WO2012029440A1 - 立方晶窒化硼素焼結体工具 - Google Patents

立方晶窒化硼素焼結体工具 Download PDF

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Publication number
WO2012029440A1
WO2012029440A1 PCT/JP2011/066814 JP2011066814W WO2012029440A1 WO 2012029440 A1 WO2012029440 A1 WO 2012029440A1 JP 2011066814 W JP2011066814 W JP 2011066814W WO 2012029440 A1 WO2012029440 A1 WO 2012029440A1
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Prior art keywords
boron nitride
sintered body
cubic boron
compound
cbn
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PCT/JP2011/066814
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English (en)
French (fr)
Inventor
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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Application filed by 住友電工ハードメタル株式会社 filed Critical 住友電工ハードメタル株式会社
Priority to CA2778198A priority Critical patent/CA2778198C/en
Priority to CN201180004615.6A priority patent/CN102665976B/zh
Priority to EP11821458.4A priority patent/EP2612719B1/en
Priority to US13/503,327 priority patent/US8993132B2/en
Priority to IN3125DEN2012 priority patent/IN2012DN03125A/en
Priority to KR1020127011397A priority patent/KR20120062015A/ko
Priority to JP2012531748A priority patent/JP5732663B2/ja
Publication of WO2012029440A1 publication Critical patent/WO2012029440A1/ja

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Definitions

  • the present invention relates to a cBN sintered body mainly composed of cubic boron nitride (hereinafter also referred to as cBN).
  • a high-hardness sintered body using cubic boron nitride is known.
  • the cBN particles have higher hardness, strength, and toughness than the ceramic binder, function as a skeleton in the sintered body, and maintain a material strength that can withstand cutting of high hardness hardened steel.
  • the ceramic binder serves to sinter cBN particles, which are hardly sinterable materials, at an industrial level pressure temperature, and at the same time has a lower reactivity with iron than chemical, thermal and chemical. Adds the ability to suppress wear.
  • the cBN sintered bodies are roughly classified into two types, one is a high cBN content rate, cBN is bonded to each other, and the balance is a cBN sintered body made of a binding material mainly composed of Co or Al (hereinafter, high cBN content rate sintered body) and another, Ti nitride (TiN) or carbide (TiC) having relatively low cBN content, low contact rate between cBNs, and low affinity with iron ) Through ceramics (hereinafter abbreviated as a low cBN content sintered body).
  • the former sintered body with high cBN content has excellent mechanical properties (high hardness, high strength, high toughness) and high thermal conductivity in applications where chips are cut and shear heat is not easily generated in the chips.
  • This achieves outstanding stability and long life, and iron-based sintered parts that are dominated by mechanical wear and damage due to rubbing with hard particles, and gray cast iron that is dominated by thermal shock during high-speed intermittent cutting Suitable for high-efficiency cutting.
  • the cBN component is thermally worn with iron, which makes it more difficult than conventional carbide tools and ceramic tools.
  • the wear develops rapidly, resulting in a short life.
  • the latter low cBN content sintered body exhibits excellent wear resistance due to the action of a binder composed of TiN or TiC ceramics having a lower affinity with iron at a higher temperature than cBN.
  • the hardened steel cutting market has been cultivated as a cutting tool that can achieve tool life 10 to several tens of times longer than conventional tools. .
  • Japanese Patent Application Laid-Open No. 2000-044347 Patent Document 1
  • Japanese Patent Application Laid-Open No. 2000-04350 Patent Document 2
  • Patent Document 2 include 45 to 70% by volume of cBN particles and carbides of Group 4a, 5a, and 6a elements, It consists of a binder phase containing at least one selected from the group consisting of nitride, carbonitride, boride, Al nitride, boride, oxide, carbonitride, boride, and their mutual solid solutions.
  • a cBN sintered body in which an average value and a standard deviation of the thickness of the binder phase are defined is described.
  • Patent Document 3 discloses ultra-fine cBN particles having a particle size of 0.01 ⁇ m or more and 0.70 ⁇ m or less, 4a, 5a, 6a group elements, Al, their carbides, and nitriding.
  • the cBN sintered body composed of at least one kind of binder phase, borides and their mutual solid solutions, and mixtures, there is described a cBN sintered body in which the average thickness of the binder phase is defined.
  • centrifugal casting is a technique for producing a hollow casting without using a core by rotating a mold and utilizing centrifugal force when casting a liner.
  • the contact portion and the innermost diameter portion of the mold are rapidly cooled, so that a dendrite structure and a rose-like structure having extremely poor machinability are generated in the same region.
  • the tool life is remarkably deteriorated when the cast iron structure of the cutting portion becomes the above-mentioned dendrite structure or loose structure when finishing to the above.
