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JPS6131072B2 - - Google Patents
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JPS6131072B2 - - Google Patents

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Publication number
JPS6131072B2
JPS6131072B2 JP53139433A JP13943378A JPS6131072B2 JP S6131072 B2 JPS6131072 B2 JP S6131072B2 JP 53139433 A JP53139433 A JP 53139433A JP 13943378 A JP13943378 A JP 13943378A JP S6131072 B2 JPS6131072 B2 JP S6131072B2
Authority
JP
Japan
Prior art keywords
ultra
high pressure
group
cubic
toughness
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
JP53139433A
Other languages
Japanese (ja)
Other versions
JPS5567575A (en
Inventor
Taijiro Oonishi
Kenichi Nishigaki
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Mitsubishi Metal Corp
Original Assignee
Mitsubishi Metal Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Mitsubishi Metal Corp filed Critical Mitsubishi Metal Corp
Priority to JP13943378A priority Critical patent/JPS5567575A/en
Publication of JPS5567575A publication Critical patent/JPS5567575A/en
Publication of JPS6131072B2 publication Critical patent/JPS6131072B2/ja
Granted legal-status Critical Current

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Description

【発明の詳細な説明】[Detailed description of the invention]

この発明は、高硬度、並びに耐摩耗性、靭性、
および耐食性などが要求される、高硬度鋼やNi
基あるいはCo基スーパーアロイなどの切削用工
具、軸受、および線引ダイスなどとして使用する
のに適した超高圧焼結工具材料に関するものであ
る。 従来、一般に、上記の用途に対しては、すぐれ
た靭性を有する炭化タングステン基超硬合金が広
く使用されてきているが、近年、使用条件が苛酷
になるにしたがつて、よりすぐれた工具材料の開
発が強く望まれている。 最近、かかる要望にしたがつて、立方晶窒化ほ
う素焼結材料や、これに少量のAlおよび鉄族金
属を含有させた焼結材料が提案され、市販されて
いるが、前記の焼結材料はすぐれた耐摩耗性をも
つものの、靭性が不足したものであり、また後者
の焼結材料は、特に高い熱発生を伴なう条件下で
使用した場合に耐摩耗性が劣化するようになるな
ど、いずれも満足する特性を備えた材料ではない
のが現状である。 本発明者等は、上述のような観点から、すぐれ
た靭性、高温耐酸化性(耐熱性)、および耐摩耗
性を兼ね備えた焼結工具材料を得べく、特に立方
晶窒化ほう素に代つて、高硬度高靭性を有する立
方晶炭窒化ほう素(以下立方晶BNCという)に
着目し研究を行なつた結果、立方晶BNC粉末
に、周期律表の4a族金属の炭化物、窒化物、ほう
化物、および酸化物、同5a族金属の炭化物および
窒化物、同6a族金属の炭化物、並びにこれらの2
種以上の固溶体、さらに酸化アルミニウム、窒化
アルミニウム、炭化けい素、窒化けい素、炭化ほ
う素、および酸化イツトリウムからなる群のうち
の1種または2種以上(以下こられを総称して化
合物という)の粉末を配合し、この配合粉末を均
質混合した状態で超高圧焼結すると、靭性、耐熱
性、および耐摩耗性とを兼ね備えた焼結工具材料
が得られるという知見を得たのである。 したがつて、この発明は、上記知見にもとづい
てなされたもので、容量%で、 立方晶BNC:10〜90%、 化合物:10〜90%、 不可避不純物:5%以下、 からなる組成を有する靭性、耐熱性、および耐摩
耗性にすぐれた超高圧焼結工具材料に特徴を有す
るものである。 つぎに、この発明の超高圧焼結工具材料におい
て、成分組成範囲を上述のように限定した理由を
説明する。 (a) 立方晶BNC 立方晶BNCは、結晶構造が六方晶系あるい
は無定形のBNC粉末、すなわちBxNyCz粉末
を、少量で鉄族金属粉末と混合した状態で焼結
用金属製容器に封入し、公知の超高圧高温発生
装置を用いて、温度1200℃以上、圧力40Kb以
上、望ましくは温度1500℃以上、圧力70Kb以
上の条件で所定時間保持することによつて立方
晶の結晶構造に変換合成されるもので、この結
果得られた立方晶構造のBxNyCzは、x=yと
なつており、またzは通常0.1<z<5.0の範囲
内にある。 したがつて、以下の記載においては、BNCz
として簡便な表現を用い、x=y=1とする。 立方晶BNCは、非常に高い硬さを有すると
共に、化学的に安定な性質をもち、しかもすぐ
れた靭性も合わせもつものであるが、その含有
量が10容量%末満では、所望の耐摩耗性を確保
することができず、一方90容量%を越えて含有
させると相対的に化合物の含有量が少なくなり
過ぎて靭性および耐熱性が低下するようになる
ことから、その含有量を10〜90容量%と定め
た。 (b) 化合物 これら化合物は、いずれも高融点高硬度を有
すると共に、高温における耐酸化性にもすぐ
れ、さらに焼結時に粒界拡散を促進させて強固
な粒子間結合を形成すると共に、それ自体が焼
結性にすぐれたものであるため緻密な組織を形
成して靭性を向上させる作用があるが、その含
有量が10容量%末満では前記作用に所望の効果
が得られず、一方90容量%を越えて含有させる
と、相対的に立方晶BNCの含有量が少なくな
り過ぎて所望の耐摩耗性を確保することができ
なくなることから、その含有量を10〜90容量%
と定めた。 (c) 不可避不純物 不可避不純物は、立方晶BNC合成時に混合
される少量の鉄族金属や、材料製造に際して原
料粉末の混合時に混合容器などから混入する鉄
族金属および炭化タングステンなどから構成さ
れるものであるが、最高5容量%まで含有され
ても材料特性に何らの悪影響を及ぼさないこと
から、その上限値を5容量%と定めた。 さらに、この発明の工具材料は、上記のよう
にして合成された立方晶BNC粉末と化合物粉
末とを所定割合に配合し、長時間混合して均質
な混合粉末とした後、前記混合粉末を金属製容
器に封入し、ついて例えば特公昭38−14号公報
に記載されるような超高圧高温発生装置に装入
し、圧力および温度を上げて圧力40Kb以上、
温度1200℃以上の圧力および温度に約5分以上
保持し、冷却後、圧力を開放することによつて
製造される。 ついで、この発明の超高圧焼結工具材料を実施
例により説明する。 まず、各種の無定形BNC粉末と、Ni−Al合金
