JP2003081677A - Dispersion-enhanced cbn-based sintered compact and method of producing the same - Google Patents
Dispersion-enhanced cbn-based sintered compact and method of producing the sameInfo
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- JP2003081677A JP2003081677A JP2001272928A JP2001272928A JP2003081677A JP 2003081677 A JP2003081677 A JP 2003081677A JP 2001272928 A JP2001272928 A JP 2001272928A JP 2001272928 A JP2001272928 A JP 2001272928A JP 2003081677 A JP2003081677 A JP 2003081677A
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- Japan
- Prior art keywords
- cbn
- particles
- based sintered
- binder phase
- ultrafine
- Prior art date
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Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、切削工具または耐摩耗
工具として最適な立方晶窒化ホウ素（ＣＢＮ）基焼結体
およびその製造方法に関し、具体的には、ＣＢＮ粒子を
結合するセラミックス成分中に超微粒のＣＢＮ粒子を均
一分散させることにより、耐摩耗性と共に耐欠損性，耐
チッピング性を大幅に向上させた分散強化ＣＢＮ基焼結
体およびその製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a cubic boron nitride (CBN) -based sintered body which is most suitable as a cutting tool or wear resistant tool, and a method for producing the same, and more specifically, to a ceramic component for bonding CBN particles. The present invention relates to a dispersion-strengthened CBN-based sintered body in which abrasion resistance as well as chipping resistance and chipping resistance are significantly improved by uniformly dispersing ultrafine CBN particles into a dispersion and a method for producing the same.
【０００２】[0002]
【従来の技術】ＣＢＮは、ダイヤモンドに次ぐ高い硬度
と優れた熱伝導性を持ち、しかもダイヤモンドに比べて
鉄との親和性が低いという工具材料としての優れた長所
を有している。このＣＢＮとセラミックスや金属の結合
相とでなるＣＢＮ含有焼結体の性能向上についての検討
が多数行われており、その内、焼結体の組織構造から提
案されている代表的なものとして、特開２０００−２１
８４１１号公報，特開２０００−２４７７４６号公報，
特開２０００−４４３４８号公報および特開２０００−
２２６２６３号公報がある。2. Description of the Related Art CBN has an excellent advantage as a tool material that it has the second highest hardness after diamond and excellent thermal conductivity, and that it has a lower affinity for iron than diamond. Many studies have been conducted on the performance improvement of a CBN-containing sintered body composed of CBN and a binder phase of ceramics or a metal, and among them, as a typical one proposed from the structure structure of the sintered body, JP 2000-21
8411, JP 2000-247746 A,
JP-A-2000-44348 and JP-A-2000-
There is 226263 publication.
【０００３】[0003]
【発明が解決しようとする課題】特開２０００−２１８
４１１号公報には、平均粒径１μｍ以下の微粒立方晶窒
化硼素３０〜９０体積％と平均粒径２〜１０μｍの粗粒
立方晶窒化硼素を含有するとともに、残部の結合材の平
均粒径が微粒立方晶窒化硼素＜結合材＜粗粒立方晶窒化
硼素とした立方晶窒化硼素質焼結体切削工具が記載され
ている。また、特開２０００−２４７７４６号公報に
は、平均粒径１μｍ以下の微粒立方晶窒化硼素３０〜９
０体積％と平均粒径２〜１０μｍの粗粒立方晶窒化硼素
を含有するとともに、結合材中にＡｌＮとＡｌ２Ｏ３を
含み、Ｘ線回折測定による周期律表第４ａ，５ａ，６ａ
族元素の硼化物，これら元素の非硼化化合物，立方晶窒
化硼素のピーク強度比を限定した立方晶窒化硼素質焼結
体切削工具が記載されている。DISCLOSURE OF THE INVENTION Problems to be Solved by the Invention
No. 411 gazette contains 30 to 90% by volume of fine-grained cubic boron nitride having an average grain size of 1 μm or less and coarse-grained cubic boron nitride having an average grain size of 2 to 10 μm. A cubic boron nitride sintered body cutting tool is described in which fine-grained cubic boron nitride <bonding material <coarse-grained cubic boron nitride. Further, JP-A-2000-247746 discloses that fine grained cubic boron nitride 30-9 having an average grain size of 1 μm or less.
In addition to containing 0% by volume and coarse-grained cubic boron nitride having an average particle size of 2 to 10 μm, AlN and Al 2 O 3 were contained in the binder, and the periodic table 4a, 5a, 6a by X-ray diffraction measurement was used.
A cutting tool for cubic boron nitride sintered bodies is described in which the peak strength ratios of borides of group elements, non-boriding compounds of these elements, and cubic boron nitride are limited.