  • the cast iron structure varies greatly depending on the liner production lot, there is also a problem that the tool life is not stable, and the conventional high cBN content sintered body has insufficient wear resistance, and a satisfactory tool life can be obtained. There is no recent situation.
  • Patent Document 4 adopts Al 2 O 3 as the main component of the binder phase and adds appropriate amounts of ZrO 2 and TiC, thereby producing a centrifugal cast iron. Stabilization of tool life in machining has been attempted, but satisfactory tool life has not been obtained.
  • JP 2000-044347 A Japanese Patent Laid-Open No. 2000-04350 JP 2002-302732 A WO2008 / 087940
  • the present invention provides a cBN sintered body having high cutting performance and excellent tool life in the cutting of cast iron made by centrifugal casting mixed with the above-described dendritic structure and loose-shaped structure having poor machinability. It is an object to provide a tool.
  • the cBN sintered body composed of Al 2 O 3 , cBN, ZrO 2 , and TiC is inferior in fracture resistance because the average thickness of Al 2 O 3 is too thick.
  • the technique defines the thickness and the standard deviation of the binder phase to a proper value is known, Al 2 O 3 content is small, the wear resistance is insufficient in the process of centrifugal casting cast iron.
  • the inventors of the present invention have determined the optimal arrangement of the interface or grain boundary of the Al 2 O 3 particles that is the starting point of the crack and the optimum arrangement of the Zr compound that can be expected to strengthen Al 2 O 3 .
  • a cBN sintered body in which the particle size, the content rate, and the mixing method were changed was produced, and the correlation with the cutting performance was investigated.
  • the Zr compound and cBN particles in Al 2 O 3 is excellent in heat resistance and divide the Al 2 O 3 having poor toughness, optimize the average thickness and the standard deviation of the Al 2 O 3 By setting the range, we succeeded in achieving both heat resistance and toughness at a high level.
  • a cubic boron nitride sintered body tool having at least a cubic boron nitride sintered body composed of cubic boron nitride particles and a binder phase,
  • the cBN content is 20% by volume or more and 60% by volume or less, Containing at least Al 2 O 3 and a Zr compound in the binder phase;
  • the average value of the continuous distance occupied by Al 2 O 3 is 0.1 ⁇ m or more and 1.0 ⁇ m or less, and the standard deviation of the continuous distance occupied by the Al 2 O 3 is 0.8 or less
  • the number of contacts between Al 2 O 3 and Zr compound is X
  • Al 2 O 3 and Zr compound X / Y is 0.1 or more and 1 or less, where Y is the total number of contacts with A cubic boro
  • a cBN sintered body tool having high cutting performance and excellent tool life can be provided. That is, by optimally arranging the Zr compound and cBN particles in Al 2 O 3, is excellent in heat resistance and divide the Al 2 O 3 having poor toughness, the optimal range of the average thickness and the standard deviation of the Al 2 O 3 By setting to, we succeeded in achieving both heat resistance and toughness at a high level.
  • cBN particles and Al are bonded via a highly reactive compound (eg, TiAl, Ti, Al, TiZr, Zr, etc.) having an excellent bonding force other than Al 2 O 3.
  • a highly reactive compound eg, TiAl, Ti, Al, TiZr, Zr, etc.
  • the wear resistance and fracture resistance can be further improved.
  • the cBN sintered body tool according to the present invention is a cBN sintered body tool having at least a cBN sintered body composed of cBN particles and a binder phase at the cutting edge, and the cBN content is 20% by volume to 60% by volume.
  • the binder phase contains Al 2 O 3 and a Zr compound, and the average value and standard deviation of the distance occupied by Al 2 O 3 on an arbitrary straight line in the sintered body are 0.1 ⁇ m or more and 1.0 ⁇ m or less and 0, respectively.
  • the number of contacts between Al 2 O 3 and Zr compound is X
  • the number of contacts between Al 2 O 3 and cBN, Al 2 O 3 , Al 2 O 3 and Zr X / Y is 0.1 or more and 1 or less and the average particle size of the Zr compound is 0.01 ⁇ m or more and 0.1 ⁇ m or less
  • Y is the sum of the number of contacts with the binder phase component other than the compound. It is characterized by that.
  • the cBN sintered body tool may be a cBN sintered body tool having a cBN sintered body at least at a portion to be a cutting edge of a base material made of cemented carbide, or a cBN sintered body constituted only by a cBN sintered body.
  • a combined tool may be used.
  • you may have a hard ceramic coating layer in the cBN sintered compact surface used as a blade edge
  • the cBN sintered body has a cBN content of 20% by volume to 60% by volume.
  • the cBN content is more preferably 40% by volume to 50% by volume.
  • the binder phase is characterized by containing at least Al 2 O 3 and a Zr compound. Thereby, wear resistance and chipping resistance can be improved.
