JPH05301776A - Cubic boron nitride-based sintered compact - Google Patents
Cubic boron nitride-based sintered compactInfo
- Publication number
- JPH05301776A JPH05301776A JP4108286A JP10828692A JPH05301776A JP H05301776 A JPH05301776 A JP H05301776A JP 4108286 A JP4108286 A JP 4108286A JP 10828692 A JP10828692 A JP 10828692A JP H05301776 A JPH05301776 A JP H05301776A
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- cubic boron
- boron nitride
- nitride
- sintered body
- cutting
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Abstract
Description
【0001】[0001]
【産業上の利用分野】本発明は、例えば、切削工具等に
使用される高硬度,高靱性に優れた立方晶窒化硼素質焼
結体に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a cubic boron nitride sintered body which is used, for example, in a cutting tool and has excellent hardness and toughness.
【0002】[0002]
【従来技術】立方晶窒化硼素(Cubic Boron Nitride 以
下cBNと略す)はダイヤモンドに次ぐ高硬度を有し、
しかもダイヤモンドと異なり、鉄系金属との親和性を持
たないため、特に鉄系高硬度材の加工に用いられてい
る。2. Description of the Related Art Cubic Boron Nitride (hereinafter abbreviated as cBN) has the highest hardness next to diamond,
Moreover, unlike diamond, it has no affinity with iron-based metals, so it is used especially in the processing of iron-based high hardness materials.
【0003】このようなcBNを使用した切削工具とし
ては、cBNをコバルト(Co)等の金属で結合したも
のや、窒化チタン(TiN)等のセラミックスで結合し
た立方晶窒化硼素質焼結体が用いられている(特公昭5
2−43846号公報等参照)。As a cutting tool using such cBN, there are a cBN bonded with a metal such as cobalt (Co) and a cubic boron nitride sintered body bonded with a ceramic such as titanium nitride (TiN). It has been used (Japanese Patent Publication Sho 5)
2-43846 gazette etc.).
【0004】[0004]
【発明が解決しようとする問題点】しかしながら、この
ようなCoやTiNを結合材に用いた立方晶窒化硼素質
焼結体では、BNがCoやTiNと反応し、Co21W2
B6 ,TiB2 等の硼素化合物をいずれも含有してい
る。この硼素化合物は、高硬度であるが非常に脆い物質
であるため、焼結体の靱性を損なう。そのため、これま
での立方晶窒化硼素質焼結体を用いた切削工具は、特に
断続切削,重切削のような靱性を要求される用途に対し
ては、未だに満足する性能を得ることができなかった。However, in such a cubic boron nitride sintered body using Co or TiN as a binder, BN reacts with Co or TiN, and Co 21 W 2
It contains boron compounds such as B 6 and TiB 2 . Since this boron compound has a high hardness but is a very brittle substance, it impairs the toughness of the sintered body. Therefore, the cutting tools using the cubic boron nitride sintered material up to now cannot obtain satisfactory performance, especially for applications requiring toughness such as intermittent cutting and heavy cutting. It was
【0005】[0005]
【問題点を解決するための手段】本発明者は、立方晶窒
化硼素質焼結体の靱性を向上すべく鋭意研究した結果、
BNと結合材との反応生成相として脆い硼素化合物が生
成しないように、特定の結合材を選択すると、靱性が大
幅に向上することを見出し、本発明に至った。[Means for Solving the Problems] The inventors of the present invention have conducted extensive studies to improve the toughness of a cubic boron nitride sintered body, and as a result,
The inventors have found that when a specific binder is selected so that a brittle boron compound is not formed as a reaction product phase of BN and the binder, the toughness is significantly improved, and the present invention has been completed.
【0006】即ち、本発明の立方晶窒化硼素質焼結体
は、立方晶窒化硼素を30〜85体積%含有し、残部が
窒化珪素,窒化アルミニウム,酸化アルミニウム,酸化
珪素の混合物もしくは化合物からなるものである。この
際には、残部の化合物がSi,Al,O,Nを含むサイ
アロン結晶を主体とするものが望ましい。That is, the cubic boron nitride sintered body of the present invention contains 30 to 85% by volume of cubic boron nitride, and the balance is a mixture or compound of silicon nitride, aluminum nitride, aluminum oxide and silicon oxide. It is a thing. In this case, it is desirable that the remaining compound is mainly composed of a sialon crystal containing Si, Al, O and N.
