JPWO2017203738A1 - 焼結体およびそれを含む切削工具 - Google Patents
焼結体およびそれを含む切削工具 Download PDFInfo
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- JPWO2017203738A1 JPWO2017203738A1 JP2018518943A JP2018518943A JPWO2017203738A1 JP WO2017203738 A1 JPWO2017203738 A1 JP WO2017203738A1 JP 2018518943 A JP2018518943 A JP 2018518943A JP 2018518943 A JP2018518943 A JP 2018518943A JP WO2017203738 A1 JPWO2017203738 A1 JP WO2017203738A1
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- sintered body
- sialon
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- silicon nitride
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Abstract
Description
上記した各種のサイアロン、TiNなどを含有する焼結体を用いた切削工具は、インコネル(登録商標)などの難削材の加工において優れた耐摩耗性を発揮する一方、切削中に刃先が突発的に欠損するケースがあり、耐欠損性という点で改善の余地があった。切削工具の欠損は、高い寸法精度と表面性状を要求される航空機部品などの切削加工において重大な問題となる。
[本開示の効果]
上記によれば、難削材の加工において高い耐欠損性を発揮することができる。
[本願発明の実施形態の説明]
最初に本発明の実施態様を列記して説明する。
以下、本発明の実施形態(以下、「本実施形態」とも記す)についてさらに詳細に説明する。
従来、サイアロン、窒化ケイ素、窒化チタンなどを含んだ焼結体は、それを切削工具として用いた場合、特にNi基耐熱合金の切削加工において良好な耐摩耗性を有することが知られていた。しかし、航空機用ジェットエンジン部品などの仕上切削加工において突発的な工具の欠損が生じる場合があり課題とされていた。
第1材料は、該第1材料全体に対して5〜90体積%のAl2O3が結晶粒界または結晶粒内に分散した部分安定化ZrO2である。
中和共沈法とは、以下の工程Aおよび工程Bを含む方法である。このような方法は、たとえば2013年に発表された論文(J. Jpn. Soc. Powder Powder Metallurgy, Vol.60, No.10, P428-435)に記載されている。
ゾル−ゲル法とは、以下の工程Xを含む方法である。このような方法は、たとえば2011年に発表された論文(J. Jpn. Soc. Powder Powder Metallurgy, Vol.58, No.12, P727-732)に記載されている。
本実施形態に係る焼結体において第2材料は、サイアロン、窒化ケイ素および窒化チタンのいずれかを少なくとも含む。サイアロン、窒化ケイ素および窒化チタンはそれぞれ、0.1〜5μmの平均粒径を有することが好ましい。平均粒径が0.1μm未満の場合、第1材料などの他の粉末と混合する際、凝集しやすいため焼結不良となる傾向があり、5μmを超えると、焼結時の粒成長により強度が低下する傾向がある。第2材料のより好ましい平均粒径は、0.5〜2μmである。
本実施形態に係る焼結体は、さらに第3相を含むことが好ましい。第3相は、周期律表の第4族元素、第5族元素、第6族元素、ホウ素およびAlからなる群より選ばれる少なくとも1種の元素と、炭素、窒素、酸素およびホウ素からなる群より選ばれる少なくとも1種の元素とからなる少なくとも1種の化合物またはそれらの固溶体であることが好ましい。焼結体がこのような第3相を含むことにより、焼結性が向上し、焼結体の強度がさらに向上する。
上記の化合物の具体例を挙げると、たとえばcBN、TiC、TiN、TiB2、TiCrN、ZrC、ZrN、ZrB2、AlCrN、AlN、AlB2、HfC、HfN、VC、VN、NbC、TaC、CrC、CrN、Cr2N、MoC、WCなどを挙げることができる。第3相は、これらの化合物のいずれか1種単独で、または2種以上を組合わせて構成することができる。さらに第3相は、上記の化合物から2種以上を組み合わせてなる固溶体であってもよい。
本実施形態に係る焼結体は、第1材料を上記の方法で得ることを除き、従来公知の製造方法により製造することができ、特にその製造方法が限定されるものではない。
本実施形態に係る焼結体は、上記したように優れた耐欠損性、耐摩耗性などの特性を示すため、切削工具などに用いることが好適である。すなわち、本実施形態に係る切削工具は、上記焼結体を含む。
原料として、90体積%のβ型サイアロン(第2材料)と10体積%の第1材料とを準備した。具体的には、β型サイアロンとしてβ型サイアロン粒子粉末(商品名:「Z−2」、Zibo Hengshi Technology Development Co.,Ltd製、平均粒径2μm)と、下記のようにして中和共沈法により作製した第1材料とを用いた。第1材料は、第1材料全体に対して15体積%のAl2O3が固溶した部分安定化ZrO2であり、第1材料の粒径は0.15μmであった。
第1材料は、前述のとおり、2013年に発表された論文(J. Jpn. Soc. Powder Powder Metallurgy, Vol.60, No.10, P428-435)に基づき下記の方法により作製できる。
切削速度: 200m/min
送り: 0.2mm/rev.