  • the cBN sintered body is characterized in that an average value of continuous distances occupied by Al 2 O 3 is 0.1 ⁇ m or more and 1.0 ⁇ m or less on an arbitrary straight line in the sintered body.
  • the average value is more preferably 0.3 ⁇ m or more and 0.6 ⁇ m or less.
  • the standard deviation of the continuous distance occupied by Al 2 O 3 on the arbitrary straight line is 0.8 or less. When the standard deviation exceeds 0.8, the variation in fracture resistance increases.
  • the standard deviation is more preferably 0.2 or more and 0.6 or less.
  • the number of contacts between Al 2 O 3 and Zr compound is X
  • Al 2 O 3 and Zr compounds X / Y is 0.1 or more and 1 or less, where Y is the sum of the number of contacts with the binder phase component. If the X / Y is less than 0.1, the effect of improving the toughness of Al 2 O 3 by the Zr compound cannot be obtained, and if it exceeds 1, the effect of improving the heat resistance by Al 2 O 3 decreases.
  • the average particle size of the Zr compound is 0.01 ⁇ m or more and 0.1 ⁇ m or less.
  • the average particle size of the Zr compound is more preferably 0.03 ⁇ m or more and 0.06 ⁇ m or less.
  • the present invention divides Al 2 O 3 which is excellent in heat resistance but inferior toughness by optimally arranging the Zr compound and cBN particles in Al 2 O 3 in the cBN sintered body, By setting the average thickness and standard deviation of Al 2 O 3 within the optimum range, it is possible to achieve both the heat resistance and toughness of the sintered body at a high level.
  • the cBN sintered body tool according to the present invention preferably contains ZrC and ZrO 2 in a total amount of 0.5 volume% or more and 5 volume% or less as the Zr compound contained in the sintered body. More preferably, it is 1.5 volume% or more and 4.5 volume% or less.
  • ZrC and ZrO 2 are particularly effective in improving the toughness of Al 2 O 3 , and if the total amount of both compounds is less than 0.5% by volume in the sintered body, the effect of improving toughness cannot be obtained, and 5% by volume. In the case of exceeding, the content of Al 2 O 3 is relatively lowered, and the heat resistance is lowered.
  • X / Y is 0.5 or more and 0.9 or less
  • the reliability with respect to defects increases. That is, in the cBN sintered body tool according to the present invention, X / Y is preferably 0.5 or more and 0.9 or less on an arbitrary straight line of the sintered body.
  • a mixed powder in which cBN particles and the above-mentioned binder were uniformly mixed by a ball mill mixing method using a ZrO 2 ball media having a diameter of 3 mm was laminated on a cemented carbide support plate and filled into a Mo capsule. Then, it was sintered for 30 minutes at a pressure of 7.0 GPa and a temperature of 1600 degrees by an ultrahigh pressure apparatus.
  • cBN particles were previously coated with TiZr and Zr with an average film thickness of 30 nm using an RF sputtering PVD apparatus, and filled and sintered in the same manner as described above.
  • the composition of the cBN sintered body in each example and comparative example is shown in Table 1.
  • the obtained sintered body was cut into a predetermined shape, joined to a cemented carbide tool base material using a commercially available brazing material, and ground into a predetermined tool shape.
  • [Evaluation] Measurement of cBN sintered body characteristics
  • the cBN sintered body was mirror-polished, and a reflected electron image of the structure of the cBN sintered body in an arbitrary region was photographed at a magnification of 10,000 with an electron microscope. A contrast of light and shade corresponding to the composition was observed, and the compound was estimated from the overlapping state of various elements by attached EDX (energy dispersive X-ray analysis). As a result, it was confirmed that the black region is a cBN particle, and the gray region and the white region are binder phases. Further, it was determined that the dark gray region was Al 2 O 3 and the light white region was a Zr compound (oxide, carbide, nitride, boride, borohydride).
  • the total number of contacts on the straight line was determined so that the uniformity of the structure was at least 50 points or more. Further, the distance (length) occupied by the Al 2 O 3 continuously on the straight line of the number of straight lines was measured, and the average value and standard deviation were obtained.
  • the cBN content was binarized by image processing of the cBN particle region and the binder phase region from the sintered body structure photograph, and the occupied area of the cBN particles was defined as the volume content.
  • the binder phase composition was identified by XRD (X-ray diffraction).
  • each occupied area was calculated by image processing from the contrast of the above-mentioned sintered body structure photograph, and was defined as the volume content.
  • the average particle size of the Zr compound the average particle size of the raw material powder charged is described, and it was confirmed from the above sintered body structure photograph that the particle size of the raw material powder was generally maintained. The results are shown in Table 1. (Cutting test) About each tool produced above, the cutting test was done on condition of the following. Work material: FC250 (inner diameter machining of centrifugal cast cast iron sleeve, hardness: HB230)
  • Tool shape CNGA120408
  • Cutting speed Vc 700 m / min.