【0007】また、立方晶窒化硼素を30〜85体積%
含有し、残部が窒化珪素と窒化アルミニウムと希土類金
属酸化物との混合物もしくは化合物からなるものであ
る。この際には、残部の化合物がSi,Al,O,Nお
よび希土類金属元素を含むサイアロン結晶を主体とする
か、或いは、これと窒化珪素結晶を主体とするものが望
ましい。この場合にはαサイアロンを生成する。Further, cubic boron nitride is added in an amount of 30 to 85% by volume.
It is contained and the balance consists of a mixture or compound of silicon nitride, aluminum nitride and a rare earth metal oxide. At this time, it is preferable that the remaining compound is mainly composed of a sialon crystal containing Si, Al, O, N and a rare earth metal element, or mainly composed of this and a silicon nitride crystal. In this case, α sialon is produced.
【0008】立方晶窒化硼素を30〜85体積%含有さ
せたのは、cBN本来の特性を生かすためには、焼結体
中のcBNの含有率が30体積%以上必要だからであ
り、30体積%より少ないと、焼結体の硬度が低下し、
耐磨耗性能を損なうからである。また、85体積%を越
えると、硬度は高いものの靱性が低下し、実用に耐えな
くなってしまうからである。The cubic boron nitride is contained in an amount of 30 to 85% by volume because the content of cBN in the sintered body must be 30% by volume or more in order to utilize the original characteristics of cBN. %, The hardness of the sintered body decreases,
This is because the abrasion resistance is impaired. On the other hand, if it exceeds 85% by volume, the hardness is high, but the toughness is lowered, and it becomes unusable for practical use.
【0009】また、立方晶窒化硼素の残部を窒化珪素,
窒化アルミニウム,酸化アルミニウム,酸化珪素の混合
物或いは化合物により構成したのは、これらがBNと反
応することがなく、脆い硼素化合物を生成することがな
いからである。残部を構成する化合物としては、Si
6-x Alx Ox N8-x ( 0<X≦4.2)またはSi6-
x Alx+Y Ox N8-x+Y (0<X<6、2≦Y≦12)
主体とすることが望ましい。The remaining portion of the cubic boron nitride is silicon nitride,
The reason why it is composed of a mixture or compound of aluminum nitride, aluminum oxide and silicon oxide is that they do not react with BN and do not form a brittle boron compound. The compound constituting the balance is Si
6-x Al x O x N 8-x (0 <X ≦ 4.2) or Si 6-
x Al x + Y O x N 8-x + Y (0 <X <6, 2 ≦ Y ≦ 12)
It is desirable to be the subject.
【0010】残部が、Si6-x Alx Ox N8-x を主体
とするものである場合において、X値を0<X≦4.2
に限定したのは、X値を上記の範囲に限定したものはい
ずれも硬度,靱性に特に優れているからである。また、
残部がSi6-x Alx+Y OxN8-x+Y を主体とするもの
である場合、X値やY値を、0<X≦6、2≦Y≦12
と限定したのは、X値やY値を上記の範囲に限定したも
のはいずれも硬度,靱性に特に優れているからである。In the case where the balance consists mainly of Si 6-x Al x O x N 8-x , the X value is 0 <X≤4.2.
The reason for limiting the X value to the above range is that all of them are particularly excellent in hardness and toughness. Also,
When the balance is mainly composed of Si 6-x Al x + Y O x N 8-x + Y , the X value and the Y value are 0 <X ≦ 6, 2 ≦ Y ≦ 12.
The reason for limiting the X value and the Y value to the above ranges is that they are particularly excellent in hardness and toughness.
