content of Si at a depth of 60 nm from the surface of the particle (Si(60)), and the content of O on the surface of the particle (O(0)) were determined.
  • the content of Cr on the surface (Cr(0)) fell within the range of 70% or more and 170% or less the content of Cr at a depth of 60 nm from the surface of the particle (Cr(60)).
  • the content of Cr on the surface of the particle (Cr(0)) fell within the range of 0.2% by atom or more and 15% by atom or less.
  • the sintered density was measured in accordance with the method for measuring the density of sintered metal materials specified in JIS Z 2501 (2000), and also the relative density of each sintered body was calculated with reference to the true density of the metal powder for powder metallurgy used for producing each sintered body.
  • the Vickers hardness was measured in accordance with the Vickers hardness test method specified in JIS Z 2244 (2009).
  • the sintered bodies corresponding to Example each have a higher relative density than the sintered bodies corresponding to Comparative Example. It was also confirmed that there is a significant difference in properties such as tensile strength, 0.2% proof stress, and elongation between the sintered bodies corresponding to Example and the sintered bodies corresponding to Comparative Example.
  • Sintered bodies were obtained in the same manner as the method for producing the sintered body of sample No. 1 except that the composition and the like of the metal powder for powder metallurgy were changed as shown in Table 23, respectively.
  • Each sintered body contained very small amounts of impurities, but the description thereof in Table 23 is omitted.
  • the content of Cr on the surface of the particle (Cr(0)), the content of Cr at a depth of 60 nm from the surface of the particle (Cr(60)), the content of Si on the surface of the particle (Si(0)), the content of Si at a depth of 60 nm from the surface of the particle (Si(60)), and the content of O on the surface of the particle (O(0)) were determined.
  • the content of Cr on the surface (Cr(0)) fell within the range of 70% or more and 170% or less the content of Cr at a depth of 60 nm from the surface of the particle (Cr(60)).
  • the content of Cr on the surface of the particle (Cr(0)) fell within the range of 0.2% by atom or more and 15% by atom or less.
  • the sintered density was measured in accordance with the method for measuring the density of sintered metal materials specified in JIS Z 2501 (2000), and also the relative density of each sintered body was calculated with reference to the true density of the metal powder for powder metallurgy used for producing each sintered body.
  • the Vickers hardness was measured in accordance with the Vickers hardness test method specified in JIS Z 2244 (2009).
  • the sintered bodies corresponding to Example each have a higher relative density than the sintered bodies corresponding to Comparative Example. It was also confirmed that there is a significant difference in properties such as tensile strength, 0.2% proof stress, and elongation between the sintered bodies corresponding to Example and the sintered bodies corresponding to Comparative Example.
  • Sintered bodies were obtained in the same manner as the method for producing the sintered body of sample No. 1 except that the composition and the like of the metal powder for powder metallurgy were changed as shown in Table 25, respectively.
  • Each sintered body contained very small amounts of impurities, but the description thereof in Table 25 is omitted.
  • the content of Cr on the surface of the particle (Cr(0)), the content of Cr at a depth of 60 nm from the surface of the particle (Cr(60)), the content of Si on the surface of the particle (Si(0)), the content of Si at a depth of 60 nm from the surface of the particle (Si(60)), and the content of O on the surface of the particle (O(0)) were determined.
  • the content of Cr on the surface (Cr(0)) fell within the range of 70% or more and 170% or less the content of Cr at a depth of 60 nm from the surface of the particle (Cr(60)).
  • the content of Cr on the surface of the particle (Cr(0)) fell within the range of 0.2% by atom or more and 15% by atom or less.
  • the sintered density was measured in accordance with the method for measuring the density of sintered metal materials specified in JIS Z 2501 (2000), and also the relative density of each sintered body was calculated with reference to the true density of the metal powder for powder metallurgy used for producing each sintered body.
  • the sintered bodies corresponding to Example each have a higher relative density than the sintered bodies corresponding to Comparative Example. It was also confirmed that there is a significant difference in properties such as tensile strength, 0.2% proof stress, and elongation between the sintered bodies corresponding to Example and the sintered bodies corresponding to Comparative Example.
  • Sintered bodies were obtained in the same manner as the method for producing the sintered body of sample No. 1 except that the composition and the like of the metal powder for powder metallurgy were changed as shown in Table 27, respectively.
  • No. 194 Compar- 17.44 12.47 0.72 0.055 0.00 0.06 2.75 0.18 0.26 remainder 0.00 0.06 0.08 1.09 ative
  • Example No. 195 Compar- 16.54 12.87 0.78 0.032 0.09 0.00 2.69 0.08 0.35 remainder — 0.09 0.12 2.81 ative Example No.
  • the content of Cr on the surface (Cr(0)) fell within the range of 70% or more and 170% or less the content of Cr at a depth of 60 nm from the surface of the particle (Cr(60)).
  • the content of Cr on the surface of the particle (Cr(0)) fell within the range of 0.2% by atom or more and 15% by atom or less.
  • the sintered density was measured in accordance with the method for measuring the density of sintered metal materials specified in JIS Z 2501 (2000), and also the relative density of each sintered body was calculated with reference to the true density of the metal powder for powder metallurgy used for producing each sintered body.
