WO2011129422A1 - 被覆ｃＢＮ焼結体 - Google Patents

被覆ｃＢＮ焼結体 Download PDF

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Publication number
WO2011129422A1
WO2011129422A1 PCT/JP2011/059334 JP2011059334W WO2011129422A1 WO 2011129422 A1 WO2011129422 A1 WO 2011129422A1 JP 2011059334 W JP2011059334 W JP 2011059334W WO 2011129422 A1 WO2011129422 A1 WO 2011129422A1
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WIPO (PCT)
Prior art keywords
sintered body
cbn
cbn sintered
coated
body according
Prior art date
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Ceased
Application number
PCT/JP2011/059334
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English (en)
French (fr)
Inventor
貴英 工藤
香川　直宏
崇 梅村
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tungaloy Corp
Original Assignee
Tungaloy Corp
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Application filed by Tungaloy Corp filed Critical Tungaloy Corp
Priority to JP2012510701A priority Critical patent/JPWO2011129422A1/ja
Priority to EP11768943.0A priority patent/EP2559504B1/en
Priority to US13/639,994 priority patent/US8999531B2/en
Publication of WO2011129422A1 publication Critical patent/WO2011129422A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C22C—ALLOYS
    • C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
    • 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
    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/80—Phases present in the sintered or melt-cast ceramic products other than the main phase
    • C04B2235/85—Intergranular or grain boundary phases
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
    • C04B2237/32—Ceramic
    • C04B2237/36—Non-oxidic
    • C04B2237/361—Boron nitride
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
    • C04B2237/40—Metallic
    • C04B2237/401—Cermets
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
    • C22C2026/003—Cubic boron nitrides only
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
    • Y10T428/24942—Structurally defined web or sheet [e.g., overall dimension, etc.] including components having same physical characteristic in differing degree
    • Y10T428/2495—Thickness [relative or absolute]
    • Y10T428/24967—Absolute thicknesses specified
    • Y10T428/24975—No layer or component greater than 5 mils thick
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
    • Y10T428/263—Coating layer not in excess of 5 mils thick or equivalent
    • Y10T428/264—Up to 3 mils
    • Y10T428/265—1 mil or less

Definitions

  • the present invention relates to a coated cBN sintered body.
  • cBN cubic boron nitride sintered body
  • the binder phase being continuous in two dimensions, , Periodic Table 4a, 5a, Group 6a transition metal carbide, nitride, carbonitride, boride, Al nitride, boride, oxide, Fe, Co, Ni at least one carbide, nitride 1 or more selected from the group consisting of carbon nitride, boride, and their mutual solid solution
  • the cBN content is 45-70% by volume
  • the average particle size of cBN particles is 0.01 or more
  • cBN sintered body characterized in that it is less than 2.0 ⁇ m, the average value of the binder phase thickness is 1.0 ⁇ m or less, and its standard deviation is 0.7 or less (see Patent Document 1).
  • a cubic boron nitride (cBN) sintered compact for a tool, wherein (a) about 60 to 80% by volume of cBN having a volume average particle size of about 3 to 6 ⁇ m, (b) a ceramic binder phase, i) about 20-60% by volume of one or more of a Group IVB or Group VIB metal carbide, nitride or boride; and (ii) about 40-80% by volume of aluminum carbide, nitride, boron
  • a sintered cBN compact comprising about 40 to 20% by volume of a ceramic binder phase that is one or more of a chemical compound or an oxide, and (c) about 3 to 15% by weight of tungsten (see Patent Document 2).
  • the present invention has been made in order to solve the above problems, and is a coated cBN sintered body that is excellent in wear resistance, fracture resistance, adhesion between a coating and a substrate, and can extend the tool life as compared with the prior art. The purpose is to provide.
  • the coated cBN sintered body of the present invention comprises a base material of the cBN sintered body and a coating coated on the surface thereof.
  • the cBN sintered body has a cBN of 76 to 90% by volume, a binder phase and inevitable.
  • Impurities 10 to 24% by volume, the average particle size of cBN is 0.5 to 5.0 ⁇ m, the average thickness of the binder phase is 0.05 to 0.8 ⁇ m, The standard deviation of the thickness is 0.8 ⁇ m or less, more preferably the thermal conductivity is 60 W / (m ⁇ K) or more, and more preferably the amount of tungsten element contained in the cBN sintered body is cBN sintering. It is 0 to 8% by mass based on the whole body.
  • the coated cBN sintered body of the present invention is excellent in wear resistance, chipping resistance, and adhesion between the substrate and the coating, and has an effect that the tool life can be extended as compared with the prior art.
  • cBN sintered body of the present invention when cBN exceeds 90% by volume and the binder phase and unavoidable impurities are less than 10% by volume, the adhesion between the substrate and the coating is deteriorated and the wear resistance is reduced.
  • cBN when cBN is less than 76% by volume and the binder phase and inevitable impurities are more than 24% by volume, the proportion of the binder phase with relatively low strength increases, and the resistance to fracture is reduced due to the decrease in thermal conductivity. Both wear resistance and wear resistance are reduced. Therefore, cBN: 76 to 90% by volume, binder phase and inevitable impurities: 10 to 24% by volume.
  • cBN 77 to 85% by volume, bonded phase and inevitable impurities: 15 to 23% by volume is more preferable, and among them, cBN: 77 to 83% by volume, bonded phase and inevitable impurities: 17 to 23% by volume are further added. preferable.
  • the content of the cBN, the binder phase, and the inevitable impurities is determined by taking a cross-sectional structure of the cBN sintered body with a SEM (scanning electron microscope) and analyzing the cross-sectional structure photograph taken at a magnification of 1000 to 5000 times. Can be sought.
  • the average particle size of the cBN of the present invention is less than 0.5 ⁇ m, the surface area of the binder phase surrounding each cBN particle becomes small, so that it becomes difficult to hold cBN during cutting, and the heat conduction of the sintered body The rate decreases, the crack growth cannot be suppressed, and the wear resistance and fracture resistance tend to decrease.
  • the average particle diameter of cBN is larger than 5.0 ⁇ m, the binder phase becomes thick, so that the strength is lowered and the fracture resistance tends to be lowered. Therefore, the average particle size of cBN is set to 0.5 to 5.0 ⁇ m.
  • the average particle size of cBN is preferably 0.7 to 4.0 ⁇ m, and more preferably 1.5 to 4.0 ⁇ m.
  • the average particle size of the cBN of the present invention is determined by counting the number of cBN contained per unit length and within a unit area from a photograph taken by enlarging the cross-sectional structure of the cBN sintered body 1000 to 5000 times with SEM. It can be obtained using Fullman's formula (Formula 1).
  • (Formula 1) dm (4 / ⁇ ) ⁇ (NL / NS)
  • dm is the average particle diameter
  • ⁇ is the circularity ratio
  • NL is the number of cBN hit by an arbitrary straight line on the cross-sectional structure
  • NS is the number of cBN included in an arbitrary unit area. .
  • the binder phase of the cBN sintered body of the present invention is Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Co, Ni, Al metals, carbides of these metals, carbonitrides, nitrides, It consists of at least one selected from boronitrides, borides, oxides, and their mutual solid solutions.
  • the tool life in cutting of hardened steel is improved. Since it improves, it is further more preferable.
  • the average value of the binder phase thickness of the cBN sintered body of the present invention is less than 0.05 ⁇ m, the adhesion between the substrate and the coating is deteriorated and the wear resistance is lowered, and the average value of the binder phase thickness is reduced.
  • the thickness exceeds 0.8 ⁇ m the fracture resistance deteriorates, so the average value of the thickness of the binder phase was set to 0.05 to 0.8 ⁇ m.
  • the average thickness of the binder phase is more preferably 0.1 to 0.5 ⁇ m.
  • the standard deviation of the thickness of the binder phase in the cBN sintered body of the present invention is obtained using the following (Equation 2).
  • (Formula 2) In the formula 2, the standard deviation of the thickness of the ⁇ binding phase, D i is the measured value of the thickness of the bonding phase, D is the average value of the thickness of the bonding phase, n represents a number of measurements.).
