JPH06298567A - Sialon-based sintered compact and sintered and coated material - Google Patents
Sialon-based sintered compact and sintered and coated materialInfo
- Publication number
- JPH06298567A JPH06298567A JP5107584A JP10758493A JPH06298567A JP H06298567 A JPH06298567 A JP H06298567A JP 5107584 A JP5107584 A JP 5107584A JP 10758493 A JP10758493 A JP 10758493A JP H06298567 A JPH06298567 A JP H06298567A
- Authority
- JP
- Japan
- Prior art keywords
- sialon
- sintered body
- based sintered
- sintered compact
- boundary phase
- 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.)
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Abstract
Description
【0001】[0001]
【産業上の利用分野】本発明は、β−サイアロンを主成
分とするマトリックスと、残りがHfおよび/またはZ
rと希土類元素とでなる複合酸化物を主成分とする粒界
相とからなるサイアロン基焼結体およびその表面に被膜
を被覆してなる被覆サイアロン基焼結体に関し、具体的
には、特に 旋削工具,フライス工具,ドリル,エンド
ミル等の切削工具または缶成形用型,スリッター,ブッ
シュ,ガイド,ノズル,バルブ,ボール等の耐摩耗工具
として最適なサイアロン基焼結体およびその表面に被膜
を被覆してなる被覆サイアロン基焼結体に関する。BACKGROUND OF THE INVENTION The present invention relates to a matrix containing β-sialon as a main component and the balance Hf and / or Z.
More specifically, the present invention relates to a sialon-based sintered body composed of a grain boundary phase containing r and a rare earth element as a main component, and a coated sialon-based sintered body having a surface coated with a film. A sialon-based sintered body that is most suitable for cutting tools such as turning tools, milling tools, drills, end mills, and can-molding dies, slitters, bushes, guides, nozzles, valves, balls, etc. And a coated sialon-based sintered body.
【0002】[0002]
【従来の技術】一般に、サイアロンおよび窒化ケイ素焼
結体は、その優れた機械的強度,靭性,耐熱衝撃性によ
り切削工具や耐摩耗工具、あるいはタービン翼やエンジ
ン部品として実用されている。2. Description of the Related Art In general, sialon and silicon nitride sintered bodies are practically used as cutting tools, wear resistant tools, turbine blades and engine parts due to their excellent mechanical strength, toughness and thermal shock resistance.
【0003】ここで、粒界相を含まないサイアロンある
いは窒化ケイ素では、破壊モードは主として粒内破壊と
なるため靭性に著しく劣り、実用化されている焼結体
は、主として希土類酸化物を含む粒界相とサイアロンま
たは窒化ケイ素とからなる複合焼結体である。このた
め、その焼結体の耐熱性等の高温特性は、主成分である
サイアロンまたは窒化ケイ素よりも融点の低い粒界相の
性質により決定されるが、従来の焼結体における粒界相
の耐熱性は決して充分なものとは云えず、高温での強度
低下が著しいという問題がある。Here, in Sialon or silicon nitride containing no grain boundary phase, the fracture mode is mainly intragranular fracture, so that the toughness is remarkably inferior, and the practically used sintered body is mainly a grain containing rare earth oxides. It is a composite sintered body composed of a boundary phase and sialon or silicon nitride. Therefore, the high temperature characteristics such as heat resistance of the sintered body are determined by the properties of the grain boundary phase having a lower melting point than that of sialon or silicon nitride, which is the main component. It cannot be said that the heat resistance is sufficient, and there is a problem that the strength is remarkably reduced at high temperatures.
【0004】この問題を解決しようとした代表的な窒化
ケイ素を主成分とする窒化ケイ素基焼結体として、特開
昭62−153169号公報がある。As a typical silicon nitride-based sintered body containing silicon nitride as a main component to solve this problem, there is JP-A-62-153169.
