WO2012057184A1 - 立方晶窒化硼素焼結体及び立方晶窒化硼素焼結体工具 - Google Patents

立方晶窒化硼素焼結体及び立方晶窒化硼素焼結体工具 Download PDF

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WO2012057184A1
WO2012057184A1 PCT/JP2011/074628 JP2011074628W WO2012057184A1 WO 2012057184 A1 WO2012057184 A1 WO 2012057184A1 JP 2011074628 W JP2011074628 W JP 2011074628W WO 2012057184 A1 WO2012057184 A1 WO 2012057184A1
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sintered body
zro
volume
cbn
less
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PCT/JP2011/074628
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English (en)
French (fr)
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克己 岡村
真知子 阿部
久木野　暁
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住友電工ハードメタル株式会社
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Priority to KR1020127024304A priority Critical patent/KR101848941B1/ko
Priority to JP2012512127A priority patent/JP5841050B2/ja
Priority to CN201180017127.9A priority patent/CN102821898B/zh
Priority to EP11836317.5A priority patent/EP2633930A4/en
Priority to CA2794396A priority patent/CA2794396C/en
Priority to US13/700,041 priority patent/US8962505B2/en
Publication of WO2012057184A1 publication Critical patent/WO2012057184A1/ja

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23B—TURNING; BORING
    • B23B27/00—Tools for turning or boring machines; Tools of a similar kind in general; Accessories therefor
    • B23B27/14—Cutting tools of which the bits or tips or cutting inserts are of special material
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    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23B—TURNING; BORING
    • B23B27/00—Tools for turning or boring machines; Tools of a similar kind in general; Accessories therefor
    • B23B27/14—Cutting tools of which the bits or tips or cutting inserts are of special material
    • B23B27/18—Cutting tools of which the bits or tips or cutting inserts are of special material with cutting bits or tips or cutting inserts rigidly mounted, e.g. by brazing
    • B23B27/20—Cutting tools of which the bits or tips or cutting inserts are of special material with cutting bits or tips or cutting inserts rigidly mounted, e.g. by brazing with diamond bits or cutting inserts
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    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/583—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride
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    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/6303—Inorganic additives
    • C04B35/6306—Binders based on phosphoric acids or phosphates
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    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23C—MILLING
    • B23C2222/00—Materials of tools or workpieces composed of metals, alloys or metal matrices
    • B23C2222/14—Cast iron
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    • B23C—MILLING
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Definitions

  • the present invention relates to a cubic boron nitride sintered body (cBN sintered body) excellent in wear resistance and fracture resistance, and a sintered body tool using the same.
  • the present invention relates to a cubic boron nitride sintered body having excellent wear resistance and fracture resistance as a centrifugal cast iron cutting tool.
  • Centrifugal cast iron has a problem that the machinability is poor and the tool life for cutting centrifugal cast iron is remarkably short as compared with cast iron using a normal sand mold.
  • Centrifugal cast iron has a fine and dense A-type structure found in conventional sand cast iron, so that the wear of the cutting tool greatly proceeds due to thermal reaction with the work material. Machinability is significantly reduced.
  • a cBN sintered body added with Al 2 O 3 having excellent oxidation resistance and chemical stability is effective as a cutting tool.
  • the cBN sintered body to which Al 2 O 3 is added has low toughness and sinterability.
  • Patent Literature 1 and Patent Literature 2 disclose a cBN sintered body in which fracture resistance is improved by adding ZrO 2 to Al 2 O 3 .
  • Patent Document 1 in a cBN sintered body containing Al 2 O 3 , TiC or TiCN, and ZrO 2 , the cBN component is 50% by volume to 80% by volume, and TiC is 1% by volume to 20% by volume. and below or TiCN less than 15 vol% 0.5 vol%, Al 2 O 3 and ZrO 2 to which contained 50 vol% or less than 15 vol%, and the weight ratio of ZrO 2 / Al 2 O 3 is 0
  • a cBN sintered body formed using a raw material having a composition of 1 or more and 4 or less is disclosed.
  • the weight ratio defined by ZrO 2 / Al 2 O 3 is converted into a volume content ratio, 0.065 ⁇ ZrO 2 / Al 2 O 3 ⁇ 2.62 is established.
  • Patent Document 2 discloses that 40 to 70% by volume of cBN particles, 15 to 45% by volume of titanium nitride as a main component of the binder phase, Al 2 O 3 , ZrO 2 as subcomponents of the binder phase, It has a composition comprising 15 to 35 volume% of mixed powder of AlN and SiC needle crystals, and the composition of the secondary component of the binder phase is 50 to 65 volume% of Al 2 O 3 and 1 to 5 volume of ZrO 2.
  • a sintered body material having a ratio of AlN 20 to 40% by volume and SiC needle crystal 5 to 15% by volume is disclosed.
  • the present invention provides cBN sintering that is excellent in wear resistance and fracture resistance even in the processing of difficult-to-cut centrifugal cast iron having a rose-like structure and a dendrite structure. And a cBN sintered body tool.