  • the standard deviation of the thickness of the binder phase exceeds 0.8 ⁇ m, the adhesion between the substrate and the coating and the fracture resistance are reduced, so the thickness is set to 0.8 ⁇ m or less.
  • a more preferable standard deviation of the thickness of the binder phase is 0.6 ⁇ m or less.
  • the standard deviation of the thickness of the binder phase is preferably in the range of 0.05 to 0.8 ⁇ m. A range of 0.05 to 0.6 ⁇ m is more preferable.
  • the average value and standard deviation of the thickness of the binder phase are as follows. The cross-sectional structure of the cBN sintered body is magnified 3000 to 5000 times with a SEM and photographed, and the resulting cross-sectional structure photograph of 3000 to 5000 times is arbitrarily linear. For the binder phase on the straight line, the length of the straight line intersecting the binder phase is measured as the thickness of the binder phase, and the average value and standard deviation are calculated.
  • the larger the number of measurement of the thickness of the binder phase the higher the reliability of the average value and the standard deviation, which is preferable.
  • a WC-based cemented carbide ball is used in the process of mixing raw material powders. It is preferable to perform ball mill mixing. However, when a WC-based cemented carbide ball is used, tungsten element is mixed into the cBN sintered body.
  • the tungsten element mixed in the cBN sintered body exists in the form of WC, WB, W 2 B, CoWB, W 2 Co 21 B 6 , Co 3 W 3 C, W, or the like.
  • the amount of tungsten element contained in the cBN sintered body of the present invention is preferably 0 to 8% by mass, of which 0 to 5% by mass Of these, 0 to 3% by mass is more preferable.
  • the tungsten element amount of the cBN sintered body of the present invention can be measured using EDS (energy dispersive X-ray analyzer) or ICP-AES (inductively coupled plasma emission spectrometer).
  • the cBN sintered body of the present invention Fe mixed in from the manufacturing process of the cBN sintered body can be mentioned.
  • the total of inevitable impurities is 1.0% by mass or less with respect to the entire cBN sintered body, and usually can be suppressed to 0.5% by mass or less with respect to the entire cBN sintered body. It does not affect the value.
  • in this invention in the range which does not impair the characteristic of the cBN sintered compact of this invention, in addition to cBN, a binder phase, and an unavoidable impurity, it contains a small amount of other components that cannot be said to be an unavoidable impurity. Also good.
  • the thermal conductivity of the cBN sintered body of the present invention is less than 60 W / (m ⁇ K), wear due to a chemical reaction occurs due to temperature rise, and the wear resistance tends to decrease. Therefore, the thermal conductivity of the cBN sintered body Is preferably 60 W / (m ⁇ K) or more.
  • the thermal conductivity of the cBN sintered body of the present invention is preferably as high as possible, and more preferably 75 W / (m ⁇ K) or more. Since the thermal conductivity of the cBN sintered body of the present invention does not exceed 160 W / (m ⁇ K), the thermal conductivity is preferably in the range of 60 to 160 W / (m ⁇ K).
  • the thermal conductivity of the cBN sintered body of the present invention can be measured by a laser flash method or the like.
  • the coated cBN sintered body obtained by coating the surface of the cBN sintered body base material of the present invention with a coating is preferable because the wear resistance, lubricity and oxidation resistance are improved.
  • the coating is made of Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Al, Si metals, oxides, carbides, carbonitrides, nitrides, borides, and mutual solid solutions of these metals.
  • the coating may be composed of either a single layer or a laminate of two or more layers, and at least one layer of the coating is also preferably an alternately laminated film in which thin films having different layer thicknesses of 5 to 200 nm are alternately laminated.
  • the total film thickness of the entire coating film is preferably 0.3 to 15 ⁇ m because the average film thickness is less than 0.3 ⁇ m, and the wear resistance is lowered, and if it exceeds 15 ⁇ m, the chipping resistance is lowered. Of these, 0.5 to 5 ⁇ m is more preferable.
  • the film can be coated by conventional PVD method and CVD method.
  • the coated cBN sintered body of the present invention is excellent in wear resistance, fracture resistance, and adhesion between the substrate and the coating.
  • the coated cBN sintered body of the present invention is preferably used as a coated cBN sintered body for a cutting tool because it can extend the tool life as compared with the conventional one when used as a cutting tool, and among them, the coated cBN sintered body for a hardened steel cutting tool. More preferably, it is used as a body.
  • the coated cBN sintered body of the present invention can be produced, for example, by the following method.
  • a coarse cBN powder having an average particle size of more than 2.0 ⁇ m and 7.0 ⁇ m or less and a fine cBN powder having an average particle size of 0.5 ⁇ m or more and 2.0 ⁇ m or less, and the coarse cBN powder by the volume ratio: the fine cBN powder (9.5 to 7): (0.5 to 3) (however, the total of the coarse cBN powder and the fine cBN powder is 10).
  • the thickness of the binder phase of the cBN sintered body can be reduced, and the thermal conductivity of the cBN sintered body can be increased.
  • a binder phase forming powder other than the cBN powder is mixed using a wet ball mill composed of a WC-based cemented carbide ball, an organic solvent, and a pot, and the organic solvent is evaporated to obtain a mixed powder.
  • the mixed powder is heat-treated at a temperature of 700 ° C. or higher and 1000 ° C. or lower to cause a brittle phase.
  • Step 4 The brittle phase is mixed and finely pulverized using a wet ball mill composed of a WC-based cemented carbide ball, an organic solvent, and a pot.
  • Step 5 The brittle phase powder obtained in Step 3 and the fine cBN powder having an average particle size of 0.5 ⁇ m or more and 2.0 ⁇ m or less are mixed, and the brittle phase and the fine cBN powder finely ground are mixed. Loosen and disperse them uniformly.
  • the mixing method include a wet ball mill with a mixing time of 1 to 24 hours, and ultrasonic mixing with a mixing time of 1 to 30 minutes.
  • Step 6 To the mixed powder obtained in Step 4, coarse cBN powder having an average particle size of more than 2.0 ⁇ m and 7.0 ⁇ m or less is added and mixed, and these are uniformly dispersed.
  • the mixing method include a wet ball mill with a mixing time of 2 to 6 hours, and ultrasonic mixing with a mixing time of 1 to 30 minutes.
  • Step 7 The mixed powder obtained in Step 5 is put into a metal capsule such as Ta, Nb, Mo, Zr, etc., and the metal capsule is loaded into an ultrahigh pressure and high temperature generator, and the pressure is 6 to 8 GPa and the temperature is 1200 to 1600 ° C.
  • the cBN sintered body of the present invention When sintered under conditions, the cBN sintered body of the present invention is obtained.
  • the coated cBN sintered body of the present invention can be obtained by coating the surface of the cBN sintered body of the present invention with a PVD method or a CVD method.
  • Co powder and WC powder having an average particle size of 2.0 ⁇ m were prepared and weighed so as to have the composition shown in Table 1.
  • the binder phase forming powder other than the cBN powder was mixed using a wet ball mill composed of a WC-based cemented carbide ball, an organic solvent, and a pot. The obtained mixed powder was heat-treated at 850 ° C. to make a brittle phase.
  • the resulting brittle phase was finely pulverized using a wet ball mill composed of WC-based cemented carbide balls, an organic solvent, and a pot.
  • Fine cBN powder having an average particle diameter of 1.0 ⁇ m was added to the finely pulverized brittle phase powder, and mixed for 1 hour using a wet ball mill composed of a WC-based cemented carbide ball, an organic solvent, and a pot.
  • a coarse cBN powder having an average particle size of 3.2 ⁇ m was further added to this mixture, and mixed for 6 hours using a wet ball mill composed of a WC-based cemented carbide ball, an organic solvent, and a pot.
  • the obtained mixed powder is put into a Ta capsule, and the Ta capsule is loaded into an ultra-high pressure and high temperature generator and sintered at the sintering temperature and sintering pressure shown in Table 2 to produce the cBN sintered body of the invention and the comparative product. Obtained.
  • the obtained cBN sintered body was subjected to X-ray diffraction measurement to qualitatively analyze the composition of the cBN sintered body.
  • the cross-sectional structure of the cBN sintered body was photographed with a SEM at a magnification of 3000 to 5000 times.