【０００４】さらに、特開２０００−４４３４８号公報
には、高圧相窒化ホウ素５０〜８０体積％とチタン化合
物（ＴｉＣ，ＴｉＮ，ＴｉＣＮ）およびアルミニウムか
らなる結合相５０〜２０体積％からなる高硬度焼結体に
おいて、高圧相窒化ホウ素が１〜８μｍの粗粒子６０〜
８０体積％と０．０２〜１μｍの微粒子２０〜４０体積
である鋳鉄切削加工用高硬度焼結体が記載されている。Further, in Japanese Unexamined Patent Publication No. 2000-44348, high-hardness firing consisting of 50 to 80% by volume of high-pressure phase boron nitride and 50 to 20% by volume of a binder phase composed of titanium compounds (TiC, TiN, TiCN) and aluminum. In the aggregate, the high-pressure phase boron nitride contains coarse particles 60 of 1 to 8 μm.
A high-hardness sintered body for cutting cast iron having 80% by volume and 20 to 40 volume of 0.02 to 1 μm fine particles is described.
【０００５】これら３件の公報に記載されているＣＢＮ
基焼結体は、微粒のＣＢＮ粒子を配合することによっ
て、切削時に起こるＣＢＮ粒子の脱落や結合材の摩耗，
脱落による工具摩耗，欠損を防止したものではあるが、
微粒ＣＢＮの配合量が多いあるいは粒径が結合材より著
しく粗大であるために、焼結体の組織中に微粒ＣＢＮの
凝集体を生じ、却って粒子脱落による摩耗やこの凝集体
からの欠損を発生し易いと言う問題がある。CBN described in these three publications
By mixing fine CBN particles in the base sintered body, the CBN particles may fall off during cutting, wear of the binder,
Although it prevents tool wear and chipping due to falling off,
Since the amount of fine CBN is large or the grain size is significantly larger than that of the binder, agglomerates of fine CBN are formed in the structure of the sintered body, which in turn causes wear due to particle loss and defects from this aggregate. There is a problem that it is easy to do.
【０００６】次に、特開２０００−２２６２６３号公報
には、４ａ，５ａ，６ａ族金属の炭化物，窒化物，炭窒
化物および鉄族金属から選ばれる１種以上の微粒子を被
覆した立方晶窒化ホウ素粒子を用いた立方晶窒化ホウ素
複合サーメット工具とその製造方法が記載させている。
本公報に記載されているＣＢＮ焼結体は、ＣＢＮ粒子近
傍での結合材粒子が微細となるために、燒結性の改善、
硬さ向上やＣＢＮ粒子の脱落防止による寿命改善が図れ
るものの、結合材の強度や耐摩耗性の改善が不十分なた
めに性能向上が少ないと言う問題がある。Next, Japanese Patent Laid-Open No. 2000-226263 discloses cubic nitriding coated with one or more kinds of fine particles selected from carbides, nitrides, carbonitrides of group 4a, 5a, and 6a metals. A cubic boron nitride composite cermet tool using boron particles and a method for making the same are described.
In the CBN sintered body described in this publication, since the binder particles in the vicinity of the CBN particles are fine, the sintering property is improved,
Although the hardness can be improved and the life of the CBN particles can be improved by preventing the particles from falling off, there is a problem that the performance improvement is small because the strength and wear resistance of the binder are insufficiently improved.
【０００７】本発明は、上述のような問題点を解決した
もので、具体的には、超微粒ＣＢＮの適量を結合材中に
均一分散させ、結合相を微細組織にすると共に結合材自
体を分散強化することによって、焼結体の硬さ，強度，
靱性を向上させて耐摩耗性，耐欠損性などを大幅に向上
させた分散強化ＣＢＮ基焼結体およびその製造方法の提
供を目的とする。The present invention has solved the above-mentioned problems. Specifically, an appropriate amount of ultrafine CBN is uniformly dispersed in the binder to form a binder phase having a fine structure and the binder itself. By strengthening the dispersion, the hardness, strength, and
An object of the present invention is to provide a dispersion-strengthened CBN-based sintered body having improved toughness and greatly improved wear resistance, fracture resistance and the like, and a method for producing the same.
【０００８】[0008]
【課題を解決するための手段】本発明者らは、ＣＢＮと
結合相とでなる焼結体の耐摩耗性と耐欠損性の同時向上
について検討していたところ、結合相中に超微粒ＣＢＮ
の適量を均一分散させると、燒結中での結合相の粒子成
長が抑制されて結合相が均一微粒な組織となると同時に
超微粒ＣＢＮにより結合相が分散強化されて、強度や靱
性が大幅に向上して耐チッピング性や耐欠損性が改善さ
れること、均一微細に分散した超微粒ＣＢＮは切削時に
脱落し難いために結合相そのものの耐摩耗性が改善され
ること、結合相を分散強化するには、超微粒ＣＢＮと結
合材成分とを予め混合して熱処理し、これを粉砕して分
散強化結合材の微粉末を得た後、通常粒度のＣＢＮ粉と
混合して燒結すれば良いと言う知見を得て、本発明を完
成するに至ったものである。Means for Solving the Problems The inventors of the present invention have studied simultaneous improvement of wear resistance and fracture resistance of a sintered body composed of CBN and a binder phase.