粉末を用い、これを容量%で90:10の割合に配合
し、通常の条件で混合した後、Ta製容器に封入
し、公知の超高圧高温発生装置にて、圧力:70〜
80Kb、温度:1500〜1700℃、保持時間:20分の
条件で処理し、冷却後圧力解放して取出し、引続
いて酸洗し、かつ比重差を利用する分離法にて分
離処理を行なうことによつて原料粉末として用い
るための各種の立方晶BNCz(Z:012,0.8,
0.95、および4.5)粉末を製造した。 つぎに、これらの平均粒径:3μmを有する各
種のBNCz粉末のほかに、別途用意した0.2〜3μ
mの範囲内の平均粒径を有する各種の化合物粉
末、並びに従来超高圧焼結工具材料を製造するた
めの立方晶BN粉末を原料粉末として用い、これ
らをそれぞれ第1表に示される配合組成に配合
し、ボールミル中で48時間湿式混合し、乾燥した
後、この混合粉末を外径:12mmφのステンレス鋼
This invention has high hardness, wear resistance, toughness,
High-hardness steel and Ni
The present invention relates to ultra-high pressure sintered tool materials suitable for use as cutting tools, bearings, wire drawing dies, etc., such as base or Co-base superalloys. Conventionally, tungsten carbide-based cemented carbide, which has excellent toughness, has generally been widely used for the above-mentioned applications, but in recent years, as usage conditions have become more severe, better tool materials have been sought. development is strongly desired. Recently, in response to such demands, cubic boron nitride sintered materials and sintered materials containing small amounts of Al and iron group metals have been proposed and commercially available. Although it has excellent wear resistance, it lacks toughness, and the latter sintered material deteriorates in wear resistance especially when used under conditions that involve high heat generation. Currently, none of these materials have satisfactory properties. From the above-mentioned viewpoints, the present inventors have developed a method to replace cubic boron nitride in order to obtain a sintered tool material that has excellent toughness, high-temperature oxidation resistance (heat resistance), and wear resistance. As a result of research focusing on cubic boron carbonitride (hereinafter referred to as cubic BNC), which has high hardness and high toughness, it was found that cubic BNC powder contains carbides, nitrides, and boron of group 4a metals of the periodic table. oxides, carbides and nitrides of Group 5a metals, carbides of Group 6a metals, and these two
solid solutions of more than one species, and one or more of the group consisting of aluminum oxide, aluminum nitride, silicon carbide, silicon nitride, boron carbide, and yttrium oxide (hereinafter collectively referred to as compounds) They found that if the blended powders were homogeneously mixed and sintered under ultra-high pressure, a sintered tool material with good toughness, heat resistance, and wear resistance could be obtained. Therefore, this invention was made based on the above knowledge, and has a composition consisting of: cubic BNC: 10 to 90%, compound: 10 to 90%, and unavoidable impurities: 5% or less, in terms of volume %. It is an ultra-high pressure sintered tool material with excellent toughness, heat resistance, and wear resistance. Next, the reason why the composition range of the ultra-high pressure sintered tool material of the present invention is limited as described above will be explained. (a) Cubic BNC Cubic BNC is produced by mixing BNC powder with a hexagonal or amorphous crystal structure, that is, BxNyCz powder, in a small amount with iron group metal powder and sealing it in a metal container for sintering. It is synthesized by converting it into a cubic crystal structure by holding it for a predetermined period of time at a temperature of 1200°C or higher and a pressure of 40Kb or higher, preferably at a temperature of 1500°C or higher and a pressure of 70Kb or higher using a known ultra-high pressure and high temperature generator. The resulting cubic crystal structure BxNyCz has x=y, and z is usually in the range of 0.1<z<5.0. Therefore, in the following description, BNCz