  • tissue photograph was calculated
  • a straight line was arbitrarily drawn on the cross-sectional structure photograph, and for the binder phase on the straight line, the length of the straight line intersecting the binder phase was measured as the thickness of the binder phase, and the average value and standard deviation were obtained. .
  • the number of measured thicknesses of the binder phase was 600 per sample. Further, the average length of cBN was determined by counting the unit length and the number of cBN per unit area from a photograph taken by magnifying the cross-sectional structure 1000 to 5000 times with SEM and using the Fullman formula.
  • the amount of tungsten element contained in the cBN sintered body was measured using EDS.
  • the thermal conductivity of the cBN sintered body was measured by a laser flash method.
  • the cBN sintered bodies of sample numbers 1 to 6 and 8 are cut into a predetermined shape by a wire electric discharge machine, and the cBN sintered body of sample number 7 is cut into a predetermined shape by a laser cutting machine.
  • the cutting tool having an ISO standard CNGA120408 cutting insert shape was obtained by grinding and finishing. This cutting tool was coated with a TiCN film having an average film thickness of 1.0 ⁇ m by the PVD method to obtain a cutting tool of a coated cBN sintered body.
  • Table 5 shows the tool life of the inventive product and the comparative product.
  • Table 5 shows that the inventive product has a longer tool life than the comparative product.
  • the amount of cBN exceeds 80% by volume, the proportion of the binder phase decreases, the adhesion between the substrate and the coating decreases, and the tool life starts to decrease due to the increase in the amount of tungsten element. If the amount of cBN is less than 75% by volume, the thermal conductivity is lowered, and the average value and standard deviation of the thickness of the binder phase is increased, so that the tool life is reduced.
  • Fine cBN powder with an average particle size of 1.0 ⁇ m, coarse cBN powder with an average particle size of 3.2 ⁇ m, TiN powder with an average particle size of 1.5 ⁇ m, TiC powder with an average particle size of 1.2 ⁇ m, an average particle size of 1.2 ⁇ m TiCN powder and Al powder having an average particle diameter of 3.1 ⁇ m were prepared and weighed so as to have the composition shown in Table 6.
  • the binder phase forming powder other than the cBN powder was mixed using a wet ball mill composed of a WC-based cemented carbide ball, an organic solvent, and a pot.
  • the obtained mixed powder was heat-treated at 850 ° C. to make a brittle phase.
  • the resulting brittle phase was finely pulverized using a wet ball mill composed of WC-based cemented carbide balls, an organic solvent, and a pot.
  • a fine cBN powder having an average particle diameter of 1.0 ⁇ m is added to finely pulverized brittle phase powder, and a WC-based cemented carbide ball, an organic solvent, and a pot are included.
  • a coarse ball cBN powder having an average particle diameter of 3.2 ⁇ m was further added to the obtained mixture, and a wet ball mill composed of a WC-based cemented carbide ball, an organic solvent, and a pot was added. And mixed by the mixing method shown in Table 8.
  • coarse cBN powder having an average particle size of 3.2 ⁇ m was further added to the obtained mixture, and ultrasonic mixing shown in Table 8 was performed.
  • the obtained mixed powder was put into a Ta capsule, and the Ta capsule was loaded into an ultrahigh pressure and high temperature generator, and sintered at a sintering pressure of 7.4 GPa and a sintering temperature of 1450 ° C. to obtain a cBN sintered body.
  • a sintering pressure of 7.4 GPa and a sintering temperature of 1450 ° C. was measured in the same manner as in Example 1. .
  • the amount of tungsten element contained in the cBN sintered body was measured using EDS.
  • the thermal conductivity of the cBN sintered body was measured by a laser flash method. The results are shown in Table 10.
  • the cBN sintered body was cut into a predetermined shape with a wire electric discharge machine, brazed to a CNGA-shaped carbide substrate, and ground and finished to obtain a cutting tool having an ISO standard CNGA120408 cutting insert shape.
  • This cutting tool was coated with a (Al, Cr) N film having an average film thickness of 1.3 ⁇ m by the PVD method to obtain a cutting tool made of a coated cBN sintered body. The following cutting test was performed using the obtained cutting tool.
  • Fine cBN powder with an average particle size of 0.4 to 1.0 ⁇ m, coarse cBN powder with an average particle size of 3.2 to 5.7 ⁇ m, TiN powder with an average particle size of 1.5 ⁇ m, and Al powder with an average particle size of 3.1 ⁇ m Were prepared and weighed so as to have the composition shown in Table 11.
  • the binder phase forming powder other than the cBN powder was mixed using a wet ball mill composed of a WC-based cemented carbide ball, an organic solvent, and a pot.
  • the obtained mixed powder was heat-treated at 850 ° C. to make a brittle phase.
  • the resulting brittle phase was finely pulverized using a wet ball mill composed of WC-based cemented carbide balls, an organic solvent, and a pot.
  • Sample No. 22 was prepared by adding a coarse cBN powder having an average particle size of 5.7 ⁇ m shown in Table 11 to a finely pulverized brittle phase powder, and a wet ball mill comprising a WC-based cemented carbide ball, an organic solvent, and a pot. And mixed for 6 hours.
  • the obtained mixed powder was put into a Ta capsule, and the Ta capsule was loaded into an ultrahigh pressure and high temperature generator, and sintered at a sintering temperature and a sintering pressure shown in Table 12 to obtain a cBN sintered body.
  • binder phase forming powders other than cBN powder were mixed using a wet ball mill composed of WC-based cemented carbide balls, an organic solvent, and a pot.
  • the obtained mixed powder was heat-treated at 850 ° C. to make a brittle phase.
  • the resulting brittle phase was finely pulverized using a wet ball mill composed of WC-based cemented carbide balls, an organic solvent, and a pot.
  • Add fine cBN powder with an average particle size of 1.0 ⁇ m shown in Table 11 to the finely crushed brittle phase powder and mix for 1 hour using a wet ball mill consisting of WC-based cemented carbide balls, organic solvent and pot did.
  • a coarse cBN powder having an average particle size of 2.4 to 5.7 ⁇ m was further added to this mixture, and mixed for 6 hours using a wet ball mill composed of a WC-based cemented carbide ball, an organic solvent, and a pot.
  • the obtained mixed powder was put into a Ta capsule, and the Ta capsule was loaded into an ultrahigh pressure and high temperature generator, and sintered at a sintering temperature and a sintering pressure shown in Table 12 to obtain a cBN sintered body.
  • the amount of tungsten element contained in the cBN sintered body was measured using EDS. Further, the thermal conductivity of the cBN sintered body was measured by a laser flash method. The results are shown in Table 14.
  • the cBN sintered body was cut into a predetermined shape with a wire electric discharge machine, brazed to a CNGA-shaped carbide substrate, and ground and finished to obtain a cutting tool having an ISO standard CNGA120408 cutting insert shape.
  • the cutting tool is coated with a film composed of alternately laminated films in which thin layers made of (Ti, Si) N having a thickness of 20 nm and thin layers made of (Al, Cr) N having a thickness of 20 nm are alternately laminated by the PVD method. Then, the coating film was coated so that the total film thickness was 1.8 ⁇ m in average film thickness, and a cutting tool made of a coated cBN sintered body was obtained. The following cutting test was performed using the obtained cutting tool. The tool life of the cutting tool is shown in Table 15.
  • Table 15 shows that sample No. 16 has low wear resistance and chipping resistance. This is presumably because cBN is fine and has low thermal conductivity and cracks are likely to propagate. Table 15 also shows that Sample No. 22 has low wear resistance and chipping resistance. This is thought to be because the binder phase is selectively worn because cBN is coarse and the average value and standard deviation of the binder phase thickness are large.