  • the present invention is as follows. (1) 20% by volume or more and 65% by volume or less of cBN with respect to the entire sintered body, and as a binder, Al 2 O 3 is 34% by volume or more and less than 80% by volume with respect to the entire sintered body.
  • X nitrides, carbides, carbonitrides, borides, at least a kind (hereinafter referred to as X) is selected from the group consisting of boronitride compound and a solid solution thereof, and a ZrO 2, the sum of X and ZrO 2 in but not more than 6.0 vol% 1.0 vol% or more with respect to the entire sintered body, ZrO 2 and Al 2 O 3 volume ratio ZrO 2 / Al 2 O 3 is less than 0.010 or more 0.100 It is a certain cBN sintered body, and among the X-ray diffraction peaks of the cBN sintered body, the intensity of the (101) plane of tetragonal ZrO 2 is the same as that of I tetragonal ZrO 2 (101), ⁇ Al 2 O 3 (110) When the surface strength is I ⁇ Al2O3 (110), I tetragonal crystal ZrO2 (101) / I ⁇ Al2O3 (110) is 0.1 or more and
  • the wear resistance useful as a cutting tool used for processing difficult-to-cut materials such as centrifugal cast cast iron having a rose-like structure and a dendrite structure exists.
  • a cBN sintered body having excellent fracture resistance can be obtained.
  • cBN is 20 volume% or more and 65 volume% or less with respect to the entire sintered body
  • Al 2 O 3 is 34 volume% or more and 80 volume with respect to the entire sintered body as a binder.
  • % At least one selected from the group consisting of nitrides, carbides, carbonitrides, borides, boronitrides and their solid solutions of Zr (hereinafter referred to as X), and ZrO 2 , the total X and ZrO 2 is not more than 6.0 vol% 1.0 vol% or more with respect to the entire sintered body, ZrO 2 and Al 2 O 3 volume ratio ZrO 2 / Al 2 O 3 is 0.010
  • the cBN sintered body is less than 0.100, and the intensity of the (101) plane of tetragonal ZrO 2 is I tetragonal ZrO 2 (101), ⁇ Al 2 among the X-ray diffraction peaks of the cBN sintered body.
  • the strength of the (110) plane of O 3 is I ⁇ Al2O3 (110)
  • the cBN sintered body is characterized in that I tetragonal ZrO2 (101) / I ⁇ Al2O3 (110) is 0.1 or more and 3 or less.
  • content in the sintered compact of cBN is 20 volume% or more and 65 volume% or less with respect to the whole sintered compact, Preferably it is 40 volume% or more and 50 volume% or less.
  • the cBN component is less than 20% by volume, in the cutting of difficult-to-cut centrifugal cast iron, the strength is insufficient, the fracture resistance is lowered, and the cutting edge is chipped.
  • it exceeds 65% by volume the content of Al 2 O 3 is relatively lowered, so that the heat resistance is lowered, and it becomes easy to react with the heat generated during the cutting process, and the wear tends to proceed.
  • the composition of each component with respect to the entire sintered body can be measured, for example, as follows, but is the same as the composition of the raw material used and does not change.
  • the composition of each component of the sintered body first, the cBN sintered body was mirror-polished, and a structure in an arbitrary region was photographed as a reflected electron image of a scanning electron microscope at a magnification of 10,000 times.
  • the contrast of the three gradations corresponding to the composition is observed, and at the same time, the portion observed the blackest in the analysis by EDX (energy dispersive X-ray analyzer) measuring the same field of view is the cBN particle
  • the portion observed in the middle color tone was found to be Al 2 O 3 particles, and the brightest portion observed was a Zr compound (oxide, carbide, nitride, boride, boronitride).
  • the volume content of each component was determined.
  • the composition of the Zr compound was quantified by chemical analysis such as plasma emission spectroscopy (ICP) or gas analysis.
  • the cBN sintered body of the present invention contains Al 2 O 3 in an amount of 34% by volume to less than 80% by volume, preferably 50% by volume to 60% by volume, based on the entire sintered body.
  • Al 2 O 3 content is less than 34% by volume, the wear resistance is lowered, and when it is 80% by volume or more, the fracture resistance is lowered.
  • Al 2 O 3 it is possible to prevent the progress of wear due to the reaction between the cast iron and the blade edge component by utilizing the properties of oxidation resistance and chemical stability of Al 2 O 3 .
  • voids are easily generated on the surface of cBN, sinterability is reduced, and fracture resistance is reduced.
  • Al 2 O 3 has high heat resistance, but lacks toughness, so that Al 2 O 3 alone tends to cause chipping at the cutting edge.
  • At least one selected from the group consisting of Zr nitrides, carbides, carbonitrides, borides, boronitrides and their solid solutions (hereinafter referred to as X) and ZrO 2 are combined in the cBN sintered body. in contained less 6.0 vol% 1.0 vol% or more with respect to the entire sintered body, ZrO 2 and Al 2 O 3 volume ratio ZrO 2 / Al 2 O 3 is less than 0.010 or more 0.100 is there.