If the appropriate amount of is dispersed uniformly, the grain growth of the binder phase during sintering is suppressed and the binder phase becomes a uniform fine grain structure, and at the same time the binder phase is dispersed and strengthened by the ultrafine CBN, and the strength and toughness are greatly improved. The chipping resistance and chipping resistance are improved, and because the ultrafine CBN particles that are uniformly and finely dispersed are difficult to drop during cutting, the wear resistance of the binder phase itself is improved, and the binder phase is dispersed and strengthened. For this, ultrafine CBN and a binder component are mixed in advance and heat-treated, and this is pulverized to obtain a fine powder of a dispersion-strengthening binder, which is then mixed with CBN powder of a normal grain size and sintered. Based on the knowledge obtained, the present invention has been completed.
【０００９】本発明の分散強化ＣＢＮ基焼結体は、平均
粒子径０．５μｍ以下の超微粒ＣＢＮ粒子１〜２５体積
％と、セラミックス及び／又は鉄族金属を主成とする結
合相５〜６５体積％と、残りが平均粒子径１〜１０μｍ
のＣＢＮ粒子と不可避不純物からなるＣＢＮ基焼結体に
おいて、該超微粒ＣＢＮ粒子は該結合相中に均一分散し
ており、該超微粒ＣＢＮ粒子の該結合相に対する体積割
合が０．１〜１．０であることを特徴とするものであ
る。The dispersion-strengthened CBN-based sintered body of the present invention comprises 1 to 25% by volume of ultrafine CBN particles having an average particle diameter of 0.5 μm or less and a binder phase 5 mainly composed of ceramics and / or iron group metal. 65% by volume and the rest having an average particle size of 1 to 10 μm
In the CBN-based sintered body composed of CBN particles and unavoidable impurities, the ultrafine CBN particles are uniformly dispersed in the binder phase, and the volume ratio of the ultrafine CBN particles to the binder phase is 0.1 to 1. It is characterized by being 0.0.
【００１０】本発明の分散強化ＣＢＮ基焼結体における
超微粒ＣＢＮ粒子は、平均粒子径が０．５μｍを超えて
大きくなると結合相中に均一分散され難くなるために分
散強化の効果がなく、またその含有量が１体積％未満で
は分散粒子が少なくて分散強化による耐摩耗性，耐欠損
性改善の効果がなく、逆に２５体積％を超えて多くなる
と結合相中に凝集体を生じて摩耗，欠損とも増加する。
また、CBN平均粒子径は、0.01μm未満のものを得るには
製造上の困難を伴うため、0.01μm以上であることが実
用上好ましい。The ultrafine CBN particles in the dispersion-strengthened CBN-based sintered body of the present invention have no effect of dispersion strengthening because it becomes difficult to uniformly disperse them in the binder phase when the average particle size increases beyond 0.5 μm. On the other hand, if the content is less than 1% by volume, there are few dispersed particles and there is no effect of improving wear resistance and fracture resistance by dispersion strengthening. Conversely, if it exceeds 25% by volume, aggregates are formed in the binder phase. Both wear and loss increase.
Further, it is practically preferable that the average particle size of CBN be 0.01 μm or more because it is difficult to produce a CBN having an average particle size of less than 0.01 μm.
【００１１】本発明の分散強化ＣＢＮ基焼結体における
超微粒ＣＢＮ粒子は、結合相中に均一分散しており、具
体的には、３個以上の粒子が合体した凝集体を形成して
おらず、ＣＢＮと結合相との接触面積に対するＣＢＮと
ＣＢＮとの接触面積の割合が０．５以下のものである。
また、結合相に対する体積割合（超微粒ＣＢＮ量／結合
相量）は、０．１未満では超微粒ＣＢＮの分散による焼
結時での結合相の粒成長抑制効果が少なくて粗大組織と
なり、また超微粒ＣＢＮの分散強化の効果が少ないため
に耐摩耗性，耐欠損性の改善効果がなく、逆に１．５を
超えて大きくなると結合相中に均一分散し難くなって凝
集体を生じ、耐摩耗性，耐欠損性とも低下するため、
０．１〜１．０に定めた。The ultrafine CBN particles in the dispersion-strengthened CBN-based sintered body of the present invention are uniformly dispersed in the binder phase. Specifically, three or more particles are united to form an aggregate. The ratio of the contact area between CBN and CBN to the contact area between CBN and the binder phase is 0.5 or less.