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Abstract

　耐摩耗性、耐欠損性、基材と被膜との密着性に優れ、従来よりも工具寿命を延長 できる被覆ｃＢＮ焼結体の提供を目的にする。　ｃＢＮ焼結体の基材とその表面に被覆された被膜とからなり、ｃＢＮ焼結体は、ｃＢＮ：７６～９０体積％と、結合相および不可避的不純物：１０～２４体積％とからなり、ｃＢＮの平均粒径は０．５～５．０μｍであり、結合相の厚さの平均値が０．０５～０．８μｍであり、結合相の厚さの標準偏差が０．８μｍ以下である被覆ｃＢＮ焼結体。

Description

被覆ｃＢＮ焼結体
　本発明は被覆ｃＢＮ焼結体に関する。
　立方晶窒化硼素焼結体（ｃＢＮ）の従来技術として、ｃＢＮ粒子を結合相で焼結した焼結体であって、前記結合相が二次元的に見て連続しており、この結合相は、周期律表４ａ，５ａ，６ａ族遷移金属の炭化物、窒化物、炭窒化物、硼化物、Ａｌの窒化物、硼化物、酸化物、Ｆｅ、Ｃｏ、Ｎｉの少なくとも１種の炭化物、窒化物、炭窒化物、硼化物、およびこれらの相互固溶体よりなる群から選択される１種以上を含み、ｃＢＮの含有率が体積％で４５－７０％で、ｃＢＮ粒子の平均粒度が０．０１以上２．０μｍ未満であり、結合相厚みの平均値が１．０μｍ以下で、その標準偏差が０．７以下であることを特徴とするｃＢＮ焼結体がある（特許文献１参照。）。
　また、工具用の立方晶窒化ホウ素（ｃＢＮ）焼結成形体であって、（ａ）体積平均粒度約３～６μｍのｃＢＮ約６０～８０体積％、（ｂ）セラミック結合剤相であって、（ｉ）その約２０～６０体積％が第ＩＶＢ族又は第ＶＩＢ族金属の炭化物、窒化物又はホウ化物の１種以上で（ｉｉ）その約４０～８０体積％がアルミニウムの炭化物、窒化物、ホウ化物又は酸化物の１種以上であるセラミック結合剤相約４０～２０体積％、及び（ｃ）タングステン約３～１５重量％を含んでなる焼結ｃＢＮ成形体がある（特許文献２参照。）。
特開２００８－２０８０２７号公報 特開２００４－１６０６３７号公報
　近年、切削加工において、被削材の難削性が増す一方で加工の高能率化が求められている。上記特許文献１の発明や上記特許文献２の発明を切削工具として用いたとき、耐欠損性が低く、これらの要求に十分に答えられないという問題があった。本発明は、上記問題を解決するためになされたものであり、耐摩耗性、耐欠損性、被膜と基材との密着性に優れ、従来よりも工具寿命を延長できる被覆ｃＢＮ焼結体を提供することを目的とする。
　本発明者等が研究を重ねたところ、ｃＢＮ（立方晶窒化硼素）の含有量を高くし、結合相の厚さのバラツキを小さくしたｃＢＮ焼結体の基材に被膜を被覆すると、耐摩耗性および耐欠損性が共に向上するという知見を得た。すなわち、本発明の被覆ｃＢＮ焼結体は、ｃＢＮ焼結体の基材とその表面に被覆された被膜とからなり、ｃＢＮ焼結体は、ｃＢＮ：７６～９０体積％と、結合相および不可避的不純物：１０～２４体積％とからなり、ｃＢＮの平均粒径は０．５～５．０μｍであり、結合相の厚さの平均値が０．０５～０．８μｍであり、結合相の厚さの標準偏差が０．８μｍ以下であり、より好ましくは、熱伝導率が６０Ｗ／（ｍ・Ｋ）以上であり、より好ましくは、ｃＢＮ焼結体に含まれるタングステン元素量がｃＢＮ焼結体全体に対して０～８質量％であるものである。
　本発明の被覆ｃＢＮ焼結体は、耐摩耗性、耐欠損性、基材と被膜との密着性に優れ、従来よりも工具寿命を延長できるという効果を奏する。
　本発明のｃＢＮ焼結体において、ｃＢＮが９０体積％を超えて多くなり、結合相および不可避的不純物が１０体積％未満になると、基材と被膜との密着性が悪くなり耐摩耗性が低下し、逆にｃＢＮが７６体積％未満になり、結合相および不可避的不純物が２４体積％を超えて多くなると、相対的に強度の低い結合相の割合が増え、熱伝導率の低下により耐欠損性および耐摩耗性が共に低下する。そのため、ｃＢＮ：７６～９０体積％、結合相および不可避的不純物：１０～２４体積％とした。その中でもｃＢＮ：７７～８５体積％、結合相および不可避的不純物：１５～２３体積％がより好ましく、その中でもｃＢＮ：７７～８３体積％、結合相および不可避的不純物：１７～２３体積％がさらに好ましい。ｃＢＮと、結合相および不可避的不純物の含有量は、ｃＢＮ焼結体の断面組織をＳＥＭ（走査電子顕微鏡）で撮影し、１０００～５０００倍で撮影された断面組織写真を画像解析することで、求めることができる。
　本発明のｃＢＮの平均粒径は、０．５μｍ未満であると個々のｃＢＮ粒子を囲む結合相の表面積が小さくなるため、切削中にｃＢＮを保持することが難しくなり、焼結体の熱伝導率が低下し、亀裂の進展を抑制することができなくなり耐摩耗性と耐欠損性が低下する傾向が見られる。ｃＢＮの平均粒径は、５．０μｍを超えて大きくなると結合相が厚くなるため強度が低下し耐欠損性が低下する傾向が見られる。そのため、ｃＢＮの平均粒径は０．５～５．０μｍとした。その中でもｃＢＮの平均粒径は０．７～４．０μｍであると好ましく、その中でも１．５～４．０μｍであるとさらに好ましい。本発明のｃＢＮの平均粒径は、ｃＢＮ焼結体の断面組織をＳＥＭで１０００～５０００倍に拡大して撮影した写真から、単位長さあたり及び単位面積内に含まれるｃＢＮ数をカウントし、フルマンの式（式１）を用いて求めることができる。
（式１）
　ｄｍ＝（４／π）×（ＮＬ／ＮＳ）
（式１中、ｄｍは平均粒径、πは円周率、ＮＬは断面組織上の任意の直線によってヒットする単位長さあたりのｃＢＮ数、ＮＳは任意の単位面積内に含まれるｃＢＮの数である。）。
　本発明のｃＢＮ焼結体の結合相は、Ｔｉ、Ｚｒ、Ｈｆ、Ｖ、Ｎｂ、Ｔａ、Ｃｒ、Ｍｏ、Ｗ、Ｃｏ、Ｎｉ、Ａｌの金属、これら金属の炭化物、炭窒化物、窒化物、硼窒化物、硼化物、酸化物およびこれらの相互固溶体の中から選ばれた少なくとも１種からなる。具体的には、ＴｉＮ、ＴｉＣＮ、ＴｉＣ、ＴｉＢ2、ＴｉＢＮ、ＴｉＡｌＮ、Ｔｉ2ＡｌＮ、ＡｌＮ、ＡｌＢ2、Ａｌ2Ｏ3、ＺｒＣ、ＨｆＣ、ＶＣ、ＮｂＣ、ＴａＣ、Ｃｒ3Ｃ2、Ｍｏ2Ｃ、ＺｒＮ、ＨｆＮ、ＶＮ、ＮｂＮ、ＴａＮ、ＣｒＮ、ＷＣ、ＷＢ、Ｗ2Ｂ、ＣｏＷＢ、Ｗ2Ｃｏ21Ｂ6、Ｃｏ3Ｗ3Ｃ、Ｗ、Ｃｏ、Ｎｉなどを挙げることができる。その中でも焼入鋼の切削加工においては、ＴｉＮ、ＴｉＣＮ、ＴｉＣ、ＡｌＮ、ＡｌＢ2、Ａｌ2Ｏ3、ＴｉＢ2、ＣｏＷＢ、Ｗ2Ｃｏ21Ｂ6、ＷＣの中の少なくとも１種であると、工具寿命が向上するので、さらに好ましく、その中でもＴｉＮ、ＴｉＣＮ、ＴｉＣ、ＡｌＮ、ＡｌＢ2、Ａｌ2Ｏ3、ＴｉＢ2の中の少なくとも１種であると、焼入鋼の切削加工における工具寿命が向上するので、さらに好ましい。