【0011】さらに、残部を窒化珪素と窒化アルミニウ
ムと希土類金属酸化物とから構成したのは、これらも硼
素化合物を生成することがなく、また、特に希土類金属
を含むことにより、結合相自体が高強度高硬度で耐熱性
に優れたものとなるために、焼結体全体の特性を高める
ことができるからである。この発明における残部の化合
物は、Mx ( Si, Al) 12( O, N) 16(ただし、M
は希土類金属元素,0<X≦2)を主体とするか、或い
はこれと窒化珪素を主体とするものが望ましい。ここ
で、0<X≦2としたのは、この範囲内だと硬度,靱性
に特に優れているからである。尚、本発明で用いられる
希土類金属としては、Sc,Y,La,Ce,Pr,N
d,Sm,Gd,Tb,Dy,Ho,Er,Yb等があ
る。Further, since the balance is composed of silicon nitride, aluminum nitride and rare earth metal oxide, these also do not produce a boron compound, and the binder phase itself is high because it contains a rare earth metal in particular. This is because the strength of the sintered body is high and the heat resistance is excellent, so that the characteristics of the entire sintered body can be improved. The remaining compound in the present invention is M x (Si, Al) 12 (O, N) 16 (provided that M x
Is preferably a rare earth metal element, 0 <X ≦ 2) as a main component, or a substance mainly containing this and silicon nitride. Here, 0 <X ≦ 2 is set because the hardness and toughness are particularly excellent in this range. The rare earth metals used in the present invention include Sc, Y, La, Ce, Pr and N.
d, Sm, Gd, Tb, Dy, Ho, Er, Yb, etc.
【0012】本発明の立方晶窒化硼素質焼結体は、金属
粉末を添加しないことに特徴がある。即ち、従来、cB
Nの焼結に際しては、Al等の金属元素を助剤として添
加することが広く行われているが、本発明においてはそ
のような金属元素の添加は不必要である。むしろ、Al
等の金属元素を助剤として添加すると結合相中からSi
が析出し、焼結体の特性、即ち、靱性や強度等が低下す
る結果となるからである。よって、本発明の立方晶窒化
硼素質焼結体によれば、AlやSi等の金属が実質的に
存在しないことも大きな特徴である。The cubic boron nitride sintered body of the present invention is characterized in that no metal powder is added. That is, conventionally, cB
When sintering N, it is widely practiced to add a metal element such as Al as an auxiliary agent, but the addition of such a metal element is unnecessary in the present invention. Rather, Al
When a metal element such as Si is added as an auxiliary agent, Si is added from the binder phase.
Is deposited, resulting in deterioration of the properties of the sintered body, that is, toughness, strength and the like. Therefore, according to the cubic boron nitride sintered body of the present invention, it is also a great feature that metals such as Al and Si are substantially absent.
【0013】本発明の立方晶窒化硼素質焼結体の製造方
法としては、原料粉末としてcBN粉末、その他所望の
Si3 N4 ,AlN,Al2 O3 ,SiO2 ,Li
2 O,CaO,Y2 O3 ,希土類元素酸化物等を準備
し、これらを前述した特定の組成に秤量し、充分に混合
する。その後、混合粉末を所定形状に成形する。成形手
段としてはプレス成形,射出成形,鋳込み成形,押出成
形等周知の成形手段を用いることができる。As the method for producing the cubic boron nitride sintered body of the present invention, the raw material powder is cBN powder, and other desired Si 3 N 4 , AlN, Al 2 O 3 , SiO 2 , Li.
2 O, CaO, Y 2 O 3 , rare earth element oxides, etc. are prepared, weighed to the specific composition described above, and mixed sufficiently. Then, the mixed powder is molded into a predetermined shape. As the molding means, known molding means such as press molding, injection molding, casting molding, extrusion molding can be used.
【0014】次に上記成形体を高温高圧発生装置を用い
て、例えば、特公昭39−8948に開示されるように
高温高圧で焼結する。即ち、圧力3.5〜6GPa、温
度1300〜1800℃で15〜120分間保持し、本
発明の立方晶窒化硼素質焼結体を得る。Next, the above-mentioned compact is sintered using a high temperature and high pressure generator at high temperature and high pressure as disclosed in, for example, Japanese Patent Publication No. 39-8948. That is, the cubic boron nitride sintered material of the present invention is obtained by holding at a pressure of 3.5 to 6 GPa and a temperature of 1300 to 1800 ° C. for 15 to 120 minutes.