切込み: 0.3mm
湿式/乾式: 湿式(クーラント:エマルジョン)
クーラント供給圧力: 0.15MPa
旋盤: LB4000(オークマ社製)
被削材: インコネル(登録商標)718[大同スペシャルメタル株式会社製、溶体化・時効硬化処理材、ロックウェル硬度HRC(先端半径0.2mmかつ先端角120°のダイヤモンド円錐を使い150kgfの負荷をかけたもの)が44相当品、ASTM(American Society for Testing and Materials)のE112に規定される粒度番号9の粒度]
被削材の形状: 円筒状(外径φ95mm)。
(第2材料の影響)
上記で準備した第1材料(前駆体)のみを用い、上記の表1のとおりの圧力および焼結温度の条件で15分間維持して焼結することにより、焼結体No.1H〜1Kの4種の焼結体を得た。これらの焼結体から作製した切削工具に対して上記と同様の切削試験を行なった。さらに、焼結体No.1H〜1KについてAl2O3の粒径も上記と同様にして測定した。これらの結果を上記の表1に示す。
焼結方法の比較として、焼結体No.1A〜1Eに用いたものと同じ混合物であって未焼結のものを、圧力30MPa、1500℃あるいは圧力2.5GPa、1500℃で15分間維持して焼結することにより焼結体No.1Lおよび1Mを得た。この焼結体No.1Lおよび1Mから作製した切削工具に対し、上記と同様にして切削試験を行なった。焼結体No.1Lおよび1Mについても、上記と同様にAl2O3の粒径を測定した。これらの結果を上記表1に示す。
焼結体中の第1材料の含有量を以下の表2のとおり変更することを除き、他はすべて実施例1の焼結体No.1C(すなわち焼結温度が1500℃のもの)と同様の条件で焼成することにより、6種類の焼結体を作製した(焼結体No.2A、No.2B、No.2C、No.2D、No.2E、No.2F)。
焼結体中の第1材料(含有量:10体積%)を、以下の第1材料(1)〜第1材料(5)にそれぞれ置き換えることを除き、他はすべて実施例1の焼結体No.1Cと同様にし、5種類の焼結体を作製した。
第1材料(1)で表される焼結体は、実施例1に記載される中和共沈法により作製され、第1材料(1)は、5体積%のAl2O3が固溶した部分安定化ZrO2であり、この部分安定化ZrO2の平均粒径は0.15μmである。
第1材料(2)で表される焼結体は、実施例1に記載される中和共沈法により作製され、第1材料(2)は、30体積%のAl2O3が固溶した部分安定化ZrO2であり、この部分安定化ZrO2の平均粒径は0.15μmである。
第1材料(3)で表される焼結体は、実施例1に記載される中和共沈法により作製され、第1材料(3)は、50体積%のAl2O3が固溶した部分安定化ZrO2であり、この部分安定化ZrO2の平均粒径は0.15μmである。
第1材料(4)で表される焼結体は、実施例1に記載される中和共沈法により作製され、第1材料(4)は、90体積%のAl2O3が固溶した部分安定化ZrO2であり、この部分安定化ZrO2の平均粒径は0.15μmである。
第1材料(5)で表される焼結体は、実施例1に記載される中和共沈法により作製され、第1材料(5)は、95体積%のAl2O3が固溶した部分安定化ZrO2であり、この部分安定化ZrO2の平均粒径は0.15μmである。