Further, if the volume ratio to the binder phase (amount of ultrafine CBN / amount of binder phase) is less than 0.1, the grain growth suppressing effect of the binder phase during sintering due to dispersion of the ultrafine CBN is small and a coarse structure is formed. Since the effect of strengthening the dispersion of ultrafine CBN is small, there is no effect of improving wear resistance and fracture resistance. On the contrary, when it exceeds 1.5, it becomes difficult to uniformly disperse in the binder phase, and aggregates are formed. Since both wear resistance and fracture resistance decrease,
It was set to 0.1 to 1.0.
【００１２】本発明の分散強化ＣＢＮ基焼結体における
結合相は、具体的には、ＴｉＣ，ＴｉＮ，ＴｉＮ，Ｔｉ
（ＣＮ），ＺｒＮ，ＨｆＣ，ＮｂＮ，ＴａＣ，ＷＣ，Ｚ
ｒＯ2，ＴｉＢ2，ＭｏＳｉ2などの周期律表第４ａ，５
ａ，６ａ族元素の炭化物，窒化物，酸化物，ホウ化物，
ケイ化物、Ａｌ2Ｏ3，ＡｌＮ，ＡｌＢ12などのアルミニ
ウムの窒化物，酸化物，ホウ化物、ＡｌＣＴｉ2，（Ｔ
ｉＡｌ）Ｎ，ＡｌＢＭｏなどの複合化合物，相互固溶
体、Ｃｏ，Ｎｉ，Ｆｅなどの金属，合金およびこれら金
属と上記化合物との混合物，複合化合物などを上げるこ
とができる。特に、これら結合相の粒度が平均粒径で１
μｍ以下であると、結合相中への超微粒ＣＢＮ粒子の分
散が均一となるので好ましい。また、製造工程での困難
性から、0.02μm以上であることが実用上好ましい。The binder phase in the dispersion-strengthened CBN-based sintered body of the present invention is specifically TiC, TiN, TiN, Ti.
(CN), ZrN, HfC, NbN, TaC, WC, Z
Periodic Table 4a, 5 of rO 2 , TiB 2 , MoSi 2 etc.
Carbides, nitrides, oxides, borides of a and 6a group elements,
Silicides, aluminum nitrides such as Al 2 O 3 , AlN, and AlB 12 , oxides, borides, AlCTi 2 , (T
iAl) N, AlBMo and other complex compounds, mutual solid solutions, metals such as Co, Ni and Fe, alloys and mixtures of these metals with the above compounds, complex compounds and the like can be mentioned. In particular, the average particle size of these binder phases is 1
It is preferable that the particle size is not more than μm because the ultrafine CBN particles are uniformly dispersed in the binder phase. Further, from the viewpoint of difficulty in the manufacturing process, it is practically preferable that the thickness is 0.02 μm or more.
【００１３】本発明の分散強化ＣＢＮ基焼結体における
残りのＣＢＮ粒子は、平均粒子径が１μｍ未満では相対
的に結合相量が不足して燒結し難くなり、逆に１０μｍ
を超えて大きくなるとＣＢＮ粒子同士の接触が強固とな
るために高圧燒結あるいは結合相の増量が必要となる。If the average particle size of the remaining CBN particles in the dispersion-strengthened CBN-based sintered body of the present invention is less than 1 μm, the amount of the binder phase is relatively insufficient and it is difficult to sinter, and conversely 10 μm.
If it exceeds the range, the contact between CBN particles becomes strong, so that high-pressure sintering or an increase in the amount of the binder phase is required.
【００１４】本発明の分散強化ＣＢＮ基焼結体における
超微粒ＣＢＮ粒子は、平均層厚０．０１〜０．２μｍの
ホウ化チタン及び／又は窒化チタンのＴｉ化合物により
囲繞されていると、結合相との接着強度が高まって超微
粒ＣＢＮの脱落摩耗が起こり難くなるので好ましい。Ｔ
ｉ化合物により囲繞は、超微粒ＣＢＮ粒子と結合相成分
粒子が均一分散した混合粉末を燒結する際に、拡散反応
によって超微粒ＣＢＮ粒子の表面に形成されるものであ
る。Ｔｉ化合物層の厚みは、超微粒ＣＢＮ粒子の径を超
えない範囲が好ましい。When the ultrafine CBN particles in the dispersion-strengthened CBN-based sintered body of the present invention are surrounded by a Ti compound of titanium boride and / or titanium nitride having an average layer thickness of 0.01 to 0.2 μm, they are bonded. It is preferable because the adhesive strength with the phase is increased and the falling wear of the ultrafine CBN is less likely to occur. T
The enclosure with the i compound is formed on the surface of the ultrafine CBN particles by a diffusion reaction when sintering the mixed powder in which the ultrafine CBN particles and the binder phase component particles are uniformly dispersed. The thickness of the Ti compound layer is preferably in a range not exceeding the diameter of the ultrafine CBN particles.