Using a simple expression, x=y=1. Cubic BNC has extremely high hardness, chemical stability, and excellent toughness, but if its content is less than 10% by volume, it will not have the desired wear resistance. On the other hand, if the content exceeds 90% by volume, the content of the compound will be relatively too small and the toughness and heat resistance will decrease. It was set at 90% capacity. (b) Compounds All of these compounds have high melting points and high hardness, as well as excellent oxidation resistance at high temperatures.Furthermore, they promote grain boundary diffusion during sintering to form strong interparticle bonds. Since it has excellent sinterability, it forms a dense structure and has the effect of improving toughness, but if its content is less than 10% by volume, the desired effect cannot be obtained; If the content exceeds 10 to 90% by volume, the content of cubic BNC will be relatively too small and it will be impossible to secure the desired wear resistance.
It was determined that (c) Unavoidable impurities Unavoidable impurities consist of small amounts of iron group metals that are mixed during cubic BNC synthesis, iron group metals and tungsten carbide that are mixed in from mixing containers when mixing raw material powder during material production. However, since it does not have any adverse effect on the material properties even if it is contained up to 5% by volume, the upper limit was set at 5% by volume. Furthermore, the tool material of the present invention is obtained by blending the cubic BNC powder synthesized as described above and a compound powder in a predetermined ratio, mixing for a long time to make a homogeneous mixed powder, and then adding the mixed powder to a metal. It is then placed in an ultra-high pressure and high temperature generator such as that described in Japanese Patent Publication No. 38-14, and the pressure and temperature are increased to a pressure of 40 Kb or more.
It is manufactured by maintaining the pressure and temperature at a temperature of 1200°C or more for about 5 minutes or more, and then releasing the pressure after cooling. Next, the ultra-high pressure sintered tool material of the present invention will be explained with reference to Examples. First, various amorphous BNC powders and Ni-Al alloy powders were mixed in a volume ratio of 90:10, mixed under normal conditions, and then sealed in a Ta container. Pressure: 70~ with high pressure and high temperature generator
80Kb, temperature: 1500-1700℃, holding time: 20 minutes, after cooling, pressure is released and taken out, followed by pickling, and separation treatment using a separation method that utilizes the difference in specific gravity. Various cubic BNCz (Z: 012, 0.8,
0.95, and 4.5) powder was produced. Next, in addition to these various BNCz powders with an average particle size of 3 μm, we prepared separately prepared BNCz powders of 0.2 to 3 μm.
Various compound powders having an average particle size within the range of After blending and wet mixing in a ball mill for 48 hours and drying, this mixed powder is made of stainless steel with an outer diameter of 12 mmφ.