  • Feed amount f 0.3 mm / rev.
  • Cutting depth ap 0.05mm
  • Tool life with cutting fluid The time when the flank wear amount or chipping reached 0.2 mm was judged as the tool life.
  • the tool of the example showed superior cutting performance compared to the tool of the comparative example.

Abstract

　立方晶窒化硼素粒子と結合相で構成される立方晶窒化硼素焼結体を少なくとも刃先に有する立方晶窒化硼素焼結体工具であって、ｃＢＮ含有率が２０体積％以上６０体積％以下であり、結合相に少なくともＡｌ2Ｏ3、及びＺｒ化合物を含み、焼結体中の任意の直線上において、Ａｌ2Ｏ3が占める連続する距離の平均値が０．１μｍ以上１．０μｍ以下であり、かつ該Ａｌ2Ｏ3が占める連続する距離の標準偏差が０．８以下であり、当該直線上において、Ａｌ2Ｏ3とＺｒ化合物との接点の数をＸ、Ａｌ2Ｏ3とｃＢＮとの接点の数と、Ａｌ2Ｏ3とＡｌ2Ｏ3及びＺｒ化合物以外の結合相成分との接点の数との合計をＹとした場合、Ｘ／Ｙが０．１以上１以下であり、Ｚｒ化合物の平均粒径が０．０１μｍ以上０．１μｍ以下であることを特徴とする。

Description

立方晶窒化硼素焼結体工具
　本発明は立方晶窒化硼素（以下、ｃＢＮとも記載する）を主成分とするｃＢＮ焼結体に関する。
　従来、立方晶窒化硼素を用いた高硬度の焼結体が知られている。ｃＢＮ粒子は硬度、強度、靭性がセラミックス結合材より高く、焼結体中の骨格として働き、高硬度焼入鋼の切削に耐えうる材料強度を保持する役割を果たす。一方、セラミックス結合材は、難焼結性材料であるｃＢＮ粒子を工業レベルの圧力温度で焼結可能とする役割を果たすと同時に、鉄との反応性がｃＢＮより低いため、化学的・熱的摩耗を抑制する働きを付加する。
　ｃＢＮ焼結体は、大きく２つに分類され、１つはｃＢＮ含有率が高く、ｃＢＮ同士が結合し、残部がＣｏやＡｌを主成分とする結合材からなるｃＢＮ焼結体（以降、高ｃＢＮ含有率焼結体と略す）と、もう１つは、ｃＢＮ含有率が比較的低く、ｃＢＮ同士の接触率が低く、鉄との親和性の低いＴｉの窒化物（ＴｉＮ）や炭化物（ＴｉＣ）からなるセラミックスを介して結合されているものである（以降、低ｃＢＮ含有率焼結体と略す）。
　前者の高ｃＢＮ含有率焼結体は、切り屑が分断され、切り屑でのせん断熱の発生し難い用途では、ｃＢＮの優れた機械特性（高硬度、高強度、高靭性）と高熱伝導率により、抜群の安定性と長寿命を達成し、硬質粒子との擦れによる機械的な摩耗や損傷が支配的な鉄系焼結部品や高速断続切削時の熱衝撃による損傷が支配的なねずみ鋳鉄の高能率切削に適している。しかしながら、連続した切り屑により発生する多量のせん断熱により刃先が高温に曝される焼入鋼などの加工では、ｃＢＮ成分が鉄との熱的な摩耗により、従来の超硬工具やセラミックス工具よりも急速に摩耗が発達するため短寿命となる。
　一方、後者の低ｃＢＮ含有率焼結体は、ｃＢＮよりも、高温下での鉄との親和性の低いＴｉＮやＴｉＣセラミックスからなる結合材の働きにより、優れた耐摩耗性を発揮し、特に、従来の超硬工具やセラミックス工具では実用加工ができなかった焼入鋼加工において、従来工具の１０倍～数十倍の工具寿命を達成できる切削工具として、焼入鋼切削市場を開拓してきた。
　これらのｃＢＮ焼結体としては種々のものが開発されている。
　例えば、特開２０００－０４４３４７号公報（特許文献１）および特開２０００－０４４３５０号公報（特許文献２）には、４５～７０体積％のｃＢＮ粒子と、４ａ，５ａ，６ａ族元素の炭化物、窒化物、炭窒化物、硼化物、Ａｌの窒化物、硼化物、酸化物、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種以上を含む結合相とからなるｃＢＮ焼結体において、結合相の厚みの平均値と標準偏差を規定したｃＢＮ焼結体が記載されている。