  • the total content of X and ZrO 2 is 1.0% by volume or more and 6.0% by volume or less, the fracture resistance is improved.
  • the total of X and ZrO 2 is more preferably more than 2.5% by volume and not more than 4.0% by volume, and the wear resistance is further improved.
  • the wear resistance and fracture resistance can be improved. If the ZrO 2 / Al 2 O 3 is less than 0.010, the effect of improving the toughness of Al 2 O 3 by ZrO 2 cannot be obtained, and the fracture resistance is lowered, and if it is 0.100 or more, the wear resistance is lowered.
  • the volume ratio ZrO 2 / Al 2 O 3 between ZrO 2 and Al 2 O 3 is more preferably 0.02 or more and less than 0.06.
  • the intensity of the (101) plane of tetragonal ZrO 2 is expressed by I tetragonal ZrO 2 (101 )
  • the strength of the (110) plane of ⁇ Al 2 O 3 is I ⁇ Al2O3 (110)
  • the ratio of I tetragonal ZrO2 (101) / I ⁇ Al2O3 (110) is 0.1 or more and 3 or less.
  • I tetragonal ZrO2 (101) / I ⁇ Al2O3 (110) is less than 0.1, the effect of improving the sinterability cannot be obtained, and when it exceeds 3, the wear resistance is lowered.
  • I tetragonal ZrO2 (101) / I ⁇ Al2O3 (110) is more preferably 0.2 or more and 0.5 or less.
  • the peak intensity of tetragonal ZrO 2 (101) can be selectively increased, and even if the content of Al 2 O 3 is relatively increased by a small amount of ZrC, I Tetragonal ZrO2 (101) / I ⁇ Al2O3 (110) can achieve 0.2 or more and 0.5 or less, improving sinterability, and improving fracture resistance and productivity.
  • ZrC is preferably contained in the cBN sintered body in an amount of 0.1% by volume to 3.0% by volume.
  • the sintered body of the present invention is obtained by sintering the above sintered body raw material.
  • Al 2 O 3 , ZrO 2 and X are pulverized and mixed in advance to produce a binder.
  • the cBN sintered body of the present invention can be produced by sintering the mixed powder obtained by uniformly mixing the cBN particles and the binder under ultra high pressure conditions (5.5 to 7 GPa, 1300 to 1800 ° C.).
  • the volume average particle diameter of Al 2 O 3 used as the binder is preferably 1 ⁇ m or less, and more preferably 50 to 500 nm.
  • the volume average particle size of X and ZrO 2 used as the binder is preferably 1 ⁇ m or less, and more preferably 10 to 100 nm.
  • the cBN sintered body tool of the present invention includes a cBN sintered body tool having a cBN sintered body at least at a portion to be a cutting edge of a cemented carbide base material, or a cBN sintered body constituted only by a cBN sintered body.
  • Examples include body tools. These can be produced according to a known method. Further, a hard ceramic coating layer may be provided on the surface of the cBN sintered body.
  • Example 1 Al 2 O 3 having a volume average particle diameter of 1 ⁇ m or less, ZrO 2 having a volume average particle diameter of 0.5 ⁇ m or less, and a Zr-based compound having a volume average particle diameter of 1 ⁇ m or less are used in the composition shown in Table 1, and ⁇ 0.6 mm in advance.
  • the above compound was mixed and pulverized for 150 minutes in a solvent of ethanol at a flow rate of 0.6 L / min with a ZrO 2 ball media, and the media was removed, so that the ultrafine Zr compound was dissolved in Al 2 O 3 .
  • a specially dispersed specially dispersed material was produced.
  • the volume average particle diameter of Al 2 O 3 after mixing and pulverization was 250 nm, and the volume average particle diameters of X and ZrO 2 were 50 nm.
  • a mixed powder obtained by uniformly mixing cBN particles (volume average particle diameter 2 ⁇ m) having the composition shown in Table 1 and the above-mentioned binder with a ball medium made of ZrO 2 having a diameter of 3 mm by a ball mill mixing method is laminated on a cemented carbide support plate, and Mo After filling the capsules made, it was sintered for 30 minutes at a pressure of 6.5 GPa and a temperature of 1700 ° C. by an ultra-high pressure device to prepare a sintered body.
  • the compound was identified by X-ray diffraction measurement, and I tetragonal ZrO2 (101) / I ⁇ Al2O3 (110) was determined.
  • Examples 2 to 10 Comparative Examples 1 to 5
  • a cBN sintered body was produced in the same manner as in Example 1 except that the composition of the sintered body raw material and the compound were changed to those shown in Table 1.
  • Example 3 in which / I ⁇ Al2O3 (110) is in the range of 0.2 to 0.5 has the smallest amount of wear, and the best result is obtained without occurrence of chipping or chipping.