実施例4では、原料として実施例1に用いた第1材料(15体積%のAl2O3が固溶した部分安定化ZrO2、粒径0.15μm)を用いた。さらに、第2材料としてα型窒化ケイ素粒子粉末(商品名:「SN E−10」、宇部興産株式会社製、平均粒径0.5μm)、β型窒化ケイ素粒子粉末(商品名:「SN−F1」、デンカ株式会社製、平均粒径2μm)、α型サイアロン粒子粉末(商品名:「アロンブライト YL−C」、デンカ株式会社製)、上記β型サイアロン粒子粉末(平均粒径2μm)、TiN粉末(商品名:「TiN−01」、日本新金属株式会社製、平均粒径1μm)、以下に示される方法によって合成される立方晶型窒化ケイ素(c−Si3N4)および立方晶型サイアロン(c−SiAlON)からなる群より選ばれる少なくともいずれか1種または2種以上を用いた。
立方晶型窒化ケイ素を作製するため、まず上記のβ型窒化ケイ素を500g、およびヒートシンクとして作用する銅粉末を9500gを混合し、得られた混合物を鋼管に封入した。その後、温度1900℃、衝撃圧力40GPaとなるように設定した量の爆薬を用い、混合物を封入した鋼管に対して衝撃圧縮を付与することにより、立方晶型窒化ケイ素を合成した。衝撃圧縮後、鋼管内の混合粉末を取り出し、酸洗浄により銅粉を除去することにより立方晶型窒化ケイ素の合成粉末を得た。
管電圧: 45kV
管電流: 40A
フィルター: 多層ミラー
光学系: 平行ビーム法
X線回折法: θ−2θ法
測定範囲: 2θ=10〜80°
スキャンステップ: 0.03°
スキャン速度: 1ステップ/秒。
まずCeO2粉末(商品名:「微粒子タイプ Cグレード」、信越化学工業株式会社製、平均粒径0.6μm)、Si粉末(商品名:「SIE19PB」、株式会社高純度化学研究所製、粒径45μm以下)、Al粉末(商品名:「300A」、ミナルコ株式会社製、粒径45μm以下)およびSiO2粉末(商品名:「FB−5D」、デンカ株式会社製、平均粒径5μm)を準備した。本実施例では、Mサイアロン(M=Ce)粉末を合成するため、これらの粉末を適宜選択し、CexSi6-x-zAlzOzN8-zで表されるCeサイアロンにおいてxが0〜2.2、zが2となるように配合し、それぞれを焼結体No.5A〜5Eの出発原料とした。焼結体No.5A〜5Eの出発原料から換算したCeサイアロンの原子比xの値を表5に示す。
管電圧: 45kV
管電流: 15mA
フィルター: 多層ミラー
光学系: 平行ビーム法
X線回折法: θ−2θ法
測定範囲: 2θ=20〜100°
スキャンステップ: 0.02°
スキャン速度: 1ステップ/秒。
まずTi粉末(商品名:「TC-200」、東邦チタニウム株式会社製、平均粒径17μm)、Zr粉末(商品名:「ジルコニウム(粉末)<−40μ>」、三津和化学薬品株式会社製、粒径40μm以下、純度98%以上)、Fe粉末(商品名:「超微粒純鉄粉」、JFEスチール株式会社製、平均粒径1μm)、Y2O3粉末(商品名:「微粒品(高BET品)」、日本イットリウム株式会社製、平均粒径1μm)、CaO粉末(商品名:「酸化カルシウム」、高純度化学研究所株式会社製、純度99.8%)とともに、Ceサイアロンの合成時に用いたSi粉末、Al粉末およびSiO2粉末を準備した。本実施例では、これらの粉末を適宜選択し、MxSi6-x-zAlzOzN8-zで表されるMサイアロンを合成するため、xが0.2、かつzが2となるように配合し、それぞれ焼結体No.6A〜6Eの出発原料とした。さらに、Ceに代えて、以下の表6に示すとおりの金属原料を用いた以外は実施例5と同様にし、Rcが以下の表6に示すとおりのM0.2Si3.8Al2O2N6で表されるMサイアロンの合成粉末を得た。