【0015】[0015]
【作用】本発明の立方晶窒化硼素質焼結体では、BNと
反応しない結合材を使用しているので硼素化合物が生成
せず、このため、焼結体の靱性が向上し、例えば、これ
を切削工具として使用した場合、断続切削,重切削にお
ける性能を大幅に向上することができる。さらに、結合
相として、窒化珪素と窒化アルミニウムと希土類金属酸
化物を使用することにより、硼素化合物が生成せずに靱
性が向上するとともに、結合相自体としても高強度高硬
度で耐熱性に優れるため、さらに優れた特性を有する焼
結体を得ることができ、切削時における性能を従来より
も大幅に向上することができる。In the cubic boron nitride sintered body of the present invention, since a binder that does not react with BN is used, no boron compound is generated, which improves the toughness of the sintered body. When used as a cutting tool, the performance in intermittent cutting and heavy cutting can be greatly improved. Furthermore, since silicon nitride, aluminum nitride, and a rare earth metal oxide are used as the binder phase, the toughness is improved without forming a boron compound, and the binder phase itself has high strength, high hardness, and excellent heat resistance. Further, it is possible to obtain a sintered body having further excellent characteristics, and it is possible to significantly improve the performance during cutting as compared with the conventional case.
【0016】[0016]
実施例1 原料粉末として、cBN(平均結晶粒径2〜4μm),
及びSi3 N4 ,Al2 O3 ,AlN,SiO2 粉末を
用い、これらを表1に示す割合で秤量混合して所定形状
に成形し、この後、超高圧高温発生装置を用いて、表1
に示す圧力、温度で所定時間保持し、焼成した。Example 1 As a raw material powder, cBN (average crystal grain size 2 to 4 μm),
And Si 3 N 4 , Al 2 O 3 , AlN, and SiO 2 powders, which are weighed and mixed at a ratio shown in Table 1 to form a predetermined shape, and thereafter, an ultrahigh pressure and high temperature generator is used to 1
The pressure and temperature shown in (1) were maintained for a predetermined period of time and baked.
【0017】[0017]
【表1】 [Table 1]
【0018】そして、立方晶窒化硼素質焼結体を取り出
し鏡面加工し、SEM(走査型電子顕微鏡)により組織
観察をしたところ、ポアのない緻密な組織を示した。Then, the cubic boron nitride sintered body was taken out, mirror-polished, and microscopically observed by SEM (scanning electron microscope). As a result, a dense structure without pores was shown.
【0019】また、得られた焼結体に対してビッカース
硬度、ビッカース硬度用ダイヤモンド圧子を用いて荷重
20kgで圧痕法により破壊靱性を測定した。さらに、
X線回折法により結晶相を調べた。The fracture toughness of the obtained sintered body was measured by the indentation method with a Vickers hardness and a Vickers hardness diamond indenter at a load of 20 kg. further,
The crystal phase was examined by the X-ray diffraction method.
【0020】そして、各試料を用いて下記に示す切削条
件で乾式断続切削試験を行った。Then, a dry interrupted cutting test was performed on each sample under the following cutting conditions.
【0021】(断続切削試験) 被削材 SKD11(HRC60.5mm幅、4本
溝入り) 切削速度 100m/min 切り込み 0.2mm 送り 0.1mm/rev 切削時間 5min 上記の実験結果を表2に示す。(Intermittent cutting test) Work material SKD11 (H RC 60.5 mm width, with 4 grooves) Cutting speed 100 m / min Cutting depth 0.2 mm Feed 0.1 mm / rev Cutting time 5 min The above experimental results are shown in Table 2 Shown in.
【0022】[0022]
【表2】 [Table 2]
【0023】尚、この表2において、切削試験結果は、
5分間断続切削しても欠損しない場合を○、欠損した場
合を×とした。In Table 2, the cutting test results are
When there was no defect even after intermittent cutting for 5 minutes, it was evaluated as ◯, and when it was damaged, it was evaluated as x.