  • the cBN sintered body of the present invention is excellent in wear resistance and fracture resistance, and is difficult to cut such as centrifugal cast cast iron having a rose-like structure and a dendrite structure in addition to a fine and dense A-type structure. It is useful as a cutting tool used for machining a cutting material.

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Abstract

　本発明は、難削性の遠心鋳造鋳鉄の加工においても、耐摩耗性、及び耐欠損性に優れるｃＢＮ焼結体及びｃＢＮ焼結体工具を提供することを目的とする。　本発明のｃＢＮ焼結体は、ｃＢＮを２０体積％以上６５体積％以下と、結合材として、Ａｌ２Ｏ３を３４体積％以上８０体積％未満と、Ｚｒの窒化物、炭化物、炭窒化物、硼化物、硼窒化物及びこれらの固溶体から選択される少なくとも一種（以下Ｘ）と、ＺｒＯ２とを含み、ＸとＺｒＯ２の合計が１．０体積％以上６．０体積％以下であり、ＺｒＯ２とＡｌ２Ｏ３の体積比率ＺｒＯ２／Ａｌ２Ｏ３が０．０１０以上０．１００未満であり、該ｃＢＮ焼結体のＸ線回折ピークのうち、正方晶ＺｒＯ２の（１０１）面の強度をＩ正方晶ＺｒＯ２（１０１）、αＡｌ２Ｏ３の（１１０）面の強度をＩαＡｌ２Ｏ３（１１０）としたときに、Ｉ正方晶ＺｒＯ２（１０１）／ＩαＡｌ２Ｏ３（１１０）が０．１以上３以下である。

Description

立方晶窒化硼素焼結体及び立方晶窒化硼素焼結体工具
　本発明は、耐摩耗性、及び耐欠損性に優れる立方晶窒化硼素焼結体（ｃＢＮ焼結体）及びそれを用いた焼結体工具に関する。特に遠心鋳造鋳鉄切削工具として耐摩耗性、及び耐欠損性に優れた立方晶窒化硼素焼結体に関する。
　近年、エンジンの軽量化のために、シリンダブロックの材質が鋳鉄からアルミに代わる傾向にあり、ブロックのシリンダーライナーとして遠心鋳造法により製造された鋳鉄の採用が増加している。
　遠心鋳造鋳鉄は、通常の砂型を用いた鋳鉄に比べて、被削性が悪く、遠心鋳造鋳鉄を切削する工具寿命が著しく短い問題があった。
　遠心鋳造鋳鉄は、従来の砂型鋳造鋳鉄にも見られるＡ型組織が微細かつ密に存在することにより、被削材との熱的な反応により切削工具の摩耗が大きく進行し、遠心鋳造鋳鉄の被削性が著しく低下する。
　このような難削性の遠心鋳造鋳鉄加工に対応する為に、切削工具としては、耐酸化性、化学的安定性に優れるＡｌ２Ｏ３を添加したｃＢＮ焼結体が効果的であることが知られている。しかし、Ａｌ２Ｏ３を添加したｃＢＮ焼結体は、靭性、及び焼結性が低くなる。その問題を解決するものとして、Ａｌ２Ｏ３にＺｒＯ２を添加することにより耐欠損性を向上させたｃＢＮ焼結体が特許文献１や特許文献２に開示されている。
　例えば、特許文献１ではＡｌ２Ｏ３と、ＴｉＣ又はＴｉＣＮと、ＺｒＯ２を含むｃＢＮ焼結体において、ｃＢＮ成分が５０体積％以上８０体積％以下であり、ＴｉＣを１体積％以上２０体積％以下又はＴｉＣＮを０．５体積％以上１５体積％以下と、Ａｌ２Ｏ３及びＺｒＯ２を１５体積％以上５０体積％以下含有しており、かつＺｒＯ２／Ａｌ２Ｏ３の重量比が０．１以上４以下となる組成である原料を用いて形成されたｃＢＮ焼結体が開示されている。ＺｒＯ２／Ａｌ２Ｏ３で規定されている重量比を体積含有率比に変換すると、０．０６５≦ＺｒＯ２／Ａｌ２Ｏ３≦２．６２となる。
　また、特許文献２には、ｃＢＮの粉粒４０～７０体積％と、結合相の主成分となる窒化チタン１５～４５体積％と、結合相の副成分となるＡｌ２Ｏ３、ＺｒＯ２、ＡｌＮ及びＳｉＣの針状結晶の混合粉粒１５～３５体積％とからなる組成を有し、且つ上記結合相の副成分の組成がＡｌ２Ｏ３５０～６５体積％、ＺｒＯ２１～５体積％、ＡｌＮ２０～４０体積％、及びＳｉＣの針状結晶５～１５体積％の比率となっている焼結体材料が開示されている。