【0005】[0005]
【発明が解決しようとする課題】特開昭62−1531
69号公報には、希土類元素の酸化物と、Hf,Ta,
またはNbの酸化物,炭化物,ケイ化物の群から選ばれ
た少なくとも1種と、窒化アルミニウムと、残部が窒化
ケイ素よりなるセラミックス混合物を焼成してなる窒化
ケイ素焼結体が開示されている。[Problems to be Solved by the Invention] Japanese Patent Application Laid-Open No. 62-1531
No. 69 discloses a rare earth element oxide, Hf, Ta,
Alternatively, there is disclosed a silicon nitride sintered body obtained by firing a ceramic mixture containing at least one selected from the group consisting of oxides, carbides, and silicides of Nb, aluminum nitride, and the balance silicon nitride.
【0006】この焼結体は、従来のSi3N4−Al2O3
−AlN−希土類酸化物系におけるAl2O3をHfO2
で置換することにより、高温における機械的強度を高め
ることに成功した優れた焼結体であるが、主成分がβ−
Si3N4であるため、切削工具として使用する場合、被
削材の主成分である鉄族金属との反応性に富み、耐摩耗
性に劣るという問題がある。This sintered body is a conventional Si 3 N 4 --Al 2 O 3
The Al 2 O 3 in -AlN- rare earth oxide HfO 2
It is an excellent sintered body that succeeded in increasing the mechanical strength at high temperature by replacing
Since it is Si 3 N 4, when it is used as a cutting tool, there is a problem that it is highly reactive with the iron group metal that is the main component of the work material and is poor in wear resistance.
【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、耐摩耗性に優れるβ−サイアロン
を主成分とし、高融点の複合酸化物を粒界相に、適量存
在させることにより、耐摩耗性,耐欠損性、耐熱衝撃性
に優れたサイアロン基焼結体および被覆サイアロン基焼
結体の提供を目的とする。The present invention has solved the above-mentioned problems. Specifically, a complex oxide containing β-sialon having a high wear resistance as a main component and a high melting point as a grain boundary phase is used in an appropriate amount. An object of the present invention is to provide a sialon-based sintered body and a coated sialon-based sintered body which are excellent in wear resistance, fracture resistance and thermal shock resistance when present.
【0008】[0008]
【課題を解決するための手段】本発明者は、β−サイア
ロン(Si6-Z−Al zO zN8-Z、0<z≦4.2)、
α−サイアロン〔M’y(Si,Al)12(O,
N)16、M’=Li,Mg,Ca希土類元素の1種、0
<y≦2〕またはSi3N4を主成分とする焼結体につい
て、切削時の耐摩耗性により検討したところ、β−サイ
アロンを主成分とした焼結体は、被削材の主成分である
鉄族金属との反応が生じ難く、耐摩耗性に著しく優れる
という知見を得た。The present inventor has found that β-sia
Ron (Si6-Z-Al zO zN8-Z, 0 <z ≦ 4.2),
α-sialon [M'y (Si, Al)12(O,
N)16, M '= Li, Mg, Ca one of rare earth elements, 0
<Y ≦ 2] or Si3NFourFor the sintered body containing
The wear resistance during cutting was examined to find that β-size
The sintered body containing Aron as the main component is the main component of the work material.
Reacts with iron group metals less easily and has excellent wear resistance
I got the knowledge.
【0009】また、β−サイアロンを主成分としたマト
リックスにHfおよび/またはZrと希土類元素からな
る複合酸化物の粒界相を混在させると、室温および高温
における強度,靭性,耐熱衝撃性が著しく改善され、切
削工具として使用すると、耐摩耗性と耐欠損性の両方に
優れた焼結体が得られるという知見を得た。本発明は、
これらの知見に基づいて完成するに至ったものである。Further, when a grain boundary phase of a composite oxide composed of Hf and / or Zr and a rare earth element is mixed in a matrix containing β-sialon as a main component, strength, toughness, and thermal shock resistance at room temperature and high temperature become remarkable. It was found that a sintered body which is improved and is excellent in both wear resistance and fracture resistance when used as a cutting tool. The present invention is
It was completed based on these findings.
【0010】本発明のサイアロン基焼結体は、β−サイ
アロンを主成分とするマトリックス75〜99重量%
と、残部がR2M2-XO7-2X(但し、Rは、Sc,Yを含
めた希土類元素の中の少なくとも1種を表わし、Mは、
Hfおよび/またはZrを表わし、−1<x<1からな
り、Oは酸素を表わす。)で表わされる複合酸化物を主
成分とする粒界相とからなるものである。The sialon-based sintered body of the present invention comprises a matrix containing β-sialon as a main component in an amount of 75 to 99% by weight.