　また、特開２００２－３０２７３２号公報（特許文献３）には、粒径が０．０１μｍ以上０．７０μｍ以下の超微粒ｃＢＮ粒子と、４ａ，５ａ，６ａ族元素、Ａｌ、それらの炭化物、窒化物、硼化物およびそれらの相互固溶体、混合体の少なくと１種からなる結合相とからなるｃＢＮ焼結体において、結合相の厚みの平均値を規定したｃＢＮ焼結体が記載されている。
　また前記のとおり、鋳鉄の高能率切削では、高ｃＢＮ含有率焼結体が実用化されている。近年、自動車エンジンの高性能化に伴い、軽量化を狙いシリンダブロックのアルミ化が進んでいる。シリンダブロックのピストン摺動部分であるライナーについては強度と耐摩耗性に優れる鋳鉄が採用されるが、砂型鋳鉄より量産性に優れる遠心鋳造鋳鉄が採用されることが近年、増加している。遠心鋳造法とは、ライナーの鋳造の際に、鋳型を回転させ遠心力を利用して中子を用いずに中空の鋳物を作る手法である。
　前記遠心鋳造法では、原理上、鋳型の接触部や最内径部が急冷されるため、同領域では被削性が著しく悪いデンドライト組織やバラ状組織が生成されるが、切削加工により所望の内径に仕上げる際に、切削箇所の鋳鉄組織が前記のデンドライト組織やバラ状組織となる場合に工具寿命が著しく悪化する問題がある。さらに、ライナーの製造ロットによっても、鋳鉄組織が大きく変化するため、工具寿命が安定しない問題もあり、従来の高ｃＢＮ含有率焼結体では耐摩耗性が不足し、満足する工具寿命が得られていないのが最近の実情である。
　そのような事情を鑑みて、ＷＯ２００８／０８７９４０号公報（特許文献４）では、結合相の主成分にＡｌ2Ｏ3を採用し、かつ、ＺｒＯ2とＴｉＣを適量添加することにより、遠心鋳造鋳鉄加工における工具寿命の安定化が図られてきたが、満足のいく工具寿命が得られていなかった。
特開２０００－０４４３４７号公報 特開２０００－０４４３５０号公報 特開２００２－３０２７３２号公報 ＷＯ２００８／０８７９４０号公報
　本発明は、上記問題点に鑑みて、前記の被削性が悪いデンドライト組織やバラ状組織が混在した遠心鋳造製鋳鉄の切削において、切削性能が高く、かつ工具寿命に優れたｃＢＮ焼結体工具を提供することを課題とする。
　デンドライト組織やバラ状組織を有する鋳鉄をｃＢＮ焼結体工具で切削した際の摩耗形態を詳細に観察した結果、Ｔｉ化合物やＡｌ化合物で構成される結合相の中でも、耐熱性に優れるＡｌ2Ｏ3粒子の界面又は粒界で亀裂が発生し、同亀裂が伝播することにより摩耗が進行し、場合によっては欠損に至っていることを突き止めた。
　従来技術では、Ａｌ2Ｏ3、ｃＢＮ、ＺｒＯ2、ＴｉＣで構成されるｃＢＮ焼結体は、Ａｌ2Ｏ3の平均厚みが厚すぎるため、耐欠損性に劣っていた。また、結合相の厚みと標準偏差を適正値に規定した技術は公知であるが、Ａｌ2Ｏ3含有量が小さく、遠心鋳造鋳鉄の加工では耐摩耗性が不足していた。
　そこで、発明者らは、亀裂の起点となるＡｌ2Ｏ3粒子の界面又は粒界の最適配置及びＡｌ2Ｏ3を強化する効果が期待できるＺｒ化合物の最適配置を見極めるために、各成分の粒度と含有率及び混合方法を変化させたｃＢＮ焼結体を作製し、切削性能との相関を調査した。その結果、Ｚｒ化合物とｃＢＮ粒子をＡｌ2Ｏ3中に最適配置させることにより、耐熱性に優れるが靭性に劣るＡｌ2Ｏ3を分断し、Ａｌ2Ｏ3の平均厚みと標準偏差を最適な範囲に設定することによって、耐熱性と靭性を高次元で両立させることに成功した。
　すなわち、本発明は以下の構成を有する。
（１）立方晶窒化硼素粒子と結合相で構成される立方晶窒化硼素焼結体を少なくとも刃先に有する立方晶窒化硼素焼結体工具であって、
ｃＢＮ含有率が２０体積％以上６０体積％以下であり、
結合相に少なくともＡｌ2Ｏ3、及びＺｒ化合物を含み、