　遠心鋳造法では、回転させた円柱の型に溶融鋳鉄を流し込むことにより、薄いスリーブを製造できるメリットがあるが、型との接触部や最内径部は急冷されるため、鋳鉄組織が微細化し、デンドライト組織やバラ状組織といった異常組織が生成される。デンドライト組織やバラ状組織といった異常組織は非常に被削性が悪い。ごく最近の遠心鋳造鋳鉄製スリーブでは、シリンダボア間の距離を短くするために、より薄肉化が進み、従来の遠心鋳造鋳鉄の切削領域であった微細かつ密なＡ型組織に加えて、従来の遠心鋳造鋳鉄では切削する領域では無かったバラ状組織やデンドライト組織が存在する領域を切削する必要が生じている。バラ状組織やデンドライト組織が存在する領域を切削するのは、従来の遠心鋳造鋳鉄に比べてより熱的に過酷な状況下での加工となる為、被削性が著しく低下することが問題である。
　上記の特許文献に記載されている焼結体でこのような遠心鋳造鋳鉄を加工すると、熱伝導率がＡｌ２Ｏ３と比較して著しく低いＺｒＯ２を多く含むことにより焼結体の熱伝導率が低下し、加工中の被削材との反応が大きく進行することにより、耐摩耗性が著しく低下する。
国際公開第第２００８／０８７９４０号 特許第２９７１２０３号公報
　本発明は、上記微細かつ密なＡ型組織に加えて、バラ状組織やデンドライト組織が存在する難削性の遠心鋳造鋳鉄の加工においても、耐摩耗性、及び耐欠損性に優れるｃＢＮ焼結体及びｃＢＮ焼結体工具を提供することを目的とする。
　本発明者ら鋭意検討を行った結果、ｃＢＮ焼結体において、結合材として、Ａｌ２Ｏ３と、ＺｒＯ２とともに、Ｚｒの窒化物、炭化物、炭窒化物、硼化物、硼窒化物及びこれらの固溶体からなる群の中から選択される少なくとも一種を添加することにより、ＺｒＯ２のＸ線の回折強度が変化することを発見し、また、Ｉ正方晶ＺｒＯ２（１０１）／ＩαＡｌ２Ｏ３（１１０）と切削性能及び焼結性に相関があることを見出した。また、ｃＢＮ焼結体のＺｒＯ２とＡｌ２Ｏ３の体積比率と、Ｉ正方晶ＺｒＯ２（１０１）／ＩαＡｌ２Ｏ３（１１０）の数値を規定値内にすることにより、耐摩耗性と耐欠損性の双方を格段に向上させることができることを見出し本発明に至った。
　即ち、本発明は以下のとおりである。
（１）ｃＢＮを焼結体全体に対して２０体積％以上６５体積％以下と、結合材として、Ａｌ２Ｏ３を焼結体全体に対して３４体積％以上８０体積％未満と、Ｚｒの窒化物、炭化物、炭窒化物、硼化物、硼窒化物及びこれらの固溶体からなる群の中から選択される少なくとも一種（以下Ｘとする）と、ＺｒＯ２とを含み、ＸとＺｒＯ２の合計が焼結体全体に対して１．０体積％以上６．０体積％以下であり、ＺｒＯ２とＡｌ２Ｏ３の体積比率ＺｒＯ２／Ａｌ２Ｏ３が０．０１０以上０．１００未満であるｃＢＮ焼結体であって、該ｃＢＮ焼結体のＸ線回折ピークのうち、正方晶ＺｒＯ２の（１０１）面の強度をＩ正方晶ＺｒＯ２（１０１）、αＡｌ２Ｏ３の（１１０）面の強度をＩαＡｌ２Ｏ３（１１０）としたときに、Ｉ正方晶ＺｒＯ２（１０１）／ＩαＡｌ２Ｏ３（１１０）が０．１以上３以下であることを特徴とするｃＢＮ焼結体。
（２）前記ＸとしてＺｒＣを含むことを特徴とする前記（１）に記載のｃＢＮ焼結体。
（３）前記のＩ正方晶ＺｒＯ２（１０１）／ＩαＡｌ２Ｏ３（１１０）が０．２以上０．５以下であることを特徴とする前記（１）又は（２）に記載のｃＢＮ焼結体。
（４）少なくとも刃先となる部分に前記（１）～（３）のいずれかに記載のｃＢＮ焼結体を有することを特徴とするｃＢＮ焼結体工具。
　本発明によると、微細かつ密なＡ型組織に加えて、バラ状組織やデンドライト組織が存在する遠心鋳造鋳鉄等の難削な被削材の加工に用いる切削工具として有用な、耐摩耗性と耐欠損性に優れたｃＢＮ焼結体を得ることができる。