【0024】表1及び表2により、本発明の立方晶窒化
硼素質焼結体は、硬度が2300以上で、靱性が6.4
MPa・m1/2 以上であった。また、5分間断続切削し
ても欠損しなかった。これに対して、試料No,9は硼素
化合物が生じており、硬度,靱性が低く、欠損が生じ
た。尚、試料No,8の結晶相は同定することができなか
った。According to Tables 1 and 2, the cubic boron nitride sintered body of the present invention has a hardness of 2300 or more and a toughness of 6.4.
It was at least MPa · m 1/2 . In addition, there was no loss even after intermittent cutting for 5 minutes. On the other hand, in the samples No. 9 and 9, the boron compound was generated, the hardness and toughness were low, and defects were generated. The crystal phase of sample No. 8 could not be identified.
【0025】実施例2 原料粉末として、cBN(平均結晶粒径2〜4μm),
及びSi3 N4 ,Al2 O3 ,AlN,SiO2 粉末
と、Er2 O3 ,Yb2 O3 ,Y2 O3 を含有する粉末
を表3に示す割合で秤量混合し、これらを所定形状に成
形後、超高圧高温発生装置を用いて、表3に示す圧力、
温度で所定時間保持し、焼成した。Example 2 As raw material powder, cBN (average crystal grain size 2 to 4 μm),
And Si 3 N 4, Al 2 O 3, AlN, and SiO 2 powder, the powder containing Er 2 O 3, Yb 2 O 3, Y 2 O 3 were weighed in a ratio shown in Table 3, these predetermined After forming into a shape, using an ultrahigh pressure and high temperature generator, the pressure shown in Table 3
The temperature was maintained for a predetermined period of time and the firing was performed.
【0026】[0026]
【表3】 [Table 3]
【0027】そして、立方晶窒化硼素質焼結体を取り出
し鏡面加工し、実施例1と同様に組織観察をしたとこ
ろ、ポアのない緻密な組織を示した。Then, the cubic boron nitride sintered body was taken out and subjected to mirror finishing, and the structure was observed in the same manner as in Example 1. As a result, a dense structure without pores was shown.
【0028】また、得られた焼結体に対して、実施例1
と同様に、ビッカース硬度,破壊靱性を測定し、結晶相
を調べた。In addition, for the obtained sintered body, Example 1
Similarly to, the Vickers hardness and the fracture toughness were measured and the crystal phase was examined.
【0029】そして、各試料を用いて下記に示す切削条
件で乾式断続切削試験を行った。Then, a dry interrupted cutting test was performed on each sample under the following cutting conditions.
【0030】(断続切削試験) 被削材 SKD11(HRC60.5mm幅、4本
溝入り) 切削速度 100m/min 切り込み 0.2mm 送り 0.1mm/rev 切削時間 5min 上記の結果を表4に示す。(Intermittent cutting test) Work material SKD11 (H RC 60.5 mm width, with 4 grooves) Cutting speed 100 m / min Cutting depth 0.2 mm Feed 0.1 mm / rev Cutting time 5 min The above results are shown in Table 4. Show.
【0031】[0031]
【表4】 [Table 4]
【0032】表3及び表4により、本発明の立方晶窒化
硼素質焼結体は、硬度が2350以上で、靱性が6.9
以上であった。これに対して、試料No,15は、切削試
験において欠損しなかったが、磨耗のため、1分間で切
削できなくなった。また、試料No,18は硼素化合物が
生じており、硬度,靱性が低く、欠損が生じた。尚、試
料No,17の結晶相は同定することができなかった。From Tables 3 and 4, the cubic boron nitride sintered body of the present invention has a hardness of 2350 or more and a toughness of 6.9.
That was all. On the other hand, Sample No. 15 was not broken in the cutting test, but could not be cut in 1 minute due to abrasion. Further, Samples No. 18 and 18 had a boron compound, which had low hardness and toughness, and had a defect. The crystal phase of sample No. 17 could not be identified.