【００１５】本発明の分散強化ＣＢＮ基焼結体は、原材
料となる超微粒ＣＢＮ粉末，結合相形成粉末，通常粒子
ＣＢＮ粉末を混合した後、超高圧燒結しても得られる
が、優れた特性，性能を発揮させるには、以下の製造工
程，方法が好ましい。The dispersion-strengthened CBN-based sintered body of the present invention can be obtained by mixing ultrafine CBN powder as a raw material, binder phase forming powder, and normal particle CBN powder, and then sintering by ultrahigh pressure. The following manufacturing steps and methods are preferable for exhibiting the performance.
【００１６】すなわち、本発明の分散強化ＣＢＮ基焼結
体の製造方法は、平均粒径０．５μｍ以下の超微粒ＣＢ
Ｎ粉末と、周期律表第４ａ，５ａ，６ａ族元素の金属，
炭化物，窒化物，酸化物，ホウ化物、アルミニウムの金
属，酸化物，窒化物，ホウ化物，ケイ化物、及び鉄族金
属の中の少なくとも一種以上の結合相形成粉末とを混合
粉砕する第１工程、混合粉末を真空中，７００℃〜１０
００℃で熱処理する第２工程、熱処理した混合粉末を微
粉砕する第３工程、得られた超微粒ＣＢＮ分散の結合相
粉末と場合によっては該結合相形成粉末と、１〜１０μ
ｍＣＢＮ粉末とを混合する第４工程、次いで圧力４〜６
ＧＰａ，温度１４００〜１６００℃の超高圧高温下でも
って焼結する第５工程からなることを特徴とするもので
ある。That is, the method of manufacturing the dispersion-strengthened CBN-based sintered body of the present invention uses ultrafine CB having an average particle size of 0.5 μm or less.
N powder and metal of Group 4a, 5a, 6a group of periodic table,
First step of mixing and pulverizing carbide, nitride, oxide, boride, aluminum metal, oxide, nitride, boride, silicide, and at least one or more binder phase forming powders of iron group metals , Mixed powder in vacuum, 700 ℃ ~ 10
Second step of heat treatment at 00 ° C., third step of pulverizing the heat-treated mixed powder, the obtained ultrafine CBN-dispersed binder phase powder and, if necessary, the binder phase forming powder and 1 to 10 μm
Fourth step of mixing with mCBN powder, then pressure 4-6
It is characterized by comprising a fifth step of sintering under an ultrahigh pressure and high temperature of GPa and a temperature of 1400 to 1600 ° C.
【００１７】本発明の分散強化ＣＢＮ基焼結体の製造方
法における結合相形成粉末は、金属Ａｌと非化学量論組
成からなるＴｉＮX，Ｔｉ（ＣＮ）X（ｘ＝０．６〜０．
９）とを主成分とする混合粉末、もしくは金属Ａｌと金
属Ｃｏとを主成分とする混合粉末が好ましい。The binder phase forming powder in the method for producing the dispersion-strengthened CBN-based sintered body of the present invention comprises TiN x , Ti (CN) x (x = 0.6-0.
A mixed powder containing 9) as a main component or a mixed powder containing metal Al and metal Co as main components is preferable.
【００１８】本発明の分散強化ＣＢＮ基焼結体の製造方
法における第２工程は、結合相成分、例えばＴｉＮとＡ
ｌを反応させて脆性なＴｉ2ＡｌＮなどを生成させ、第
３工程での微粉砕による伴う超微粒ＣＢＮ粒子の結合相
中への均一分散を助長するものである。The second step in the method for producing the dispersion-strengthened CBN-based sintered body of the present invention is the binder phase component such as TiN and A.
1 is reacted to generate brittle Ti 2 AlN or the like, and promotes uniform dispersion of the accompanying ultrafine CBN particles in the binder phase by fine grinding in the third step.
【００１９】[0019]
【作用】本発明の本発明の分散強化ＣＢＮ基焼結体は、
結合相中に分散した超微粒ＣＢＮ粒子が、結合相を微細
組織にすると共に分散強化機構により、結合相の硬さ，
強度，靱性を向上させて耐摩耗性と耐欠損性，耐チッピ
ング性を同時に改善する作用をし、その製造方法は、超
微粒ＣＢＮ粉末と結合相形成粉末との混合物を熱処理し
た後に微粉砕することが、結合相中に超微粒ＣＢＮ粒子
が均一微細に分散させる作用をしている。The operation of the dispersion-strengthened CBN-based sintered body of the present invention is as follows.
The ultrafine CBN particles dispersed in the binder phase make the binder phase into a fine structure and the hardness of the binder phase by the dispersion strengthening mechanism.