　本発明のｃＢＮ焼結体の結合相の厚さの平均値が０．０５μｍ未満になると、基材と被膜との密着性が悪くなり耐摩耗性が低下し、結合相の厚さの平均値が０．８μｍを超えて大きくなると耐欠損性が低下してしまうことから、結合相の厚さの平均値は０．０５～０．８μｍとした。その中でも結合相の厚さの平均値が０．１～０．５μｍであるとさらに好ましい。
　本発明のｃＢＮ焼結体における結合相の厚さの標準偏差は次の（式２）を用いて求められる。
（式２）
Figure JPOXMLDOC01-appb-I000001
（式２中、σは結合相の厚さの標準偏差、Ｄｉは結合相の厚さの測定値、Ｄは結合相の厚さの平均値、ｎは測定数である。）。
結合相の厚さの標準偏差は０．８μｍを超えると基材と被膜との密着性や耐欠損性が低下するので、０．８μｍ以下とした。さらに好ましい結合相の厚さの標準偏差は０．６μｍ以下である。なお、結合相の厚さの標準偏差を０．０５μｍ未満にすることは製造上難しいので、現実的には、結合相の厚さの標準偏差は０．０５～０．８μｍの範囲が好ましく、０．０５～０．６μｍの範囲がさらに好ましい。結合相の厚さの平均値と標準偏差は、ｃＢＮ焼結体の断面組織をＳＥＭで３０００～５０００倍に拡大して写真撮影し、得られた３０００～５０００倍の断面組織写真に任意に直線を引き、その直線上にある結合相について、結合相と交差する直線の長さを結合相の厚さとして測定して、その平均値と標準偏差を計算する。このとき、画像解析を行って、結合相の厚さを測定しても好ましい。また、結合相の厚さの測定数は多いほど平均値と標準偏差の信頼性が増すので好ましく、具体的には、例えば、１断面あたり２００以上の測定数で少なくとも３断面を測定した６００以上の測定数であると好ましい。
　本発明のｃＢＮ焼結体の製造方法において、本発明で規定される結合相の厚さの平均値と標準偏差を実現するために、原料粉末を混合する工程ではＷＣ基超硬合金ボールを使用したボールミル混合を行うと好ましい。しかしながら、ＷＣ基超硬合金ボールを使用するとタングステン元素がｃＢＮ焼結体に混入する。ｃＢＮ焼結体に混入したタングステン元素はＷＣ、ＷＢ、Ｗ2Ｂ、ＣｏＷＢ、Ｗ2Ｃｏ21Ｂ6、Ｃｏ3Ｗ3Ｃ、Ｗなどの形で存在する。これらのＷの金属およびタングステン化合物は切削時の欠損や亀裂の起点となりやすいので、本発明のｃＢＮ焼結体に含まれるタングステン元素量は０～８質量％が好ましく、その中でも０～５質量％がさらに好ましく、その中でも０～３質量％がさらに好ましい。なお、本発明のｃＢＮ焼結体のタングステン元素量はＥＤＳ（エネルギー分散型Ｘ線分析装置）またはＩＣＰ－ＡＥＳ（誘導結合プラズマ発光分光分析装置）などを用いて測定することができる。
　本発明のｃＢＮ焼結体の不可避的不純物としては、ｃＢＮ焼結体の製造工程から混入されるＦｅを挙げることができる。不可避的不純物の合計はｃＢＮ焼結体全体に対して１．０質量％以下であり、通常はｃＢＮ焼結体全体に対して０．５質量％以下に抑えることができるので、本発明の特性値に影響を及ぼすことはない。なお、本発明においては、本発明のｃＢＮ焼結体の特性を損わない範囲で、ｃＢＮと結合相と不可避的不純物に他に、不可避的不純物とはいえない他の成分を少量含有してもよい。
　本発明のｃＢＮ焼結体の熱伝導率が６０Ｗ／（ｍ・Ｋ）未満になると温度上昇により化学反応による摩耗が生じ耐摩耗性が低下する傾向を示すので、ｃＢＮ焼結体の熱伝導率は６０Ｗ／（ｍ・Ｋ）以上が好ましい。本発明のｃＢＮ焼結体の熱伝導率は高いほど好ましく、７５Ｗ／（ｍ・Ｋ）以上であるとさらに好ましい。なお、本発明のｃＢＮ焼結体の熱伝導率が１６０Ｗ／（ｍ・Ｋ）を超えて高くなることはないので、熱伝導率は６０～１６０Ｗ／（ｍ・Ｋ）の範囲が好ましい。本発明のｃＢＮ焼結体の熱伝導率はレーザーフラッシュ法などにより測定することができる。
　本発明のｃＢＮ焼結体基材の表面に被膜を被覆した被覆ｃＢＮ焼結体は耐摩耗性、潤滑性、耐酸化性が向上するため、好ましい。被膜はＴｉ、Ｚｒ、Ｈｆ、Ｖ、Ｎｂ、Ｔａ、Ｃｒ、Ｍｏ、Ｗ、Ａｌ、Ｓｉの金属、これら金属の酸化物、炭化物、炭窒化物、窒化物、硼化物およびこれらの相互固溶体の中から選ばれた少なくとも１種からなる。具体的にはＴｉＣ、ＴｉＣＮ、ＴｉＮ、（Ｔｉ，Ａｌ）Ｎ、（Ｔｉ，Ｓｉ）Ｎ、（Ａｌ，Ｃｒ）Ｎ、（Ａｌ，Ｃｒ）ＮＯ、（Ｔｉ，Ａｌ，Ｃｒ）Ｎ、Ａｌ2Ｏ3、（Ａｌ，Ｃｒ）2Ｏ3などが挙げられる。被膜は単層または２層以上の積層のいずれで構成されても好ましく、被膜の少なくとも１層は、組成が異なる層厚５～２００ｎｍの薄膜を交互に積層した交互積層膜でも好ましい。被膜全体の総膜厚は、平均膜厚で、０．３μｍ未満であると耐摩耗性が低下し、１５μｍを超えると耐欠損性が低下することから、０．３～１５μｍであると好ましく、その中でも０．５～５μｍであるとさらに好ましい。なお、被膜は従来からあるＰＶＤ法、ＣＶＤ法によって被覆できる。
　本発明の被覆ｃＢＮ焼結体は、耐摩耗性、耐欠損性、基材と被膜との密着性に優れる。本発明の被覆ｃＢＮ焼結体は、切削工具として用いると従来よりも工具寿命を延長できることから、切削工具用被覆ｃＢＮ焼結体として用いると好ましく、その中でも焼入鋼切削工具用被覆ｃＢＮ焼結体として用いるとさらに好ましい。
　本発明の被覆ｃＢＮ焼結体は、例えば、以下の方法で製造することができる。
［工程１］平均粒径２．０μｍ超７．０μｍ以下の粗粒ｃＢＮ粉末と、平均粒径０．５μｍ以上２．０μｍ以下の微粒ｃＢＮ粉末と、Ｔｉ、Ｚｒ、Ｈｆ、Ｖ、Ｎｂ、Ｔａ、Ｃｒ、Ｍｏ、Ｗ、Ｃｏ、Ｎｉ、Ａｌの金属、これらの金属の炭化物、炭窒化物、窒化物、硼化物、酸化物およびこれらの相互固溶体の中から選ばれた少なくとも１種からなる結合相形成用粉末を用意し、粗粒ｃＢＮ粉末と微粒ｃＢＮ粉末の割合は体積比で粗粒ｃＢＮ粉末：微粒ｃＢＮ粉末＝（９．５～７）：（０．５～３）（但し、粗粒ｃＢＮ粉末と微粒ｃＢＮ粉末の合計は１０とする。）の範囲内で、粗粒ｃＢＮ粉末は５６～７６体積％、微粒ｃＢＮ粉末は４～２４体積％、結合相形成用粉末は１０～２４体積％、これらの合計は１００体積％となるように粗粒ｃＢＮ粉末と微粒ｃＢＮ粉末と結合相形成用粉末を秤量する。上記のように平均粒径２．０μｍ超７．０μｍ以下の粗粒ｃＢＮ粉末と平均粒径０．５μｍ以上２．０μｍ以下の微粒ｃＢＮ粉末を、体積比で粗粒ｃＢＮ粉末：微粒ｃＢＮ粉末＝（９．５～７）：（０．５～３）（但し、粗粒ｃＢＮ粉末と微粒ｃＢＮ粉末の合計は１０とする。）の範囲内にすることにより、ｃＢＮの平均粒径を０．５～５．０μｍの範囲内にするとともに、ｃＢＮ焼結体の結合相の厚さを薄くし、ｃＢＮ焼結体の熱伝導率を高くすることができる。