And the balance is R 2 M 2-X O 7-2X (wherein R represents at least one of rare earth elements including Sc and Y, and M represents
It represents Hf and / or Zr, consists of -1 <x <1, and O represents oxygen. ) And a grain boundary phase containing a complex oxide as a main component.
【0011】本発明のサイアロン基焼結体におけるマト
リックスは、マトリックス中の50重量%以上がβ−サ
イアロン(組成式:Si6-Z−Al zO zN8-Z、0<z
≦4.2)であり、その他α−Si3N4,β−Si
3N4,α−サイアロン(組成式:M’y(Si,Al)
12(O,N)16、M’=Li,Mg,Ca,希土類元素
の中の少なくとも1種、0<y≦2),ケイ素アルミニ
ウム酸窒化物(例えば、Si12Al18O39N8)または
炭化ケイ素の中の少なくとも1種が含まれている。Mat in the sialon-based sintered body of the present invention
In the matrix, 50% by weight or more of the matrix is β-sax.
Earon (Composition formula: Si6-Z-Al zO zN8-Z, 0 <z
≦ 4.2) and other α-Si3NFour, Β-Si
3NFour, Α-sialon (compositional formula: M'y (Si, Al)
12(O, N)16, M '= Li, Mg, Ca, rare earth element
At least one of the above, 0 <y ≦ 2), silicon aluminum
Uromoxynitride (eg Si12Al18O39N8) Or
At least one of silicon carbide is included.
【0012】本発明のサイアロン基焼結体における粒界
相は、粒界相中の50重量%以上がR2M2-XO7-2X(−
1<x<1)で表わされる複合酸化物でなり、他にY2
Si3N4O3(メリライト)やガラス相が含まれている
場合がある。 Regarding the grain boundary phase in the sialon-based sintered body of the present invention, 50% by weight or more of the grain boundary phase is R 2 M 2-X O 7-2X (-
It is a complex oxide represented by 1 <x <1), and Y 2
It may contain Si 3 N 4 O 3 (Mellilite) or a glass phase.
【0013】特に、R2M2-XO7-2Xの複合酸化物の中で
もHfO2とDy2O3の固溶体であるDy2Hf2O7また
は(DyY)2Hf O7として存在させると、機械的強
度,疲労強度,靭性,耐熱衝撃性,高温強度および耐摩
耗性がバランスよく優れることから好ましい粒界相であ
る。In particular, R2M2-XO7-2XAmong the complex oxides of
Also HfO2And Dy2O3Is a solid solution of Dy2Hf2O7Also
Is (DyY)2Hf O7As a mechanical strength
Degree, fatigue strength, toughness, thermal shock resistance, high temperature strength and abrasion resistance
It is a preferable grain boundary phase because it has excellent balance of wear properties.
It
【0014】焼結体中のマトリックスの量と粒界相の量
とは相対関係にあり、マトリックスの量が75重量%未
満になると、相対的に粒界相の量が25重量%を超えて
多くなり、耐摩耗性および耐熱衝撃性の低下が著しく、
逆にマトリックスの量が99重量%を超えて多くなる
と、相対的に粒界相の量が1重量%未満となって、高温
での強度低下が著しくなる。There is a relative relationship between the amount of matrix and the amount of grain boundary phase in the sintered body. When the amount of matrix is less than 75% by weight, the amount of grain boundary phase exceeds 25% by weight. Increase in wear resistance and thermal shock resistance,
On the other hand, when the amount of the matrix exceeds 99% by weight, the amount of the grain boundary phase becomes relatively less than 1% by weight, and the strength at a high temperature is significantly reduced.
【0015】以上述べてきた本発明のサイアロン基焼結
体の全表面または一部表面に周期律表の4a,5a,6
a族金属,Alの炭化物,窒化物,酸化物およびこれら
の相互固溶体もしくはダイヤモンド,ダイヤモンド状カ
ーボン,立方晶窒化ホウ素,硬質窒化ホウ素の中の少な
くとも1種の単層あるいは2種以上の複層でなる0.5
〜20μm膜厚の被膜を被覆すると、より一層、耐摩耗
性が向上するので好ましいことである。On the whole surface or a part of the surface of the sialon-based sintered body of the present invention described above, 4a, 5a, 6 of the periodic table are formed.