　本発明のｃＢＮ焼結体は、ｃＢＮを焼結体全体に対して２０体積％以上６５体積％以下と、結合材として、Ａｌ２Ｏ３を焼結体全体に対して３４体積％以上８０体積％未満と、Ｚｒの窒化物、炭化物、炭窒化物、硼化物、硼窒化物及びこれらの固溶体からなる群の中から選択される少なくとも一種（以下Ｘとする）と、ＺｒＯ２とを含み、ＸとＺｒＯ２の合計が焼結体全体に対して１．０体積％以上６．０体積％以下であり、ＺｒＯ２とＡｌ２Ｏ３の体積比率ＺｒＯ２／Ａｌ２Ｏ３が０．０１０以上０．１００未満であるｃＢＮ焼結体であって、該ｃＢＮ焼結体のＸ線回折ピークのうち、正方晶ＺｒＯ２の（１０１）面の強度をＩ正方晶ＺｒＯ２（１０１）、αＡｌ２Ｏ３の（１１０）面の強度をＩαＡｌ２Ｏ３（１１０）としたときに、Ｉ正方晶ＺｒＯ２（１０１）／ＩαＡｌ２Ｏ３（１１０）が０．１以上３以下であることを特徴とするｃＢＮ焼結体である。
　ここで、ｃＢＮの焼結体中における含有量は焼結体全体に対して２０体積％以上６５体積％以下であり、好ましくは４０体積％以上５０体積％以下である。ｃＢＮ成分が２０体積％未満では、難削な遠心鋳造鋳鉄の切削加工において、強度が足りず、耐欠損性が低下し、刃先に欠けが生じてしまう。また、６５体積％を超えると、相対的にＡｌ２Ｏ３の含有量が低下するため耐熱性が低下し、切削加工の際に生じる熱によって反応しやすくなり、摩耗が進行しやすくなる。
　尚、本発明におけて焼結体全体に対する各成分の組成は、例えば以下のようにして測定することができるが、用いた原料の組成と同じであり、変化しない。
　焼結体の各成分の組成は、まず、ｃＢＮ焼結体を鏡面研磨して、任意の領域の組織を走査型電子顕微鏡の反射電子像として倍率１００００倍で写真撮影した。撮影した写真には、組成に対応した３階調の濃淡のコントラストが観察され、同時に同一視野を測定したＥＤＸ（エネルギー分散型Ｘ線分析装置）による解析で、最も黒く観察された部分はｃＢＮ粒子、中間の色調に観察された部分はＡｌ２Ｏ３粒子、最も明るく観察された部分はＺｒ化合物（酸化物、炭化物、窒化物、硼化物、硼窒化物）であることが判明した。この反射電子像を画像解析することで、それぞれの成分の体積含有率を求めた。
　また、Ｚｒ化合物の組成は、プラズマ発光分光分析（ＩＣＰ）やガス分析等の化学分析により定量を行った。
　次に結合材について説明する。
　本発明のｃＢＮ焼結体は、Ａｌ２Ｏ３を焼結体全体に対して３４体積％以上８０体積％未満含有し、好ましくは、５０体積％以上６０体積％以下含有する。Ａｌ２Ｏ３含有率が３４体積％未満では耐摩耗性が低下し、８０体積％以上では耐欠損性が低下する。
　Ａｌ２Ｏ３を含有させることにより、Ａｌ２Ｏ３の耐酸化性、化学的安定性の性質を利用して、鋳鉄と刃先成分の反応による摩耗の進行を防ぐことができる。しかし、Ａｌ２Ｏ３を多く含む系ではｃＢＮの表面に空孔が生じやすく、焼結性が低下し、耐欠損性が低下する。
　また、Ａｌ２Ｏ３の耐熱性は高いが、靭性に欠ける為、Ａｌ２Ｏ３だけでは刃先にチッピングが発生しやすくなる。ｃＢＮと反応しやすい上に結合材中の熱伝導率が著しく向上するＺｒの窒化物、炭化物、炭窒化物、硼化物、硼窒化物及びこれらの固溶体からなる群の中から選択される少なくとも一種（以下Ｘとする）と、Ａｌ２Ｏ３の靭性を向上させる効果のあるＺｒＯ２を配合することにより、耐欠損性と耐摩耗性の両特性を大幅に高めることができる。
　Ｚｒの窒化物、炭化物、炭窒化物、硼化物、硼窒化物及びこれらの固溶体からなる群の中から選択される少なくとも一種（以下Ｘとする）とＺｒＯ２は、ｃＢＮ焼結体中に合計で焼結体全体に対して１．０体積％以上６．０体積％以下含有され、ＺｒＯ２とＡｌ２Ｏ３の体積比率ＺｒＯ２／Ａｌ２Ｏ３は０．０１０以上０．１００未満である。
　ＸとＺｒＯ２を合計１．０体積％以上６．０体積％以下含有することにより耐欠損性が向上する。ＸとＺｒＯ２の合計が２．５体積％を超え４．０体積％以下であることがより好ましく、更に耐摩耗性が向上する。