［工程２］ｃＢＮ粉末以外の結合相形成用粉末を、ＷＣ基超硬合金ボールと有機溶媒とポットとからなる湿式ボールミルを用いて混合し、有機溶媒を蒸発させ、混合粉末を得る。
［工程３］混合粉末を７００℃以上１０００℃以下の温度で熱処理して反応させて脆性のある相にする。
［工程４］脆性のある相をＷＣ基超硬合金ボールと有機溶媒とポットとからなる湿式ボールミルを用いて混合し、細かく粉砕する。
［工程５］工程３で得られた脆性のある相の粉末と平均粒径０．５μｍ以上２．０μｍ以下の微粒ｃＢＮ粉末とを混合し、細かく粉砕した脆性のある相と微粒ｃＢＮ粉末とをほぐして、これらを均一に分散させる。混合する方法としては、混合時間１～２４時間の湿式ボールミル、混合時間１～３０分間の超音波混合などを挙げることができる。
［工程６］工程４で得られた混合粉末に、平均粒径２．０μｍ超７．０μｍ以下の粗粒ｃＢＮ粉末を加えて混合し、これらを均一に分散させる。混合する方法としては、混合時間２～６時間の湿式ボールミル、混合時間１～３０分間の超音波混合などを挙げることができる。
［工程７］工程５で得られた混合粉末をＴａ、Ｎｂ、Ｍｏ、Ｚｒなどの金属カプセルに入れ、金属カプセルを超高圧高温発生装置に装填し、圧力６～８ＧＰａ、温度１２００～１６００℃の条件下で焼結すると本発明のｃＢＮ焼結体が得られる。
［工程８］本発明のｃＢＮ焼結体の表面にＰＶＤ法、ＣＶＤ法によって被膜を被覆することで本発明の被覆ｃＢＮ焼結体が得られる。
　平均粒径１．０μｍの微粒ｃＢＮ粉末、平均粒径３．２μｍの粗粒ｃＢＮ粉末、平均粒径１．５μｍのＴｉＮ粉末、平均粒径３．１μｍのＡｌ粉末、平均粒径０．４μｍのＣｏ粉末、平均粒径２．０μｍのＷＣ粉末を用意し、表１に示す配合組成になるように秤量した。ｃＢＮ粉末以外の結合相形成用粉末をＷＣ基超硬合金ボールと有機溶媒とポットとからなる湿式ボールミルを用いて混合した。得られた混合粉末を８５０℃で熱処理して反応させ脆性のある相にした。得られた脆性のある相をＷＣ基超硬合金ボールと有機溶媒とポットとからなる湿式ボールミルを用いて細かく粉砕した。細かく粉砕した脆性のある相の粉末に平均粒径１．０μｍの微粒ｃＢＮ粉末を加えて、ＷＣ基超硬合金ボールと有機溶媒とポットとからなる湿式ボールミルを用いて１時間混合した。この混合物にさらに平均粒径３．２μｍの粗粒ｃＢＮ粉末を加えて、ＷＣ基超硬合金ボールと有機溶媒とポットとからなる湿式ボールミルを用いて６時間混合した。得られた混合粉末をＴａカプセルに入れ、Ｔａカプセルを超高圧高温発生装置に装填し、表２に示す焼結温度と焼結圧力で焼結して発明品と比較品のｃＢＮ焼結体を得た。
Figure JPOXMLDOC01-appb-T000002
Figure JPOXMLDOC01-appb-T000003
　得られたｃＢＮ焼結体についてＸ線回折測定を行って、ｃＢＮ焼結体の組成を定性分析した。次にｃＢＮ焼結体の断面組織をＳＥＭで３０００～５０００倍に拡大して撮影した。得られた断面組織写真を画像解析することでｃＢＮと結合相の含有量（体積％）を求めた。また、断面組織写真に任意に直線を引き、その直線上にある結合相について、結合相と交差する直線の長さを結合相の厚さとして測定して、その平均値と標準偏差を求めた。このとき結合相の厚さの測定数は１試料当たり６００箇所であった。さらに断面組織をＳＥＭで１０００～５０００倍に拡大して撮影した写真から単位長さ及び単位面積あたりのｃＢＮ数をカウントし、フルマンの式を用いることでｃＢＮの平均粒径を求めた。
Figure JPOXMLDOC01-appb-T000004
　ＥＤＳを用いてｃＢＮ焼結体に含まれるタングステン元素量を測定した。ｃＢＮ焼結体の熱伝導率はレーザーフラッシュ法により測定した。これらの結果は表４に示した。
Figure JPOXMLDOC01-appb-T000005
　試料番号１～６，８のｃＢＮ焼結体をワイヤ放電加工機で、試料番号７のｃＢＮ焼結体をレーザーカット加工機で、所定の形状にカットしてＣＮＧＡ形状の超硬基材にろう付けし、研削仕上げ加工をしてＩＳＯ規格ＣＮＧＡ１２０４０８切削インサート形状の切削工具を得た。この切削工具にＰＶＤ法により平均膜厚１．０μｍのＴｉＣＮ膜を被覆して被覆ｃＢＮ焼結体の切削工具を得た。
　発明品と比較品の切削工具を用いて以下の切削試験を行った。発明品と比較品の工具寿命は表５に示した。
［連続切削試験］
加工形態：旋削加工、
被削材：ＳＣＭ４１５Ｈ（形状：円柱状）、
切削速度：１３０ｍ／ｍｉｎ、
送り：０．１５ｍｍ／ｒｅｖ、
切り込み：０．１５ｍｍ、
雰囲気：湿式、
寿命判定：切削工具の逃げ面摩耗が０．１ｍｍを超えたときを工具寿命とした。
［断続切削試験］
加工形態：旋削加工、
被削材：ＳＣＭ４３５Ｈ（形状：円柱に２本のＶ溝を入れた略円柱状）、
切削速度：１３０ｍ／ｍｉｎ、
送り：０．１５ｍｍ／ｒｅｖ、
切り込み：０．１５ｍｍ、
雰囲気：湿式、
寿命判定：切削工具が欠損したときを工具寿命とした。
Figure JPOXMLDOC01-appb-T000006
　表５から発明品は比較品よりも工具寿命が長いことが分かる。ｃＢＮ量が８０体積％を超えて多くなると結合相の割合が少なくなり基材と被膜との密着性が低下し、タングステン元素量が増加することにより工具寿命が低下しはじめる。ｃＢＮ量が７５体積％未満であると熱伝導率が低下し、結合相の厚さの平均値と標準偏差が大きくなることで工具寿命が低下する。
　平均粒径１．０μｍの微粒ｃＢＮ粉末、平均粒径３．２μｍの粗粒ｃＢＮ粉末、平均粒径１．５μｍのＴｉＮ粉末、平均粒径１．２μｍのＴｉＣ粉末、平均粒径１．２μｍのＴｉＣＮ粉末、平均粒径３．１μｍのＡｌ粉末を用意し、表６に示す配合組成になるように秤量した。
Figure JPOXMLDOC01-appb-T000007
