JP2004268201A - Hard carbon film-coated tool - Google Patents
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【０００１】
【発明の属する技術分野】
本発明は、硬質炭素膜被覆工具に関するものである。
【０００２】
【従来の技術】
被加工部材の高硬度及び軽量化に伴って、高硬度、高熱伝導であるダイヤモンド膜を被覆した切削工具や耐摩耗部材を活用する機運が高まっている。特に、ダイヤモンド被覆工具は、アルミ合金やグラファイト材の加工に有望であり、盛んに研究されている。以下の特許文献１から４にダイヤモンド被覆工具が開示されている。
【特許文献１】特開平８−２５９３９１号公報（第９頁表１、第１０頁表２）
【特許文献２】特開２００１−１７９５０４号公報（第５頁表５、第７頁表７）
【特許文献３】特開２００１−３２８００７号公報（第６頁表２、第７頁表３）
【特許文献４】特開２００３−２５１１７号公報（第２頁、請求項１、２）
【０００３】
特許文献１は、（２２０）のＸ線回折ピ−ク強度が他のピークに比べて強いダイヤモンドを利用することにより膜表面を平滑化させ、摺動性を高めることが開示されている。しかし、これらダイヤモンド成分のみの結晶性や摺動性を改質した場合は硬質膜全体としての耐摩耗性や摺動性のバランスの良い改善が充分には成されず、被覆工具として充分な工具寿命を得られない欠点があった。特許文献２、３は、（４００）面の配向が強いダイヤモンドと、（００８）面指数のＸ線回折ピーク強度が強い六方晶グラファイトの両者を含有している硬質炭素膜を被覆することにより、優れた工具寿命を持つ工具が開示されている。特許文献４は、ダイヤモンド被覆膜と潤滑性を有する保護膜とを組み合わせた被覆切削工具であり、該保護膜に硬質炭素膜を用いる技術が開示されている。
【０００４】
【発明が解決しようとする課題】
本発明が解決しようとする課題は、結晶性が良く耐摩耗性の優れたダイヤモンド膜表面の摺動性を高めることにより、耐摩耗性と摺動性の両者が優れた被覆工具を実現し、従来に比して格段に工具寿命の長い硬質炭素膜被覆工具を提供することである。
【０００５】
【課題を解決するための手段】
本発明者らは上記課題を解決するために鋭意研究してきた結果、超硬合金材の表面にダイヤモンド膜を被覆し、該ダイヤモンド膜の（４００）面指数のＸ線回折ピークの２θ値が０．１度以上高角側にシフトしており、該ダイヤモンド膜表面にダイヤモンドライクカーボン膜を被覆し、更に該ダイヤモンド膜の（００８）面指数のＸ線回折ピークの２θ値が０．１度以上低角側にシフトしている六方晶グラファイト成分を含有していることを特徴とする硬質炭素膜被覆工具とすることにより、優れた工具寿命を持つ工具を実現できることを見いだし本発明に想到した。
【発明の実施の形態】
【０００６】
本発明は、超硬合金材の表面にダイヤモンド膜を形成した後、その表面にダイヤモンドライクカーボン（以下、ＤＬＣと記す。）膜を被覆したことを特徴とする硬質炭素膜被覆工具である。こうすることにより、靭性と耐摩耗生の優れた超硬合金材の表面に、高硬度で耐摩耗性が特に優れているダイヤモンド皮膜が形成されており、しかもその表面に摺動特性が高いＤＬＣ膜が形成されていることにより、優れた切削特性を有し、工具寿命の長い硬質炭素膜被覆工具が実現できる。一般に、ＤＬＣ膜は２００℃付近の低温で成膜するため、基体や下層膜との密着性が低く、切削工具として使用時に容易に剥がれてしまう欠点があった。しかし、本発明においては同じカーボンから成るダイヤモンド膜の表面にＤＬＣ膜を形成しているため、下層膜と密着性が優れ、ＤＬＣ膜は切削加工時にも剥がれることなく、特に優れた摺動特性を示す。基体表面にダイヤモンド膜やＤＬＣ膜等が形成されていることは、Ｘ線回折や電子線回折、ラマン分光法等により分析できる。また、皮膜断面を走査電子顕微鏡−エネルギー分散型Ｘ線分析装置（ＳＥＭ−ＥＤＸ）により分析した時、結晶性の高いダイヤモンド膜の表面にアモルファス状の炭素膜が形成されていることからも確認できる。
【０００７】