　また、ＺｒＯ２とＡｌ２Ｏ３の体積比率ＺｒＯ２／Ａｌ２Ｏ３を０．０１０以上０．１００未満とすることにより耐摩耗性と耐欠損性を向上させることができる。前記ＺｒＯ２／Ａｌ２Ｏ３が０．０１０未満ではＺｒＯ２によるＡｌ２Ｏ３の靭性向上効果が得られなく耐欠損性が低下し、０．１００以上では耐摩耗性が低下する。ＺｒＯ２とＡｌ２Ｏ３の体積比率ＺｒＯ２／Ａｌ２Ｏ３は０．０２以上０．０６未満がより好ましい。
　また、前記ｃＢＮ焼結体のＸ線回折装置（Ｘ線管球にＣｕを使用）で測定したＸ線回折ピークのうち、正方晶ＺｒＯ２の（１０１）面の強度をＩ正方晶ＺｒＯ２（１０１）、αＡｌ２Ｏ３の（１１０）面の強度をＩαＡｌ２Ｏ３（１１０）としたときに、Ｉ正方晶ＺｒＯ２（１０１）／ＩαＡｌ２Ｏ３（１１０）が０．１以上３以下であることによって、焼結性が高まり、緻密な焼結体が得られるため、耐欠損性と耐摩耗性に優れるばかりか、焼結体の良品率が大幅に向上し、コストの低減に役立つ。Ｉ正方晶ＺｒＯ２（１０１）／ＩαＡｌ２Ｏ３（１１０）が０．１未満の場合、焼結性を高める効果が得られず、３を越える場合は耐摩耗性が低下する。Ｉ正方晶ＺｒＯ２（１０１）／ＩαＡｌ２Ｏ３（１１０）は０．２以上０．５以下がより好ましい。
　特に、ＸとしてＺｒＣを含むことにより、正方晶ＺｒＯ２（１０１）のピーク強度を選択的に高めることができ、微量のＺｒＣにより、Ａｌ２Ｏ３の含有率を相対的に高めても、Ｉ正方晶ＺｒＯ２（１０１）／ＩαＡｌ２Ｏ３（１１０）は０．２以上０．５以下を達成でき、焼結性が向上し、耐欠損性と生産性が向上する。ＺｒＣはｃＢＮ焼結体中０．１体積％以上３．０体積％以下含有されることが好ましい。
　本発明の焼結体は、上記の焼結体原料を焼結することにより得られる。
　例えば、まずＡｌ２Ｏ３とＺｒＯ２とＸを事前に粉砕混合し、結合材を作製する。次に、ｃＢＮ粒子と前記結合材を均一混合した混合粉末を超高圧条件（５．５～７ＧＰａ、１３００～１８００℃）で焼結することにより本発明のｃＢＮ焼結体を作製することができる。
　結合材として用いるＡｌ２Ｏ３の体積平均粒径は１μｍ以下であることが好ましく、５０～５００ｎｍであることがより好ましい。また、結合材として用いるＸ及びＺｒＯ２の体積平均粒径は１μｍ以下であることが好ましく、１０～１００ｎｍであることがより好ましい。
　本発明のｃＢＮ焼結体工具としては、超硬合金製の基材の少なくとも刃先となる部分にｃＢＮ焼結体を有するｃＢＮ焼結体工具、又はｃＢＮ焼結体のみで構成されるｃＢＮ焼結体工具が挙げられる。これらは公知の方法に従って作製することができる。また、ｃＢＮ焼結体表面に硬質セラミックス被覆層を有していても構わない。
　以下、実施例に基づいて本発明の実施の形態の一例を説明する。以下の実施例は例示であり、本発明を限定するものではない。
［実施例１］
　体積平均粒径１μｍ以下のＡｌ２Ｏ３と、体積平均粒径０．５μｍ以下のＺｒＯ２と、体積平均粒径１μｍ以下のＺｒ系化合物を表１に示す組成で用い、事前にφ０．６ｍｍのＺｒＯ２製ボールメディアで、流速０．６Ｌ／ｍｉｎのエタノールの溶媒中で１５０分間、上記化合物を混合微粉砕し、該メディアを取り除くことにより、超微粒のＺｒ化合物がＡｌ２Ｏ３中に均一に分散した特殊結合材を作製した。上記、混合微粉砕後のＡｌ２Ｏ３の体積平均粒径は２５０ｎｍ、またＸ及びＺｒＯ２の体積平均粒径は５０ｎｍであった。
　表１に示す組成のｃＢＮ粒子（体積平均粒径２μｍ）と上記結合材とをφ３ｍｍのＺｒＯ２製ボールメディアでボールミル混合法により均一混合した混合粉末を超硬合金製支持板に積層してＭｏ製カプセルに充填後、超高圧装置によって、圧力６．５ＧＰａ、温度１７００℃で３０分間焼結し、焼結体を作製した。Ｘ線回折測定により、化合物を同定し、Ｉ正方晶ＺｒＯ２（１０１）／ＩαＡｌ２Ｏ３（１１０）を求めた。
［実施例２～１０、比較例１～５］
　焼結体原料の組成、化合物を表１に示すものに変えた以外は実施例１と同様にしてｃＢＮ焼結体を作製した。
［評価］
　得られた焼結体をＩＳＯ規格ＳＮＧＮ０９０３１２の切削加工用チップに加工し、内径連続切削試験を行った。