　ｃＢＮ粉末以外の結合相形成用粉末をＷＣ基超硬合金ボールと有機溶媒とポットとからなる湿式ボールミルを用いて混合した。得られた混合粉末を８５０℃で熱処理して反応させ脆性のある相にした。得られた脆性のある相をＷＣ基超硬合金ボールと有機溶媒とポットとからなる湿式ボールミルを用いて細かく粉砕した。試料番号９～１２、１４，１５については、細かく粉砕した脆性のある相の粉末に平均粒径１．０μｍの微粒ｃＢＮ粉末を加えて、ＷＣ基超硬合金ボールと有機溶媒とポットとからなる湿式ボールミルを用いて表７に示す混合方法で混合した。試料番号１３については、細かく粉砕した脆性のある相の粉末に平均粒径１．０μｍの微粒ｃＢＮ粉末を加えて、表７に示す超音波混合を行った。
Figure JPOXMLDOC01-appb-T000008
　試料番号９～１２、１４，１５については、得られた混合物にさらに平均粒径３．２μｍの粗粒ｃＢＮ粉末を加えて、ＷＣ基超硬合金ボールと有機溶媒とポットとからなる湿式ボールミルを用いて表８に示す混合方法で混合した。試料番号１３については、得られた混合物にさらに平均粒径３．２μｍの粗粒ｃＢＮ粉末を加えて、表８に示す超音波混合を行った。
Figure JPOXMLDOC01-appb-T000009
　得られた混合粉末をＴａカプセルに入れ、Ｔａカプセルを超高圧高温発生装置に装填し、焼結圧力７．４ＧＰａ、焼結温度１４５０℃で焼結して、ｃＢＮ焼結体を得た。得られたｃＢＮ焼結体について実施例１と同様な方法でｃＢＮ焼結体の組成、ｃＢＮ量と結合相量、ｃＢＮの平均粒径、結合相の厚さの平均値と標準偏差を測定した。これらの結果は表９に示した。
Figure JPOXMLDOC01-appb-T000010
　ＥＤＳを用いてｃＢＮ焼結体に含まれるタングステン元素量を測定した。ｃＢＮ焼結体の熱伝導率はレーザーフラッシュ法により測定した。その結果は表１０に示した。
Figure JPOXMLDOC01-appb-T000011
　ｃＢＮ焼結体をワイヤ放電加工機で所定の形状にカットしてＣＮＧＡ形状の超硬基材にろう付けし、研削仕上げ加工をしてＩＳＯ規格ＣＮＧＡ１２０４０８切削インサート形状の切削工具を得た。この切削工具にＰＶＤ法により平均膜厚１．３μｍの（Ａｌ，Ｃｒ）Ｎ膜を被覆し被覆ｃＢＮ焼結体からなる切削工具を得た。得られた切削工具を用いて以下の切削試験を行った。
［断続切削試験］
加工形態：旋削加工、
被削材：ＳＣＭ４３５Ｈ（形状：円柱に２本のＶ溝を入れた略円柱状）、
切削速度：１３０ｍ／ｍｉｎ、
送り：０．１５ｍｍ／ｒｅｖ、
切り込み：０．１５ｍｍ、
雰囲気：湿式、
寿命判定：切削工具が欠損したときを工具寿命とした。
　切削試験の結果は表１０に併記した。表１０から、ｃＢＮ焼結体に含まれるタングステン元素量が多くなると耐欠損性が低下する傾向があることが分かる。
　平均粒径０．４～１．０μｍの微粒ｃＢＮ粉末、平均粒径３．２～５．７μｍの粗粒ｃＢＮ粉末、平均粒径１．５μｍのＴｉＮ粉末、平均粒径３．１μｍのＡｌ粉末を用意し、表１１に示す配合組成になるように秤量した。
Figure JPOXMLDOC01-appb-T000012
　試料番号１６と試料番号２２について、ｃＢＮ粉末以外の結合相形成用粉末をＷＣ基超硬合金ボールと有機溶媒とポットとからなる湿式ボールミルを用いて混合した。得られた混合粉末を８５０℃で熱処理して反応させ脆性のある相にした。得られた脆性のある相をＷＣ基超硬合金ボールと有機溶媒とポットとからなる湿式ボールミルを用いて細かく粉砕した。試料番号１６は細かく粉砕した脆性のある相の粉末に表１１に示す平均粒径０．４μｍの微粒ｃＢＮ粉末を加えて、ＷＣ基超硬合金ボールと有機溶媒とポットとからなる湿式ボールミルを用いて１０時間混合した。試料番号２２は細かく粉砕した脆性のある相の粉末に表１１に示す平均粒径５．７μｍの粗粒ｃＢＮ粉末を加えて、ＷＣ基超硬合金ボールと有機溶媒とポットとからなる湿式ボールミルを用いて６時間混合した。得られた混合粉末をＴａカプセルに入れ、Ｔａカプセルを超高圧高温発生装置に装填し、表１２に示す焼結温度と焼結圧力で焼結してｃＢＮ焼結体を得た。
　試料番号１７～２１について、ｃＢＮ粉末以外の結合相形成用粉末をＷＣ基超硬合金ボールと有機溶媒とポットとからなる湿式ボールミルを用いて混合した。得られた混合粉末を８５０℃で熱処理して反応させ脆性のある相にした。得られた脆性のある相をＷＣ基超硬合金ボールと有機溶媒とポットとからなる湿式ボールミルを用いて細かく粉砕した。細かく粉砕した脆性のある相の粉末に表１１に示す平均粒径１．０μｍの微粒ｃＢＮ粉末を加えて、ＷＣ基超硬合金ボールと有機溶媒とポットとからなる湿式ボールミルを用いて１時間混合した。この混合物にさらに平均粒径２．４～５．７μｍの粗粒ｃＢＮ粉末を加えて、ＷＣ基超硬合金ボールと有機溶媒とポットとからなる湿式ボールミルを用いて６時間混合した。得られた混合粉末をＴａカプセルに入れ、Ｔａカプセルを超高圧高温発生装置に装填し、表１２に示す焼結温度と焼結圧力で焼結してｃＢＮ焼結体を得た。
Figure JPOXMLDOC01-appb-T000013
　得られたｃＢＮ焼結体について実施例１と同様な方法でｃＢＮ焼結体の組成、ｃＢＮ量と結合相量、ｃＢＮの平均粒径、結合相の厚さの平均値と標準偏差を測定した。これらの結果は表１３に示した。
Figure JPOXMLDOC01-appb-T000014
　ＥＤＳを用いてｃＢＮ焼結体に含まれるタングステン元素量を測定した。また、ｃＢＮ焼結体の熱伝導率をレーザーフラッシュ法により測定した。それらの結果は表１４に示した。
Figure JPOXMLDOC01-appb-T000015
　ｃＢＮ焼結体をワイヤ放電加工機で所定の形状にカットしてＣＮＧＡ形状の超硬基材にろう付けし、研削仕上げ加工をしてＩＳＯ規格ＣＮＧＡ１２０４０８切削インサート形状の切削工具を得た。この切削工具にＰＶＤ法により、層厚２０ｎｍの（Ｔｉ，Ｓｉ）Ｎからなる薄層と層厚２０ｎｍの（Ａｌ，Ｃｒ）Ｎからなる薄層とを交互に積層した交互積層膜からなる被膜を、被膜全体の総膜厚が平均膜厚で１．８μｍになるように被覆し、被覆ｃＢＮ焼結体からなる切削工具を得た。得られた切削工具を用いて以下の切削試験を行った。切削工具の工具寿命は表１５に示した。
［連続切削試験］
加工形態：旋削加工、
被削材：ＳＣＭ４１５Ｈ（形状：円柱状）、
切削速度：１３０ｍ／ｍｉｎ、
送り：０．１５ｍｍ／ｒｅｖ、
切り込み：０．１５ｍｍ、
雰囲気：湿式、
寿命判定：切削工具の逃げ面摩耗が０．１ｍｍを超えたときを工具寿命とした。
［断続切削試験］
加工形態：旋削加工、