焼結体中の任意の直線上において、Ａｌ2Ｏ3が占める連続する距離の平均値が０．１μｍ以上１．０μｍ以下であり、かつ該Ａｌ2Ｏ3が占める連続する距離の標準偏差が０．８以下であり、
当該直線上において、Ａｌ2Ｏ3とＺｒ化合物との接点の数をＸ、Ａｌ2Ｏ3とｃＢＮとの接点の数と、Ａｌ2Ｏ3とＡｌ2Ｏ3及びＺｒ化合物以外の結合相成分との接点の数との合計をＹとした場合、Ｘ／Ｙが０．１以上１以下であり、
Ｚｒ化合物の平均粒径が０．０１μｍ以上０．１μｍ以下である
ことを特徴とする立方晶窒化硼素焼結体工具。
（２）前記の焼結体中に含まれるＺｒ化合物として、ＺｒＣ及びＺｒＯ2を合計で０．５体積％以上５体積％以下含むことを特徴とする上記（１）に記載の立方晶窒化硼素焼結体工具。
（３）前記の焼結体の任意の直線上において、Ｘ／Ｙが０．５以上０．９以下であることを特徴とする上記（１）又は（２）に記載の立方晶窒化硼素焼結体工具。
　本発明により、切削性能が高く、かつ工具寿命に優れたｃＢＮ焼結体工具を提供することができる。すなわち、Ｚｒ化合物とｃＢＮ粒子をＡｌ2Ｏ3中に最適配置させることにより、耐熱性に優れるが靭性に劣るＡｌ2Ｏ3を分断し、Ａｌ2Ｏ3の平均厚みと標準偏差を最適な範囲に設定することによって、耐熱性と靭性を高次元で両立させることに成功した。
　また、Ａｌ2Ｏ3とｃＢＮ粒子は結合力が弱いため、Ａｌ2Ｏ3以外の結合力に優れる高反応性化合物（例えばＴｉＡｌ、Ｔｉ、Ａｌ、ＴｉＺｒ、Ｚｒ等）を介してｃＢＮ粒子とＡｌ2Ｏ3粒子を結合させ、Ａｌ2Ｏ3中にＺｒ化合物を分散させることによって、より耐摩耗性と耐欠損性を高めることができる。特に、ＺｒやＴｉＺｒをｃＢＮ粒子に事前に被覆しておくことが好ましい。
　本発明に係るｃＢＮ焼結体工具は、ｃＢＮ粒子と結合相で構成されるｃＢＮ焼結体を少なくとも刃先に有するｃＢＮ焼結体工具であって、ｃＢＮ含有率が２０体積％以上６０体積％以下、結合相にＡｌ2Ｏ3、Ｚｒ化合物を含み、焼結体中の任意の直線上において、Ａｌ2Ｏ3が占める距離の平均値と標準偏差がそれぞれ０．１μｍ以上１．０μｍ以下及び０．８以下であり、当該直線上において、Ａｌ2Ｏ3とＺｒ化合物との接点の数をＸ、Ａｌ2Ｏ3とｃＢＮとの接点の数と、Ａｌ2Ｏ3とＡｌ2Ｏ3及びＺｒ化合物以外の結合相成分との接点の数との合計をＹとした場合、Ｘ／Ｙが０．１以上１以下であり、Ｚｒ化合物の平均粒径が０．０１μｍ以上０．１μｍ以下であることを特徴とする。
　上記ｃＢＮ焼結体工具は、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焼結体工具であっても、又はｃＢＮ焼結体のみで構成されるｃＢＮ焼結体工具であってもよい。また、刃先となる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、ｃＢＮ焼結体部分について詳述する。
　上記ｃＢＮ焼結体は、ｃＢＮ含有率が２０体積％以上６０体積％以下であることを特徴とする。ｃＢＮ含有率が２０体積％未満であると焼結体の耐欠損性が低下し、６０体積％を超えると耐摩耗性が低下する。ｃＢＮ含有率は、より好ましくは４０体積％以上５０体積％以下である。また、結合相には少なくとも、Ａｌ2Ｏ3、及びＺｒ化合物を含むことを特徴とする。これにより耐摩耗性と耐欠損性を向上させることができる。
　上記ｃＢＮ焼結体は、焼結体中の任意の直線上において、Ａｌ2Ｏ3が占める連続した距離の平均値が０．１μｍ以上１．０μｍ以下であることを特徴とする。当該平均値が０．１μｍ未満であると耐熱性が低下し、１．０μｍを超えると耐欠損性が低下する。該平均値は、より好ましくは０．３μｍ以上０．６μｍ以下である。また、当該任意の直線上において、Ａｌ2Ｏ3が占める連続した距離の標準偏差は０．８以下であることを特徴とする。当該標準偏差が０．８を超えると、耐欠損性のバラツキが大きくなる。該標準偏差は、より好ましくは０．２以上０．６以下である。