Group a metal, Al carbide, nitride, oxide and their mutual solid solution or diamond, diamond-like carbon, cubic boron nitride, hard boron nitride, and at least one single layer or two or more multiple layers Become 0.5
It is preferable to coat with a coating having a thickness of up to 20 μm because the wear resistance is further improved.
【0016】被膜の構成は、基材の表面に直接接触する
第1層がTi,Zr,Hfの炭化物,窒化物,炭酸化
物,窒酸化物及びこれらの相互固溶体でなる場合、基材
との密着性の点から好ましく、この第1層のみでなる場
合、又は第1層の表面にさらに第2層,第3層と多層の
構成にする等、用途によって使い分けることも好ましい
ことである。The composition of the coating film is such that when the first layer, which is in direct contact with the surface of the substrate, is made of Ti, Zr, and Hf carbides, nitrides, carbonates, oxynitrides, and their mutual solid solutions. It is preferable from the viewpoint of adhesiveness, and it is also preferable to use the first layer only, or to use a multilayer structure with a second layer and a third layer on the surface of the first layer, depending on the application.
【0017】本発明の焼結体は、従来から行われている
粉末冶金法を応用することにより作製することができ
る。具体的には、例えば各種の原料粉末をボールミル等
を用いて均一に混合し、圧粉成形体とした後、N2や不
活性ガス等の雰囲気中、1500〜2000℃にて焼結
することにより得ることができる。こうして得た焼結体
の表面に被膜を被覆するには、従来から行われている化
学蒸着法(CVD法)や物理蒸着法(PVD法)または
プラグマCVD法でもって行うことができる。The sintered body of the present invention can be manufactured by applying the conventional powder metallurgy method. Specifically, for example, various raw material powders are uniformly mixed using a ball mill or the like to form a powder compact, and then sintered at 1500 to 2000 ° C. in an atmosphere of N 2 or an inert gas. Can be obtained by The surface of the thus obtained sintered body can be coated with a film by a conventional chemical vapor deposition method (CVD method), physical vapor deposition method (PVD method), or pragma CVD method.
【0018】[0018]
【作用】本発明の焼結体におけるマトリックスを形成し
ているβ−サイアロンが主として耐摩耗性を向上させる
作用をし、マトリックスの粒界に存在する粒界相が強度
および靭性の向上に寄与すると共に、主として耐熱性を
向上させる作用をしているものである。The β-sialon forming the matrix in the sintered body of the present invention mainly acts to improve the wear resistance, and the grain boundary phase existing in the grain boundaries of the matrix contributes to the improvement of the strength and toughness. At the same time, it mainly functions to improve heat resistance.
【0019】[0019]
【実施例1】平均粒径0.7μmのSi3N4 粉末,
0.2μmのAl2O3 粉末,0.3μmのAlN粉
末,0.5μmのDy2O3粉末,Y2O3 粉末,Yb2O
3粉末,Er2O3粉末,0.4μmのHfO2 粉末,お
よび一次粒子径が300ÅのZrO2粉末を用いて表1
に示す割合に配合し、ボールミルによる粉砕混合を行な
った。Example 1 Si 3 N 4 powder having an average particle size of 0.7 μm,
0.2 μm Al 2 O 3 powder, 0.3 μm AlN powder, 0.5 μm Dy 2 O 3 powder, Y 2 O 3 powder, Yb 2 O
3 powder, Er 2 O 3 powder, 0.4 μm HfO 2 powder, and ZrO 2 powder with a primary particle size of 300Å were used.
The ingredients were blended in the proportions shown in, and pulverized and mixed by a ball mill.
【0020】成形助剤としてのパラフィンワックスを5
wt%添加し、1ton/cm2の圧力で金型によるプ
レス成形を行なった。5 paraffin wax as a molding aid
wt% was added, and press molding was performed using a mold at a pressure of 1 ton / cm 2 .