【表】【table】

【表】 容器に詰め、公知の超高圧高温発生装置にて、
1400〜1600℃の範囲内の所定の最高加熱温度、30
〜60Kbの範囲内の所定の最高付加圧力、10分の
保持時間の条件で焼結し、冷却し、圧力解放する
ことによつて実質的に配合組成と同一の組成(た
だし、いずれの場合も混合時にボールミルなどか
ら混入した炭化タングステンや鉄族金属を不可避
不純物として4%以下の範囲で含有する)を有す
る本発明超高圧焼結工具材料1〜27、比較超高圧
焼結工具材料1〜2、および従来超高圧焼結工具
材料をそれぞれ製造した。 なお、比較超高圧焼結工具材料1〜2は、いず
れも構成成分のうちのいずれかの成分(第1表に
※印を付したもの)がこの発明の範囲から外れた
組成をもつものである。 つぎに、この結果得られた各種の超高圧焼結工
具材料について、耐摩耗性を評価する目的でビツ
カース硬さを、また靭性を評価する目的で破壊靭
性値をそれぞれ測定し、さらに切削および研磨手
段にて切削用切刃を切出し、この切刃をWC(炭
化タングステン)基超硬合金製チツプに銀ろうを
用いてろう付けして切削工具とし、 被削材:硬さHRC62を有する軸受鋼(JIS・
SUJ2)、 切削速度:150m/min 送り:0.2mm/rev、 切込み:0.5mm、 の条件での高硬度鋼の旋削試験、並びに、 被削材:ルネ41 切削速度:80m/min、 送り:0.2mm/rev.、 切込み:1mm、 の条件でのNi基スーパーアロイの連続切削試験
を行ない、いずれの試験でも切刃の逃げ面摩耗幅
が0.2mmに至るまでの切削時間を測定した。この
測定結果を第1表に示した。 第1表に示される結果から、本発明超高圧焼結
工具材料1〜27は、いずれもすぐれた耐摩耗性お
よび靭性を有し、切削試験ではすぐれた性能を十
分に発揮するのに対して、従来超高圧焼結工具材
料は、すぐれた耐摩耗性を示すものの靭性の劣る
ものであるため、切削試験では十分満足する性能
を発揮しないことが明らかである。 また、比較超高圧焼結材料1〜2に見られるよ
うに、構成成分のうちのいずれかの成分でも、お
の含有量がこの発明の範囲から外れると上記の特
性のうちの少なくともいずれかの特性が劣つたも
のになることが明らかである。 上述のように、この発明の超高圧焼結工具材料
は、すぐれた靭性、耐熱性、および耐摩耗性を兼
ね備えているので、これらの特性が要求される高
硬度鋼やNi基あるいはCo基スーパーアロイなの
切削用工具として、また軸受や線引ダイスなどと
して使用した場合にすぐれた特性を発揮するので
ある。
[Table] Packed in a container and heated using a known ultra-high pressure and high temperature generator.
Predetermined maximum heating temperature within the range of 1400-1600℃, 30
By sintering at a predetermined maximum applied pressure within the range of ~60 Kb and a holding time of 10 minutes, cooling, and releasing the pressure, a composition that is substantially the same as the blended composition (but in both cases Invention ultra-high pressure sintered tool materials 1-27, comparative ultra-high pressure sintered tool materials 1-2, containing tungsten carbide and iron group metals mixed in from a ball mill etc. during mixing in a range of 4% or less as inevitable impurities) , and conventional ultra-high pressure sintered tool materials, respectively. In addition, comparative ultra-high pressure sintered tool materials 1 and 2 all have compositions in which any of the constituent components (those marked with * in Table 1) are outside the scope of the present invention. be. Next, for the various ultra-high pressure sintered tool materials obtained as a result, the Vickers hardness was measured for the purpose of evaluating wear resistance, and the fracture toughness value was measured for the purpose of evaluating toughness. A cutting edge is cut out using a cutting method, and this cutting edge is brazed to a WC (tungsten carbide)-based cemented carbide chip using silver solder to make a cutting tool. Work material: Hardness H R C62. Bearing steel (JIS/
SUJ2), Cutting speed: 150m/min, Feed: 0.2mm/rev, Depth of cut: 0.5mm, Turning test on high hardness steel, Work material: Rene 41 Cutting speed: 80m/min, Feed: 0.2 Continuous cutting tests were conducted on Ni-based superalloy under the following conditions: mm/rev., depth of cut: 1 mm, and in each test, the cutting time until the flank wear width of the cutting edge reached 0.2 mm was measured. The measurement results are shown in Table 1. From the results shown in Table 1, the ultra-high pressure sintered tool materials 1 to 27 of the present invention all have excellent wear resistance and toughness, and fully demonstrate excellent performance in cutting tests. Although conventional ultra-high pressure sintered tool materials exhibit excellent wear resistance, they have poor toughness, so it is clear that they do not exhibit sufficiently satisfactory performance in cutting tests. Furthermore, as seen in Comparative Ultra-High Pressure Sintered Materials 1 and 2, if the content of any of the constituent components falls outside the scope of the present invention, at least one of the above properties may be lost. It is clear that the characteristics will be inferior. As mentioned above, the ultra-high pressure sintered tool material of this invention has excellent toughness, heat resistance, and wear resistance, so it can be used in high-hardness steel, Ni-based or Co-based superstructures that require these properties. It exhibits excellent properties when used as an alloy cutting tool, as well as in bearings, wire drawing dies, etc.