  • the sintered bodies corresponding to Example each have a higher relative density than the sintered bodies corresponding to Comparative Example. It was also confirmed that there is a significant difference in properties such as tensile strength, 0.2% proof stress, and elongation between the sintered bodies corresponding to Example and the sintered bodies corresponding to Comparative Example.
  • No. 204 Compar- 17.24 12.14 0.77 0.018 0.00 0.06 2.56 0.08 0.27 remainder 0.00 0.06 0.08 3.33 ative
  • Example No. 205 Compar- 16.87 12.56 0.82 0.026 0.09 0.00 2.24 0.09 0.32 remainder — 0.09 0.11 3.46 ative Example No.
  • Each sintered body contained very small amounts of impurities, but the description thereof in Tables 29 and 30 is omitted.
  • the content of Cr on the surface of the particle (Cr(0)), the content of Cr at a depth of 60 nm from the surface of the particle (Cr(60)), the content of Si on the surface of the particle (Si(0)), the content of Si at a depth of 60 nm from the surface of the particle (Si(60)), and the content of O on the surface of the particle (O(0)) were determined.
  • the content of Cr on the surface of the particle (Cr(0)) fell within the range of 0.2% by atom or more and 15% by atom or less.
  • the sintered bodies corresponding to Example each have a higher relative density than the sintered bodies corresponding to Comparative Example. It was also confirmed that there is a significant difference in properties such as tensile strength, 0.2% proof stress, and elongation between the sintered bodies corresponding to Example and the sintered bodies corresponding to Comparative Example.
  • Sintered bodies were obtained in the same manner as the method for producing the sintered body of sample No. 1 except that the composition and the like of the metal powder for powder metallurgy were changed as shown in Tables 33 and 34, respectively.
  • No. 219 Compar- 16.34 12.63 0.77 0.054 0.00 0.06 2.84 0.08 0.36 remainder 0.00 0.06 0.08 1.11 ative
  • Example No. 220 Compar- 16.78 12.24 0.78 0.032 0.09 0.00 2.64 0.11 0.27 remainder — 0.09 0.12 2.81 ative Example No.
  • Each sintered body contained very small amounts of impurities, but the description thereof in Tables 33 and 34 is omitted.
  • the content of Cr on the surface of the particle (Cr(0)), the content of Cr at a depth of 60 nm from the surface of the particle (Cr(60)), the content of Si on the surface of the particle (Si(0)), the content of Si at a depth of 60 nm from the surface of the particle (Si(60)), and the content of O on the surface of the particle (O(0)) were determined.
  • the content of Cr on the surface (Cr(0)) fell within the range of 70% or more and 170% or less the content of Cr at a depth of 60 nm from the surface of the particle (Cr(60)).
  • the content of Cr on the surface of the particle (Cr(0)) fell within the range of 0.2% by atom or more and 15% by atom or less.
  • the sintered density was measured in accordance with the method for measuring the density of sintered metal materials specified in JIS Z 2501 (2000), and also the relative density of each sintered body was calculated with reference to the true density of the metal powder for powder metallurgy used for producing each sintered body.
  • the Vickers hardness was measured in accordance with the Vickers hardness test method specified in JIS Z 2244 (2009).
  • the sintered bodies corresponding to Example each have a higher relative density than the sintered bodies corresponding to Comparative Example. It was also confirmed that there is a significant difference in properties such as tensile strength, 0.2% proof stress, and elongation between the sintered bodies corresponding to Example and the sintered bodies corresponding to Comparative Example.
  • each of the sintered bodies of the respective sample Nos. shown in Table 37 was cut and the cross section was polished.
  • each of the sintered bodies of the respective sample Nos. shown in Table 37 was subjected to a barrel polishing treatment.
  • the specular gloss of the sintered body was measured in accordance with the method for measuring the specular gloss specified in JIS Z 8741 (1997).
  • the incident angle of light with respect to the surface of the sintered body was set to 60°, and as a reference plane for calculating the specular gloss, a glass having a specular gloss of 90 and a refractive index of 1.500 was used.
  • the measured specular gloss was evaluated according to the following evaluation criteria.
  • A The specularity of the surface is very high (the specular gloss is 200 or more).
  • the specularity of the surface is high (the specular gloss is 150 or more and less than 200).
  • the specularity of the surface is slightly high (the specular gloss is 100 or more and less than 150).
  • the specularity of the surface is slightly low (the specular gloss is 60 or more and less than 100).
  • the specularity of the surface is low (the specular gloss is 30 or more and less than 60).
  • the specularity of the surface is very low (the specular gloss is less than 30).
  • the sintered bodies corresponding to Example each have a higher specular gloss than the sintered bodies corresponding to Comparative Example. This is considered to be because the porosity near the surface of the sintered body is low, and therefore, light scattering is suppressed, however, the ratio of regular reflection is increased.

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CN116100016A (zh) * 2023-03-27 2023-05-12 西南应用磁学研究所(中国电子科技集团公司第九研究所) 一种制备铁硅铬软磁金属粉末的方法及其制得的软磁金属粉末的应用

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