【0021】得られた粉末圧粉体を大気圧の窒素雰囲気
中1750℃で2時間保持にて焼結し、さらに1000
気圧の窒素ガス雰囲気1700℃1時間保持にてHIP
処理を行ない、表2に示す焼結体組成からなる本発明品
1〜9および比較品1〜4を得た。The obtained powder compact was sintered by holding it at 1750 ° C. for 2 hours in a nitrogen atmosphere at atmospheric pressure, and further 1000
HIP at 1700 ° C for 1 hour under nitrogen atmosphere at atmospheric pressure
Treatment was performed to obtain Inventive Products 1 to 9 and Comparative Products 1 to 4 having the sintered body compositions shown in Table 2.
【0022】[0022]
【表1】 [Table 1]
【0023】[0023]
【表2】 こうして得た本発明品および比較品の室温における曲げ
強さ、さらにアルゴン雰囲気下、1200℃における曲
げ強さを測定するとともに、下記(A)条件による旋削
試験と(B)条件によるフライス切削試験を行い、これ
らの結果を表3に示した。 (A)湿式による連続旋削試験条件 被削材 :FC350 切削速度 :800m/min 切込み :1.5mm 送り :0.7mm/rev 切削時間 :2min 切削油 :水溶性切削油 チップ形状:SNGN120408 評価 :平均逃げ面摩耗量(VB) (B)乾式によるフライス切削試験条件 被削材 :FCD600(45×200mm面) 切削速度 :150m/min 切込み :1.5mm 初期送り :0.20mm/rev チップ形状:SNGN120408 評価 :チップ欠損に至る最大送り(1Passで
欠損しない場合は、0.03mm/rev送りを増加)[Table 2] The bending strengths of the inventive product and the comparative product thus obtained at room temperature and further at 1200 ° C. under an argon atmosphere were measured, and a turning test under the following conditions (A) and a milling cutting test under the conditions (B) were performed. The results are shown in Table 3. (A) Wet continuous turning test conditions Work material: FC350 Cutting speed: 800 m / min Depth of cut: 1.5 mm Feed: 0.7 mm / rev Cutting time: 2 min Cutting oil: Water-soluble cutting oil Chip shape: SNGN120408 Evaluation: Average Flank wear (V B ) (B) Dry milling cutting test conditions Work material: FCD600 (45 x 200 mm surface) Cutting speed: 150 m / min Depth of cut: 1.5 mm Initial feed: 0.20 mm / rev Chip shape: SNGN120408 Evaluation: Maximum feed leading to chip loss (0.03 mm / rev feed increased if no chipping occurs at 1 Pass)
【0024】[0024]
【表3】 [Table 3]
【0025】[0025]
【実施例2】実施例1で得た本発明品1〜4および比較
品4を用いて、それぞれの焼結体の表面にCVD法でも
って被膜を形成した。被膜は、焼結体の表面に形成させ
た層を第1層、次が第2層、その次が第3層として、表
4に示したように、それぞれの焼結体の表面に形成し
て、本発明の被覆サイアロン基焼結体No10〜13お
よび比較の被覆サイアロン基焼結体No5を得た。Example 2 Using the products 1 to 4 of the present invention and the comparative product 4 obtained in Example 1, a film was formed on the surface of each sintered body by the CVD method. The coating was formed on the surface of each sintered body as shown in Table 4 with the layer formed on the surface of the sintered body as the first layer, the second layer next, and the third layer next. Thus, coated sialon-based sintered bodies No. 10 to 13 of the present invention and comparative coated sialon-based sintered body No. 5 were obtained.
【0026】こうして得た本発明品10〜13および比
較品5を用いて、実施例1の(A)条件および(B)条
件による切削試験を行い、表4にその結果を併記した。Using the products 10 to 13 of the present invention and the comparative product 5 thus obtained, a cutting test was conducted under the conditions (A) and (B) of Example 1, and the results are shown in Table 4.
【0027】[0027]
【表4】 [Table 4]
【0028】[0028]
【発明の効果】本発明の焼結体は、従来のβ−サイアロ
ン基焼結体に比べて、切削試験における耐摩耗性が約2
7%以上も優れており、耐欠損性が2〜4ランク(0.