　更に、上記直線上において、Ａｌ2Ｏ3とＺｒ化合物との接点の数をＸとし、Ａｌ2Ｏ3とｃＢＮとの接点の数と、Ａｌ2Ｏ3とＡｌ2Ｏ3及びＺｒ化合物以外の結合相成分との接点の数との合計をＹとした場合に、Ｘ／Ｙが０．１以上１以下であることを特徴とする。当該Ｘ／Ｙが０．１未満であるとＺｒ化合物によるＡｌ2Ｏ3の靭性向上効果が得られず、１を超えるとＡｌ2Ｏ3による耐熱性向上効果が低下する。
　上記ｃＢＮ焼結体において、Ｚｒ化合物の平均粒径が０．０１μｍ以上０．１μｍ以下であることを特徴とする。Ｚｒ化合物の平均粒径が０．０１μｍ未満の場合、Ｚｒ化合物によるＡｌ2Ｏ3の靭性向上効果が得られず、０．１μｍを超えるとＺｒ化合物自体の破砕が発生しやすくなり、焼結体の耐欠損性が低下する。Ｚｒ化合物の平均粒径は、より好ましくは０．０３μｍ以上０．０６μｍ以下である。
　本発明は、上記の構成により、ｃＢＮ焼結体においてＺｒ化合物とｃＢＮ粒子をＡｌ2Ｏ3中に最適配置させることによって耐熱性には優れるが靭性に劣るＡｌ2Ｏ3を分断し、更に、Ａｌ2Ｏ3の平均厚みと標準偏差を最適な範囲に設定することによって、焼結体の耐熱性と靭性を高次元で両立させることを可能にした。
　また、前記の焼結体に含まれるＺｒ化合物として、ＺｒＣ及びＺｒＯ2を合計で０．５体積％以上５体積％以下含むことにより、耐欠損性と耐摩耗性をさらに改善できる。すなわち、本発明に係るｃＢＮ焼結体工具は、前記の焼結体に含まれるＺｒ化合物として、ＺｒＣ及びＺｒＯ2を合計で０．５体積％以上５体積％以下含むことが好ましい。より好ましくは、１．５体積％以上４．５体積％以下である。
　ＺｒＣとＺｒＯ2は特に、Ａｌ2Ｏ3の靭性を改善する効果が高く、両化合物が焼結体中で合計０．５体積％未満の場合は、靭性向上効果が得られず、５体積％超の場合は、相対的にＡｌ2Ｏ3の含有量が低下し、耐熱性が低下する。
　さらに、前記の焼結体の任意の直線上において、Ｘ／Ｙが０．５以上０．９以下であることで、欠損に対する信頼性が増す。すなわち、本発明に係るｃＢＮ焼結体工具は、前記の焼結体の任意の直線上において、Ｘ／Ｙが０．５以上０．９以下であることが好ましい。
［ｃＢＮ焼結体工具の作製］
（ｃＢＮ焼結体の作製）
　平均粒径が５０ｎｍ以下（一部の実施例および比較例を除く）の表１に示すＺｒ化合物と、平均粒径が３００ｎｍ以下のＴｉ化合物と、平均粒径が２００ｎｍ以下のＡｌ2Ｏ3とを、事前にφ０．２ｍｍのＺｒＯ2製ボールメディアで、流速０．２～０．５Ｌ／ｍｉｎのエタノールの溶媒中で３０～１２０分間、上記化合物を混合微粉砕し、同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。Ｘ／Ｙの値を制御するためには、実験的に上記範囲内で粉砕混合条件を変更するか、Ｚｒ化合物の含有量を変更することにより達成できる。
　実施例１～１１については、ｃＢＮ粒子と上記結合材とを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７．０ＧＰａ、温度１６００度で３０分間焼結した。
　実施例１２、１３については、ＲＦスパッタリングＰＶＤ装置を用いて、予めｃＢＮ粒子にそれぞれＴｉＺｒ及びＺｒを平均膜厚３０ｎｍで被覆し、上記と同様の方法で充填、焼結した。
　各実施例及び比較例におけるｃＢＮ焼結体の組成を表１に示す。
（工具の作製）
　得られた焼結体を所定の形状に切断し、超硬合金製工具母材に市販のロウ材を用いて接合し、所定の工具形状に研削加工を施した。
［評価］
（ｃＢＮ焼結体特性の測定）
　上記により得た各実施例及び比較例におけるｃＢＮ焼結体について、焼結体中の任意の直線上のＡｌ2Ｏ3の占める連続した距離の、平均値及び標準偏差を、次に説明する方法により測定した。
　まず、ｃＢＮ焼結体を鏡面研磨して、任意の領域のｃＢＮ焼結体組織を電子顕微鏡にて反射電子像を１００００倍で写真撮影した。組成に対応した濃淡のコントラストが観察され、付属のＥＤＸ（エネルギー分散型Ｘ線分析）により各種元素の重なり状態から化合物を推定した。その結果、黒色領域はｃＢＮ粒子、灰色領域と白色領域は結合相であることが確認された。さらに、濃い灰色領域はＡｌ2Ｏ3であり、濃度の薄い白色領域はＺｒ化合物（酸化物、炭化物、窒化物、硼化物、窒硼化物）であることが特定された。