被削材：ＳＣＭ４３５Ｈ（形状：円柱に２本のＶ溝を入れた略円柱状）、
切削速度：１３０ｍ／ｍｉｎ、
送り：０．１５ｍｍ／ｒｅｖ、
切り込み０．１５ｍｍ、
雰囲気：湿式、
寿命判定：切削工具が欠損したときを工具寿命とした。
Figure JPOXMLDOC01-appb-T000016
　表１５より、試料番号１６の耐摩耗性と耐欠損性が低いことが分かる。これは、ｃＢＮが微粒であるので熱伝導率が低く、亀裂が伝播しやすいためと考えられる。また、表１５より、試料番号２２の耐摩耗性と耐欠損性が低いことが分かる。これは、ｃＢＮが粗粒であり、結合相厚さの平均値と標準偏差が大きいので、結合相が選択的に摩耗するためと考えられる。

Claims (24)

  1. 　ｃＢＮ焼結体の基材とその表面に被覆された被膜とからなり、ｃＢＮ焼結体は、ｃＢＮ：７６～９０体積％と、結合相および不可避的不純物：１０～２４体積％とからなり、ｃＢＮの平均粒径は０．５～５．０μｍであり、結合相の厚さの平均値が０．０５～０．８μｍであり、結合相の厚さの標準偏差が０．８μｍ以下である被覆ｃＢＮ焼結体。
  2. 　ｃＢＮ焼結体が、ｃＢＮ：７７～８５体積％、結合相および不可避的不純物：１５～２３体積％とからなる請求項１に記載の被覆ｃＢＮ焼結体。
  3. 　ｃＢＮ焼結体が、ｃＢＮ：７７～８３体積％、結合相および不可避的不純物：１７～２３体積％とからなる請求項１に記載の被覆ｃＢＮ焼結体。
  4. 　ｃＢＮの平均粒径が０．７～４．０μｍの範囲である請求項１～３のいずれか１項に記載の被覆ｃＢＮ焼結体。
  5. 　ｃＢＮの平均粒径が１．５～４．０μｍの範囲である請求項１～３のいずれか１項に記載の被覆ｃＢＮ焼結体。
  6. 　結合相の厚さの平均値が０．１～０．５μｍの範囲である請求項１～５のいずれか１項に記載の被覆ｃＢＮ焼結体。
  7. 　結合相の厚さの標準偏差が０．０５～０．８μｍの範囲である請求項１～６のいずれか１項に記載の被覆ｃＢＮ焼結体。
  8. 　結合相の厚さの標準偏差が０．０５～０．６μｍの範囲である請求項１～６のいずれか１項に記載の被覆ｃＢＮ焼結体。
  9. 　結合相は、Ｔｉ、Ｚｒ、Ｈｆ、Ｖ、Ｎｂ、Ｔａ、Ｃｒ、Ｍｏ、Ｗ、Ｃｏ、Ｎｉ、Ａｌの金属、それらの金属の炭化物、炭窒化物、窒化物、硼窒化物、硼化物、酸化物およびこれらの相互固溶体の中から成る群より選ばれた少なくとも１種からなる請求項１～８のいずれか１項に記載の被覆ｃＢＮ焼結体。
  10. 　結合相が、ＴｉＮ、ＴｉＣＮ、ＴｉＣ、ＴｉＢ2、ＴｉＢＮ、ＴｉＡｌＮ、Ｔｉ2ＡｌＮ、ＡｌＮ、ＡｌＢ2、Ａｌ2Ｏ3、ＺｒＣ、ＨｆＣ、ＶＣ、ＮｂＣ、ＴａＣ、Ｃｒ3Ｃ2、Ｍｏ2Ｃ、ＺｒＮ、ＨｆＮ、ＶＮ、ＮｂＮ、ＴａＮ、ＣｒＮ、ＷＣ、ＷＢ、Ｗ2Ｂ、ＣｏＷＢ、Ｗ2Ｃｏ21Ｂ6、Ｃｏ3Ｗ3Ｃ、Ｗ、ＣｏおよびＮｉから成る群より選ばれた少なくとも１種からなる請求項１～８のいずれか１項に記載の被覆ｃＢＮ焼結体。
  11. 　結合相が、ＴｉＮ、ＴｉＣＮ、ＴｉＣ、ＡｌＮ、ＡｌＢ2、Ａｌ2Ｏ3、ＴｉＢ2、ＣｏＷＢ、Ｗ2Ｃｏ21Ｂ6およびＷＣから成る群より選ばれた少なくとも１種からなる請求項１～８のいずれか１項に記載の被覆ｃＢＮ焼結体。
  12. 　結合相が、ＴｉＮ、ＴｉＣＮ、ＴｉＣ、ＡｌＮ、ＡｌＢ2、Ａｌ2Ｏ3およびＴｉＢ2から成る群より選ばれた少なくとも１種からなる請求項１～８のいずれか１項に記載の被覆ｃＢＮ焼結体。
  13. 　被膜が、Ｔｉ、Ｚｒ、Ｈｆ、Ｖ、Ｎｂ、Ｔａ、Ｃｒ、Ｍｏ、Ｗ、Ａｌ、Ｓｉの金属、それらの金属の酸化物、炭化物、炭窒化物、窒化物、硼化物およびこれらの相互固溶体の中から選ばれた少なくとも１種からなる請求項１～１２のいずれか１項に記載の被覆ｃＢＮ焼結体。
  14. 　被膜が、ＴｉＣ、ＴｉＣＮ、ＴｉＮ、（Ｔｉ，Ａｌ）Ｎ、（Ｔｉ，Ｓｉ）Ｎ、（Ａｌ，Ｃｒ）Ｎ、（Ａｌ，Ｃｒ）ＮＯ、（Ｔｉ，Ａｌ，Ｃｒ）Ｎ、Ａｌ2Ｏ3および（Ａｌ，Ｃｒ）2Ｏ3から成る群より選ばれた少なくとも１種からなる請求項１～１２のいずれか１項に記載の被覆ｃＢＮ焼結体。
  15. 　被膜の少なくとも１層が、組成が異なる層厚５～２００ｎｍの薄膜を交互に積層した交互積層膜である請求項１～１４のいずれか１項に記載の被覆ｃＢＮ焼結体。
  16. 　被膜全体の総膜厚は、平均膜厚で、０．３～１５μｍである請求項１～１５のいずれか１項に記載の被覆ｃＢＮ焼結体。
  17. 　被膜全体の総膜厚は、平均膜厚で、０．５～５μｍである請求項１～１５のいずれか１項に記載の被覆ｃＢＮ焼結体。
  18. 　ｃＢＮ焼結体の熱伝導率が６０Ｗ／（ｍ・Ｋ）以上である請求項１～１７のいずれか１項に記載の被覆ｃＢＮ焼結体。
  19. 　ｃＢＮ焼結体の熱伝導率が７５Ｗ／（ｍ・Ｋ）以上である請求項１～１７のいずれか１項に記載の被覆ｃＢＮ焼結体。
  20. 　ｃＢＮ焼結体の熱伝導率が１６０Ｗ／（ｍ・Ｋ）以下である請求項１～１９のいずれか１項に記載の被覆ｃＢＮ焼結体。
  21. 　ｃＢＮ焼結体に含まれるタングステン元素量がｃＢＮ焼結体全体に対して０～８質量％である請求項１～２０のいずれか１項に記載の被覆ｃＢＮ焼結体。
  22. 　ｃＢＮが、平均粒径２．０μｍ超７．０μｍ以下の粗粒ｃＢＮ粉末と平均粒径０．５μｍ以上２．０μｍ以下の微粒ｃＢＮ粉末を、体積比で粗粒ｃＢＮ粉末：微粒ｃＢＮ粉末＝（９．５～７）：（０．５～３）（但し、粗粒ｃＢＮ粉末と微粒ｃＢＮ粉末の合計は１０とする。）の範囲内で混合したものを焼結したものである請求項１～２１のいずれか１項に記載の被覆ｃＢＮ焼結体。
  23. 　ｃＢＮが、粗粒ｃＢＮ粉末を５６～７６体積％、微粒ｃＢＮ粉末を４～２４体積％、結合相形成用粉末を１０～２４体積％とし、これらの合計が１００体積％となるように粗粒ｃＢＮ粉末、微粒ｃＢＮ粉末および結合相形成用粉末を混合したものを焼結したものである請求項２２に記載の被覆ｃＢＮ焼結体。
  24. 　請求項１～２３のいずれか１項に記載の被覆ｃＢＮ焼結体を切削工具として用いる切削工具用被覆ｃＢＮ焼結体。
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JP2018502984A (ja) * 2014-11-19 2018-02-01 ダイヤモンド イノヴェーションズ インコーポレイテッド 立方晶窒化ホウ素の多峰性粉体を調製する方法
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