06〜0.12の送り)も向上するという効果を有し、
従来の窒化ケイ素焼結体に比べて、耐摩耗性が約55〜
64%も優れており、耐欠損性が2〜3ランク(0.0
6〜0.09の送り)も向上するという効果を有してい
る。The sintered body of the present invention has a wear resistance of about 2 in the cutting test as compared with the conventional β-sialon-based sintered body.
7% or more is excellent, and the fracture resistance is 2 to 4 ranks (0.
The effect of improving the feed rate of 06 to 0.12),
Compared with conventional silicon nitride sintered bodies, the wear resistance is about 55-
64% is excellent, and the fracture resistance is 2-3 ranks (0.0
6 to 0.09) is also improved.
Claims (2)
クスを75〜99重量%と、残部が次式(A)で表わさ
れる複合酸化物を主成分とする粒界相とからなることを
特徴とするサイアロン基焼結体。 R2M2-XO7-2X ‥‥‥(A) (但し、Rは、Sc,Yを含めた希土類元素の中の少な
くとも1種を表わし、Mは、Hfおよび/またはZrを
表わし、−1<x<1からなり、Oは酸素を表わす。)1. A matrix comprising β-sialon as a main component in an amount of 75 to 99% by weight, and the balance consisting of a grain boundary phase containing a complex oxide represented by the following formula (A) as a main component. Sialon-based sintered body. R 2 M 2-X O 7-2X (A) (wherein R represents at least one of rare earth elements including Sc and Y, M represents Hf and / or Zr, -1 <x <1 and O represents oxygen.)
全面または一部表面に周期律表の4a,5a,6a族の
金属,Alの炭化物,窒化物,酸化物,およびこれらの
相互固溶体もしくはダイヤモンド,ダイヤモンド状カー
ボン,立方晶窒化ホウ素,硬質窒化ホウ素の中の少なく
とも1種の単層あるいは2種以上の複層でなる0.5〜
20μm膜厚の被膜が形成されていることを特徴とする
被覆サイアロン基焼結体。2. The whole or a part of the surface of the sialon-based sintered body according to claim 1, metals of groups 4a, 5a and 6a of the periodic table, carbides of Al, nitrides, oxides, and mutual solid solutions thereof. Alternatively, at least one kind of diamond, diamond-like carbon, cubic boron nitride, and hard boron nitride, or a multi-layer of two or more kinds of 0.5 to
A coated sialon-based sintered body, wherein a coating having a film thickness of 20 μm is formed.
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JP5107584A JP3009310B2 (en) | 1993-04-09 | 1993-04-09 | Sialon-based sintered body and its coated sintered body |
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JP5107584A JP3009310B2 (en) | 1993-04-09 | 1993-04-09 | Sialon-based sintered body and its coated sintered body |
Publications (2)
Publication Number | Publication Date |
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JPH06298567A true JPH06298567A (en) | 1994-10-25 |
JP3009310B2 JP3009310B2 (en) | 2000-02-14 |
Family
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2016136820A1 (en) * | 2015-02-27 | 2016-09-01 | 三菱マテリアル株式会社 | Radius end mill, ball end mill, and end mill |
JP2016159380A (en) * | 2015-02-27 | 2016-09-05 | 三菱マテリアル株式会社 | Ball end mill |
JP2016159379A (en) * | 2015-02-27 | 2016-09-05 | 三菱マテリアル株式会社 | Radius end mill |
-
1993
- 1993-04-09 JP JP5107584A patent/JP3009310B2/en not_active Expired - Fee Related
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2016136820A1 (en) * | 2015-02-27 | 2016-09-01 | 三菱マテリアル株式会社 | Radius end mill, ball end mill, and end mill |
JP2016159380A (en) * | 2015-02-27 | 2016-09-05 | 三菱マテリアル株式会社 | Ball end mill |
JP2016159379A (en) * | 2015-02-27 | 2016-09-05 | 三菱マテリアル株式会社 | Radius end mill |
CN107000080A (en) * | 2015-02-27 | 2017-08-01 | 三菱综合材料株式会社 | Radius end mill, ball end mill and slotting cutter |
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JP3009310B2 (en) | 2000-02-14 |
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