　次に、同写真に任意の直線を引き、当該直線上における、Ａｌ2Ｏ3とＺｒ化合物との接点の数をＸとし、Ａｌ2Ｏ3とｃＢＮとの接点の数と、Ａｌ2Ｏ3とＡｌ2Ｏ3及びＺｒ化合物以外の結合相成分との接点の数との合計をＹとして、Ｘ／Ｙの値を求めた。
　ここで、当該直線上の接点の合計数は、組織の均一性を考慮し、少なくとも５０点以上となるように直線数を決めた。また、その直線数の直線において、上記Ａｌ2Ｏ3が連続して占める距離（長さ）を測定し、その平均値および標準偏差を求めた。ｃＢＮ含有率は、前記の焼結体組織写真から、ｃＢＮ粒子領域と結合相領域を画像処理により２値化し、ｃＢＮ粒子の占有面積を体積含有率とした。結合相組成に関しては、ＸＲＤ（Ｘ線回折）により同定した。
　Ｚｒ化合物とＴｉ化合物の含有率に関しても、前記の焼結体組織写真の濃淡コントラストから、それぞれの占有面積を画像処理により算出し、体積含有率とした。Ｚｒ化合物の平均粒径に関しては、仕込みの原料粉の平均粒度を記載しており、前記の焼結体組織写真から、概ね、原料粉の粒径を維持していることを確認した。結果を表１に示す。
（切削試験）
　上記で作製した各工具について、以下の条件で切削試験を行った。
被削材　　：　ＦＣ２５０（遠心鋳造鋳鉄スリーブの内径加工、硬度：ＨＢ２３０）
工具形状　：　ＣＮＧＡ１２０４０８
切削条件　：　切削速度　　Ｖｃ＝７００ｍ／ｍｉｎ．
　　　　　　　送り量　　　　ｆ＝０．３ｍｍ／ｒｅｖ．
　　　　　　　切り込み量　ａｐ＝０．０５ｍｍ
　　　　　　　切削液あり
工具寿命　：　逃げ面摩耗量又はチッピングが０．２ｍｍに到達した時点を工具寿命と判断した。
　結果を表２に示す。
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000002
　表２より明らかなように、実施例の工具は、比較例の工具に比し、優れた切削性能を示した。
　以上のように本発明の実施の形態及び実施例について説明を行なったが、今回開示された実施の形態及び実施例はすべての点で例示であって、制限的なものではないと考えられるべきである。本発明の範囲は上記した説明だけではなくて請求の範囲によって示され、請求の範囲と均等の意味及び範囲内でのすべての変更が含まれることが意図される。

Claims (3)

  1. 　立方晶窒化硼素粒子と結合相で構成される立方晶窒化硼素焼結体を少なくとも刃先に有する立方晶窒化硼素焼結体工具であって、
    　前記立方晶窒化硼素焼結体中の立方晶窒化硼素含有率が２０体積％以上６０体積％以下であり、
    　前記結合相に少なくともＡｌ2Ｏ3、及びＺｒ化合物を含み、
    　前記立方晶窒化硼素焼結体中の任意の直線上において、Ａｌ2Ｏ3が占める連続する距離の平均値が０．１μｍ以上１．０μｍ以下であり、かつ該Ａｌ2Ｏ3が占める連続する距離の標準偏差が０．８以下であり、
    　当該直線上において、Ａｌ2Ｏ3とＺｒ化合物との接点の数をＸ、Ａｌ2Ｏ3と立方晶窒化硼素との接点の数と、Ａｌ2Ｏ3とＡｌ2Ｏ3及びＺｒ化合物以外の結合相成分との接点の数との合計をＹとした場合、Ｘ／Ｙが０．１以上１以下であり、
    　Ｚｒ化合物の平均粒径が０．０１μｍ以上０．１μｍ以下である
    ことを特徴とする立方晶窒化硼素焼結体工具。
  2. 　前記立方晶窒化硼素焼結体中に含まれるＺｒ化合物として、ＺｒＣ及びＺｒＯ2を合計で０．５体積％以上５体積％以下含むことを特徴とする請求項１に記載の立方晶窒化硼素焼結体工具。
  3. 　前記立方晶窒化硼素焼結体の任意の直線上において、Ｘ／Ｙが０．５以上０．９以下であることを特徴とする請求項１に記載の立方晶窒化硼素焼結体工具。
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