　内径８５ｍｍの遠心鋳造鋳鉄スリーブを切削速度７００ｍ／ｍｉｎ、切り込み０．３ｍｍ、送り量０．０５ｍｍ／ｒｅｖ、湿式切削［クーラント：エマルジョン（製造元：日本フルードシステム、商品名：システムカット９６）２０倍希釈］で旋削し、１ｋｍ加工後の逃げ面摩耗量と２ｋｍ加工後の刃先状態（逃げ面摩耗、チッピングの有無）を調べた。
　結果を表１に示す。
　実施例のｃＢＮ焼結体は全て、正常な研磨面が得られたのに対して、Ｘが含まれない比較例１、２は、微小な焼結体の脱落が観察され、焼結が不十分である結果であった。
　実施例１～４を比較すると、ｃＢＮ含有量が４０体積％以上５０体積％以下の範囲内である実施例３が最も摩耗量が小さく良好な結果が得られている。
　Ｘ＋ＺｒＯ２が１．０～６．０体積％の範囲内である実施例１～１０は、同値が１０．０体積％である比較例３と比較して大幅に摩耗量が小さく良好な結果が得られている。また、特に同値が２．５～４．０体積％の範囲内であって、ＺｒＯ２／Ａｌ２Ｏ３が０．０２～０．０６の範囲内であって、Ｉ正方晶ＺｒＯ２（１０１）／ＩαＡｌ２Ｏ３（１１０）が０．２～０．５の範囲内である実施例３が最も摩耗量が小さく、欠損やチッピングも発生せずに最良の結果が得られている。
　ＺｒＯ２／Ａｌ２Ｏ３が０．１２５、Ｉ正方晶ＺｒＯ２（１０１）／ＩαＡｌ２Ｏ３（１１０）が５．８である比較例４は、ＺｒＯ２自体の耐摩耗性がＡｌ２Ｏ３より大幅に劣るため、実施例１～１０に比べ大幅に摩耗量が大きく、２ｋｍ時点では、恐らく大摩耗により切削抵抗が増大し欠損に至ったと推定される。
　Ｉ正方晶ＺｒＯ２（１０１）／ＩαＡｌ２Ｏ３（１１０）が０．０５である比較例５は、焼結が不十分なため、耐摩耗性と耐欠損性が低下したと推定される。
Figure JPOXMLDOC01-appb-T000001
業上の利用可能性
　本発明のｃＢＮ焼結体は、耐摩耗性と耐欠損性に優れており、微細かつ密なＡ型組織に加えて、バラ状組織やデンドライト組織が存在する遠心鋳造鋳鉄等の難削な被削材の加工に用いる切削工具として有用である。

Claims (4)

  1. 　ｃＢＮを焼結体全体に対して２０体積％以上６５体積％以下と、結合材として、Ａｌ２Ｏ３を焼結体全体に対して３４体積％以上８０体積％未満と、Ｚｒの窒化物、炭化物、炭窒化物、硼化物、硼窒化物及びこれらの固溶体からなる群の中から選択される少なくとも一種（以下Ｘとする）と、ＺｒＯ２とを含み、ＸとＺｒＯ２の合計が焼結体全体に対して１．０体積％以上６．０体積％以下であり、ＺｒＯ２とＡｌ２Ｏ３の体積比率ＺｒＯ２／Ａｌ２Ｏ３が０．０１０以上０．１００未満であるｃＢＮ焼結体であって、該ｃＢＮ焼結体のＸ線回折ピークのうち、正方晶ＺｒＯ２の（１０１）面の強度をＩ正方晶ＺｒＯ２（１０１）、αＡｌ２Ｏ３の（１１０）面の強度をＩαＡｌ２Ｏ３（１１０）としたときに、Ｉ正方晶ＺｒＯ２（１０１）／ＩαＡｌ２Ｏ３（１１０）が０．１以上３以下であることを特徴とするｃＢＮ焼結体。
  2. 　前記ＸとしてＺｒＣを含むことを特徴とする請求項１に記載のｃＢＮ焼結体。
  3. 　前記のＩ正方晶ＺｒＯ２（１０１）／ＩαＡｌ２Ｏ３（１１０）が０．２以上０．５以下であることを特徴とする請求項１又は２に記載のｃＢＮ焼結体。
  4. 　少なくとも刃先となる部分に請求項１～３のいずれかに記載のｃＢＮ焼結体を有することを特徴とするｃＢＮ焼結体工具。
     
     
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KR101848941B1 (ko) 2018-04-13
US20130079215A1 (en) 2013-03-28
CA2794396C (en) 2017-08-29
KR20130122705A (ko) 2013-11-08
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CA2794396A1 (en) 2012-05-03

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