Claims (1)

【特許請求の範囲】 1 立方晶炭窒化ほう素:10〜90%、 周期律表の4a族金属の炭化物、窒化物、ほう化
物、および酸化物、同5a族金属の炭化物および窒
化物、同6a族金属の炭化物、並びにこれらの2種
以上の固溶体、さらに酸化アルミニウム、窒化ア
ルミニウム、炭化けい素、窒化けい素、炭化ほう
素、および酸化イツトリウムからなる群のうちの
1種または2種以上:5〜60%、 不可避不純物:5%以下、 からなる組成(以上容量%)を有し、特にすぐれ
た靭性を有する超高圧焼結工具材料。
[Claims] 1. Cubic boron carbonitride: 10 to 90%, carbides, nitrides, borides, and oxides of metals from group 4a of the periodic table, carbides, nitrides, and nitrides of metals from group 5a of the periodic table. Group 6a metal carbides, solid solutions of two or more of these, and one or more of the group consisting of aluminum oxide, aluminum nitride, silicon carbide, silicon nitride, boron carbide, and yttrium oxide: An ultra-high pressure sintered tool material having a composition (volume %) consisting of: 5 to 60%, inevitable impurities: 5% or less, and having particularly excellent toughness.
JP13943378A 1978-11-14 1978-11-14 Ultrahigh pressure sintered tool material Granted JPS5567575A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP13943378A JPS5567575A (en) 1978-11-14 1978-11-14 Ultrahigh pressure sintered tool material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP13943378A JPS5567575A (en) 1978-11-14 1978-11-14 Ultrahigh pressure sintered tool material

Publications (2)

Publication Number Publication Date
JPS5567575A JPS5567575A (en) 1980-05-21
JPS6131072B2 true JPS6131072B2 (en) 1986-07-17

Family

ID=15245073

Family Applications (1)

Application Number Title Priority Date Filing Date
JP13943378A Granted JPS5567575A (en) 1978-11-14 1978-11-14 Ultrahigh pressure sintered tool material

Country Status (1)

Country Link
JP (1) JPS5567575A (en)

Also Published As

Publication number Publication date
JPS5567575A (en) 1980-05-21

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