焼結体中のβ型サイアロン(含有量:90体積%)を、60体積%のβ型サイアロンと表7のとおりの第3相(含有量:1種または2種の合計で30体積%)に置き換えることを除き、他はすべて実施例1の焼結体No.1Cと同様にして、焼結体No.7A〜7Jとなる10種類の焼結体を作製した。
Claims (9)
- 第1材料と第2材料とを含む焼結体であって、
前記第1材料は、該第1材料全体に対して5〜90体積%のAl2O3が結晶粒界または結晶粒内に分散した部分安定化ZrO2であり、
前記第2材料は、サイアロン、窒化ケイ素および窒化チタンのいずれかを少なくとも含み、
前記焼結体は、1〜50体積%の前記第1材料を含む、焼結体。 - 前記Al2O3は、その粒径が1μm以下である、請求項1に記載の焼結体。
- 前記Al2O3は、その粒径が0.5μm以下である、請求項1または請求項2に記載の焼結体。
- 前記Al2O3は、その粒径が0.1μm以下である、請求項1〜請求項3のいずれか1項に記載の焼結体。
- 前記サイアロンおよび前記窒化ケイ素の両方またはいずれか一方は、立方晶型の結晶構造を有する、請求項1〜請求項4のいずれか1項に記載の焼結体。
- 前記サイアロンおよび前記窒化ケイ素の両方またはいずれか一方は、さらにα型の結晶構造またはβ型の結晶構造のいずれかを少なくとも有し、
前記α型の結晶構造、前記β型の結晶構造および前記立方晶型の結晶構造のそれぞれのX線回折のメインピークの強度の合計に対する前記立方晶型の結晶構造のX線回折のメインピークの強度の比率を表すピーク強度比率Rcは、20%以上である、請求項5に記載の焼結体。 - 前記サイアロンおよび前記窒化ケイ素は、MxSi6-x-zAlzOzN8-zで表され、
前記Mは、カルシウム、ストロンチウム、バリウム、スカンジウム、イットリウム、ランタノイド、マンガン、鉄、コバルト、ニッケル、銅、周期律表の第4族元素、第5族元素および第6族元素からなる群より選ばれる少なくとも1種の金属を含み、
前記MxSi6-x-zAlzOzN8-zを構成する各元素の原子比は、0.01≦x≦2、0≦z≦4.2および1.79≦6−x−z≦5.99の関係を満たす、請求項1〜請求項6のいずれか1項に記載の焼結体。 - 前記焼結体は、さらに第3相を含み、
前記第3相は、周期律表の第4族元素、第5族元素、第6族元素、ホウ素およびAlからなる群より選ばれる少なくとも1種の元素と、窒素、炭素、酸素およびホウ素からなる群より選ばれる少なくとも1種の元素とからなる化合物またはそれらの固溶体である、請求項1〜請求項7のいずれか1項に記載の焼結体。 - 請求項1〜請求項8のいずれか1項に記載の焼結体を含む、切削工具。
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