It has the effect of improving strength and toughness to simultaneously improve wear resistance, chipping resistance and chipping resistance. The manufacturing method is to heat-treat a mixture of ultrafine CBN powder and binder phase forming powder and then pulverize it. That is, the ultrafine CBN particles have a function of uniformly and finely dispersing in the binder phase.
【００２０】[0020]
【実施例１】平均粒径が０．１μｍのＣＢＮ粉末（ＵＦ
／ＣＢＮと表記），２．０μｍのＣＢＮ粉末（Ｍ／ＣＢ
Ｎと表記）および５．５μｍのＣＢＮ粉末（Ｃ／ＣＢ
Ｎ）、１．１μｍのＴｉＮ0.8粉末、０．９μｍのＡｌ
粉末、０．２μｍのＡｌ2Ｏ3粉末，１〜２μｍのＴｉ
Ｃ，ＨｆＮ，ＴａＣ，ＷＣ，Ｃｏを用いて表１に示す組
成に配合し、これを超硬合金製ボールとメタノール溶媒
を使用したボールミルでもって４８Ｈｒの混合粉砕を行
った後、０．１Ｐａの真空中で表１に併記した温度で
１．０時間の加熱処理し、次いで表１に併記した時間で
もって同様のボールミルによる微粉砕を行って、本発明
に使用する結合相用粉末Ａ〜Ｆを得た。Example 1 CBN powder (UF having an average particle size of 0.1 μm)
/ CBN), 2.0 μm CBN powder (M / CB
N) and 5.5 μm CBN powder (C / CB
N), 1.1 μm TiN 0.8 powder, 0.9 μm Al
Powder, 0.2 μm Al 2 O 3 powder, 1-2 μm Ti
C, HfN, TaC, WC, and Co were blended to the composition shown in Table 1, and this was mixed and pulverized for 48 hours with a ball mill using a cemented carbide ball and a methanol solvent. Powders A to F for the binder phase used in the present invention were obtained by heating in vacuum for 1.0 hour at the temperature shown in Table 1 and then pulverizing with the same ball mill for the time shown in Table 1. Got
【００２１】[0021]
【表１】 [Table 1]
【００２２】次に、結合相用粉末Ａ〜Ｆおよび前述した
各原料粉末を表２に示す組成に配合し、これを超硬合金
製ボールとメタノール溶媒を使用したボールミルでもっ
て２４Ｈｒ（但し、比較品は４８Ｈｒ）の混合とアルゴ
ン中での乾燥して各混合粉末を作製した。これらのプレ
ス成形体を超硬合製の円盤台金上にセットしてカプセル
を構成した後、超高圧高温装置を用いて５．５ＧＰａの
圧力、１５００℃の温度、３０分の保持時間の条件でも
って焼結し、本発明品１〜７および比較品１〜７を得
た。Next, the binder phase powders A to F and the above-mentioned respective raw material powders were blended in the composition shown in Table 2, and this was mixed with a cemented carbide ball and a ball mill using a methanol solvent for 24 hours (however, in comparison. The product was mixed for 48 hours and dried in argon to prepare each mixed powder. These press-formed bodies were set on a disc base metal made of cemented carbide to form capsules, and then a pressure of 5.5 GPa, a temperature of 1500 ° C., and a holding time of 30 minutes were used by using an ultra-high pressure and high temperature apparatus. Then, the products of the present invention 1 to 7 and comparative products 1 to 7 were obtained by sintering.
【００２３】[0023]
【表２】 [Table 2]
【００２４】こうして得た本発明品１〜７および比較品
１〜７の各ＣＢＮ基焼結体を放電加工による切断とダイ
ヤモンドによる研削、ラップ加工して測定用試料を作製
した。まず、ヌープ硬さおよびビッカース圧痕法による
破壊靱性値の測定結果を表２に併記した。次に、電界放
射型分析電顕を用いて、結合相中での超微粒ＣＢＮの分
散状態、分散量と結合相に対する体積割合、平均粒子
径、囲繞されたＴｉ化合物の平均厚みおよび結合相の平
均粒子径などを測定した（破面観察からも確認した）。
これらの結果を表３に示す。The CBN-based sintered bodies of the present invention products 1 to 7 and comparative products 1 to 7 thus obtained were cut by electric discharge machining, ground by diamond, and lapped to prepare samples for measurement. First, Table 2 also shows the measurement results of the fracture toughness values by the Knoop hardness and the Vickers indentation method. Next, using a field emission analytical electron microscope, the dispersion state of the ultrafine CBN in the binder phase, the dispersion amount and the volume ratio to the binder phase, the average particle diameter, the average thickness of the enclosed Ti compound and the binder phase The average particle diameter and the like were measured (confirmed by observing the fracture surface).
The results are shown in Table 3.