【0033】[0033]
【発明の効果】以上詳述した通り、本発明によれば、結
合材がBNと反応することなく、高硬度および高靱性を
有することにより、例えば、断続切削,重切削における
性能を大幅に向上することができる。また、結合材中の
1成分として希土類金属酸化物をさらに使用することに
より、結合材の強度硬度および耐熱性を向上することが
でき、これにより、切削時における性能を従来よりも大
幅に向上することができる。As described in detail above, according to the present invention, since the binder does not react with BN and has high hardness and high toughness, the performance in, for example, interrupted cutting and heavy cutting is significantly improved. can do. Further, by further using a rare earth metal oxide as one component in the binder, it is possible to improve the strength and hardness and heat resistance of the binder, thereby significantly improving the performance during cutting as compared with the conventional case. be able to.
Claims (4)
し、残部が窒化珪素,窒化アルミニウム,酸化アルミニ
ウム,酸化珪素の混合物もしくはそれらの化合物からな
ることを特徴とする立方晶窒化硼素質焼結体。1. A cubic boron nitride calcined material containing 30 to 85% by volume of cubic boron nitride, and the balance consisting of a mixture of silicon nitride, aluminum nitride, aluminum oxide, silicon oxide or a compound thereof. Union.
サイアロン結晶を主体とするものからなる請求項1記載
の立方晶窒化硼素質焼結体。2. The cubic boron nitride sintered body according to claim 1, wherein the remaining compound is mainly composed of a sialon crystal containing Si, Al, O, and N.
し、残部が窒化珪素と窒化アルミニウムと希土類金属酸
化物との混合物もしくは化合物からなることを特徴とす
る立方晶窒化硼素質焼結体。3. A cubic boron nitride sintered body containing 30 to 85% by volume of cubic boron nitride, and the balance being a mixture or compound of silicon nitride, aluminum nitride and a rare earth metal oxide. ..
希土類金属元素を含むサイアロン結晶を主体とすること
を特徴とする請求項3記載の立方晶窒化硼素質焼結体。4. The cubic boron nitride sintered body according to claim 3, wherein the remaining compound is mainly composed of a sialon crystal containing Si, Al, O, N and a rare earth metal element.
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JP2008121046A (en) * | 2006-11-09 | 2008-05-29 | Mitsubishi Materials Corp | High hardness high density cubic boron nitride based sintered body and method for producing the same |
JP2011116597A (en) * | 2009-12-04 | 2011-06-16 | Sumitomo Electric Ind Ltd | Sintered compact and rotating tool |
KR20110066939A (en) * | 2008-09-17 | 2011-06-17 | 다이아몬드 이노베이션즈, 인크. | Cubic Boron Nitride Ceramic Composites and Method for Producing the Same |
JP2011140414A (en) * | 2010-01-06 | 2011-07-21 | Sumitomo Electric Ind Ltd | Sintered compact and cutting tool using the sintered compact |
JP2011140415A (en) * | 2010-01-06 | 2011-07-21 | Sumitomo Electric Ind Ltd | Sintered compact and cutting tool using the sintered compact |
JP2014144911A (en) * | 2014-03-06 | 2014-08-14 | Sumitomo Electric Ind Ltd | Sintered body and cutting tool obtained by using the sintered body |
WO2016063769A1 (en) * | 2014-10-23 | 2016-04-28 | 住友電気工業株式会社 | Sintered compact |
JP2016522142A (en) * | 2013-04-30 | 2016-07-28 | エレメント シックス リミテッド | COMPOSITE MATERIAL, ARTICLE CONTAINING THE SAME, AND METHOD FOR MAKING THE SAME |
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JPS6270268A (en) * | 1986-03-19 | 1987-03-31 | 住友電気工業株式会社 | Sintered body for high hardness tools |
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KR20110066939A (en) * | 2008-09-17 | 2011-06-17 | 다이아몬드 이노베이션즈, 인크. | Cubic Boron Nitride Ceramic Composites and Method for Producing the Same |
US8354353B2 (en) | 2008-09-17 | 2013-01-15 | Diamond Innovations, Inc. | Cubic boron nitride ceramic composites and methods of making thereof |
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JP2014144911A (en) * | 2014-03-06 | 2014-08-14 | Sumitomo Electric Ind Ltd | Sintered body and cutting tool obtained by using the sintered body |
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