【００２５】[0025]
【表３】 [Table 3]
【００２６】[0026]
【実施例２】実施例１で得られた本発明品１〜６および
比較品１〜６の各焼結体を放電加工による切断、超硬合
金製チップ台金へのロー付け、ダイヤモンド砥石による
研削加工を経て、切削試験用チップ形状：ＴＮＭＡ１６
０４０８を作製した。そして、下記条件による切削試験
を行い、その結果を表４に示した。
（Ａ）外周連続乾式切削 被削材：ＳＣＭ４１５（ＨＲ
Ｃ６０．９〜６１．７）、切削速度：１５０ｍ／ｍｉ
ｎ、切込み量：０．５ｍｍ、送り量：０．１ｍｍ／ｒｅ
ｖ、評価基準：平均逃げ面摩耗量ＶＢ＝０．２ｍｍとな
るまたは途中欠損までの切削時間
（Ｂ）外周連続湿式切削 被削材：ＦＣ３０（ＨＢ２１
０〜２３０）、切削速度：５００ｍ／ｍｉｎ、切込み
量：０．５ｍｍ、送り量：０．１５ｍｍ／ｒｅｖ、評価
基準：平均逃げ面摩耗量ＶＢ＝０．２ｍｍになるまたは
途中欠損までの切削時間
（Ｃ）外周連続湿式切削 被削材：インコネル７１８、
切削速度：１２０ｍ／ｍｉｎ、切込み量：０．３ｍｍ、
送り量：０．１０ｍｍ／ｒｅｖ、評価基準：境界摩耗量
ＶＮ＝０．３ｍｍになるまでの切削時間[Embodiment 2] Each of the sintered bodies of the present invention products 1 to 6 and comparative products 1 to 6 obtained in the embodiment 1 is cut by electric discharge machining, brazed to a cemented carbide chip base metal, and diamond diamond is used. After grinding, cutting test tip shape: TNMA16
0408 was prepared. Then, a cutting test was conducted under the following conditions, and the results are shown in Table 4. (A) Peripheral continuous dry cutting Work material: SCM415 (HR
C60.9-61.7), cutting speed: 150 m / mi
n, depth of cut: 0.5 mm, feed: 0.1 mm / re
v, evaluation criteria: average flank wear amount VB = 0.2 mm or cutting time until intermediate fracture (B) outer peripheral continuous wet cutting Work material: FC30 (HB21
0-230), cutting speed: 500 m / min, depth of cut: 0.5 mm, feed rate: 0.15 mm / rev, evaluation standard: average flank wear amount VB = 0.2 mm or cutting time until midway fracture (C) Peripheral continuous wet cutting Work material: Inconel 718,
Cutting speed: 120 m / min, Depth of cut: 0.3 mm,
Feed rate: 0.10 mm / rev, Evaluation criteria: Boundary wear amount VN = Cutting time until reaching 0.3 mm
【００２７】[0027]
【表４】 [Table 4]
───────────────────────────────────────────────────── フロントページの続き Ｆターム(参考） 4G001 BA03 BA12 BA24 BA34 BA36 BA37 BA41 BA43 BA48 BA61 BA63 BB03 BB12 BB24 BB34 BB37 BB43 BB48 BB61 BC13 BC43 BC52 BC54 BD12 BD16 BD18 ─────────────────────────────────────────────────── ─── Continued front page F-term (reference) 4G001 BA03 BA12 BA24 BA34 BA36 BA37 BA41 BA43 BA48 BA61 BA63 BB03 BB12 BB24 BB34 BB37 BB43 BB48 BB61 BC13 BC43 BC52 BC54 BD12 BD16 BD18
Claims (5)
粒子１〜２５体積％と、セラミックス及び／又は鉄族金
属を主成分とする結合相５〜６５体積％と、残りが平均
粒子径１〜１０μｍのＣＢＮ粒子と不可避不純物からな
るＣＢＮ基焼結体において、該超微粒ＣＢＮ粒子は該結
合相中に均一分散しており、該超微粒ＣＢＮ粒子の該結
合相に対する体積割合が０．１〜１．０であることを特
徴とする分散強化ＣＢＮ基焼結体。1. Ultrafine CBN particles having an average particle diameter of 0.5 μm or less.
1 to 25% by volume of particles, 5 to 65% by volume of a binder phase containing ceramics and / or an iron group metal as a main component, and the rest of the CBN-based sintered body consisting of CBN particles having an average particle size of 1 to 10 μm and inevitable impurities. In, the ultrafine CBN particles are uniformly dispersed in the binder phase, and the volume ratio of the ultrafine CBN particles to the binder phase is 0.1 to 1.0. Sintered body.
ることを特徴とする請求項１記載の分散強化ＣＢＮ基焼
結体。2. The dispersion-strengthened CBN-based sintered body according to claim 1, wherein the binder phase has an average particle diameter of 1 μm or less.
ａ族元素の炭化物，窒化物，酸化物，ホウ化物，ケイ化
物、アルミニウムの窒化物，酸化物，ホウ化物、並びに
これらの複合化合物，相互固溶体、及び鉄族金属の中の
少なくとも一種以上からなることを特徴とする請求項１
又は２記載の分散強化ＣＢＮ基焼結体。3. The bonding phase is represented by Periodic Table Nos. 4a, 5a, 6
Consists of at least one or more of a-group element carbides, nitrides, oxides, borides, silicides, aluminum nitrides, oxides, borides, and their complex compounds, mutual solid solutions, and iron group metals. Claim 1 characterized by the above.
Alternatively, the dispersion-strengthened CBN-based sintered body according to item 2.
１〜０．２μｍのホウ化チタン及び／又は窒化チタンの
Ｔｉ化合物により囲繞されていることを特徴とする請求
項１，２又は３記載の分散強化ＣＢＮ基焼結体。4. The ultrafine CBN particles have an average layer thickness of 0.0.
The dispersion-strengthened CBN-based sintered body according to claim 1, wherein the dispersion-strengthened CBN-based sintered body is surrounded by a Ti compound of 1 to 0.2 μm of titanium boride and / or titanium nitride.
末と、周期律表第４ａ，５ａ，６ａ族元素の金属，炭化
物，窒化物，酸化物，ホウ化物、アルミニウムの金属，
酸化物，窒化物，ホウ化物，ケイ化物、及び鉄族金属の
中の少なくとも一種以上の結合相形成粉末とを混合粉砕
する第１工程、混合粉末を真空中，７００℃〜１０００
℃で熱処理する第２工程、熱処理した混合粉末を微粉砕
する第３工程、得られた超微粒ＣＢＮ分散粉末と場合に
よっては該結合相形成粉末と、１〜１０μｍＣＢＮ粉末
とを混合する第４工程、次いで圧力４〜６ＧＰａ，温度
１４００〜１６００℃の超高圧高温下でもって焼結する
第５工程からなることを特徴とする分散強化ＣＢＮ基焼
結体の製造方法。5. An ultrafine CBN powder having an average particle size of 0.5 μm or less, and metals, carbides, nitrides, oxides, borides, aluminum metals of elements of groups 4a, 5a and 6a of the periodic table,
First step of mixing and pulverizing oxide, nitride, boride, silicide, and at least one or more binder phase forming powders of iron group metal, the mixed powder in vacuum at 700 ° C to 1000 ° C
Second step of heat treatment at 0 ° C, third step of finely pulverizing the heat-treated mixed powder, fourth step of mixing the obtained ultrafine CBN dispersed powder and optionally the binder phase forming powder and 1-10 µm CBN powder And a fifth step of sintering at a pressure of 4 to 6 GPa and a temperature of 1400 to 1600 ° C. under an ultrahigh pressure and high temperature.
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| JP2006137623A (en) * | 2004-11-10 | 2006-06-01 | Tungaloy Corp | Cubic boron nitride sintered body, coated cubic boron nitride sintered body and their manufacturing methods |
| JP5298372B2 (en) * | 2006-06-12 | 2013-09-25 | 住友電工ハードメタル株式会社 | Composite sintered body |
| JP2016520030A (en) * | 2013-04-30 | 2016-07-11 | エレメント シックス リミテッド | PCBN material, method for making it, tool including it, and method of using the same |
| CN113321504A (en) * | 2021-07-06 | 2021-08-31 | 中国有色桂林矿产地质研究院有限公司 | Zirconia toughened alumina ceramic material and preparation method and application thereof |
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| JPH10245287A (en) * | 1997-03-04 | 1998-09-14 | Nof Corp | Hard layer-coated high pressure phase boron nitride sinter compact for cutting tool |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006137623A (en) * | 2004-11-10 | 2006-06-01 | Tungaloy Corp | Cubic boron nitride sintered body, coated cubic boron nitride sintered body and their manufacturing methods |
| JP5298372B2 (en) * | 2006-06-12 | 2013-09-25 | 住友電工ハードメタル株式会社 | Composite sintered body |
| US8999023B2 (en) | 2006-06-12 | 2015-04-07 | Sumitomo Electric Hardmetal Corp. | Composite sintered body |
| US10307829B2 (en) | 2006-06-12 | 2019-06-04 | Sumitomo Electric Hardmetal Corp. | Composite sintered body |
| JP2016520030A (en) * | 2013-04-30 | 2016-07-11 | エレメント シックス リミテッド | PCBN material, method for making it, tool including it, and method of using the same |
| CN113321504A (en) * | 2021-07-06 | 2021-08-31 | 中国有色桂林矿产地质研究院有限公司 | Zirconia toughened alumina ceramic material and preparation method and application thereof |
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