本発明の硬質炭素膜被覆工具は、該ダイヤモンド膜の（４００）面指数のＸ線回折ピークの２θ値が０．１度以上高角側にシフトしていることが必要である。こうすることにより、該ダイヤモンド膜の摺動性が高まり、ダイヤモンド本来の優れた耐摩耗性と相まって、優れた切削特性を有する硬質炭素膜被覆工具を実現できる。これは（４００）面指数のＸ線回折ピークの２θ値が０．１度以上高角側にシフトしていることにより、ＤＬＣ成分や六方晶グラファイト成分との結合性が高まったためと考えられる。２θ値のシフト量が０．１度未満であるときは工具特性が低下する欠点が現れる。これはダイヤモンド成分とＤＬＣ成分や六方晶グラファイト成分との間の結合力が低下するためと考えられる。
【０００８】
本発明の硬質炭素膜被覆工具は、該ダイヤモンド膜の（００８）面指数のＸ線回折ピークの２θ値が０．１度以上低角側にシフトしている六方晶グラファイト成分を含有していることが好ましい。こうすることにより、該ダイヤモンド膜中に摺動性の優れた六方晶グラファイト成分が含有されており、しかもダイヤモンド成分との間に優れた結合性を有しているため、耐摩耗性と摺動性の両者が特に優れ、しかも安定している、より優れた切削特性を有する硬質炭素膜被覆工具を実現できる。これは、六方晶グラファイト成分の（００８）面指数のＸ線回折ピークの２θ値が０．１度以上低角側にシフトしていることから、ダイヤモンドと六方晶グラファイトの両者の間で原子の共有等の干渉があり、ダイヤモンド成分とグラファイト成分の間に強い結合力が働いていると考えられる。このため、ダイヤモンドの特長である優れた耐摩耗性とグラファイトの特長である優れた摺動特性の両者を同時に併せ持つこととなり、優れた工具特性を示すようになったと判断される。六方晶グラファイト成分のシフト量が０．１度未満であるときは工具特性が低下する欠点が現れる。これはダイヤモンド成分と六方晶グラファイト成分との間の結合力が低下するためと考えられる
【０００９】
本発明における硬質炭素膜被覆工具の代表例である硬質炭素膜被覆エンドミルの例にそって述べる。本発明の被覆工具において、ダイヤモンドのＸ線回折ピークの同定は、ＪＣＰＤＳファイルのＸ線回折データファイル番号６−０６７５を用い、六方晶グラファイトのＸ線回折ピークの同定は、同ファイル番号２５−２８４のデータを用いて行った。本発明の被覆工具のダイヤモンド膜を製作するためには、熱フィラメントＣＶＤ法やマイクロ波ＣＶＤ法、ｒｆプラズマＣＶＤ法、ＥＣＲプラズマＣＶＤ法等、公知のＣＶＤ法を用いることができるが、成膜条件の調整が適宜必要である。本発明者らの研究では、成膜時の基板温度を高めるにつれてダイヤモンドの（４００）Ｘ線回折ピークがより高角側へシフトし、グラファイトの（００８）Ｘ線回折ピークはより低角側へシフトする。また、成膜ガスのＣＨ４／Ｈ２比を下げるにつれてダイヤモンドの（４００）Ｘ線回折ピークの高角側へのシフト量や、グラファイトの（００８）Ｘ線回折ピークの低角側へのシフト量が、小さくなることが分かっている。本発明の被覆工具のＤＬＣ膜を製作するためには、ガス反応を用いたｒｆプラズマＣＶＤ法やマイクロ波ＣＶＤ法、ＥＣＲプラズマＣＶＤ法や、あるいはカーボン製ターゲットを用いた物理蒸着（ＰＶＤ）法を用いることができるが、ダイヤモンド膜とＤＬＣ膜間により高い密着性が得られるため、ＣＶＤ法で成膜することが好ましい。本発明の用途は、ソリッドエンドミル型切削工具に限るものではなく、スローアウェイインサートを用いたエンドミル型切削工具やフライス用工具、旋削用工具でも良い。また、硬質炭素膜を被覆した耐摩耗材や金型、溶湯部品等でもよい。本発明の被覆工具において、硬質炭素膜の成分は炭素だけに限るものではない。本発明の効果を消失しない範囲でＣｏやＷ等の不可避の添加物や不純物を例えば数質量％程度まで含むことが許容される。次に本発明の被覆工具を実施例によって具体的に説明するが、これら実施例により本発明が限定されるものでない。
【００１０】
【実施例】
（実施例１）
ＷＣ：９４質量％、Ｃｏ：６質量％の組成よりなり、同一ロットで焼結し作製した直径６ｍｍ、２枚刃のボールエンドミル型の切削工具用超硬合金基体と、１０ｍｍ×１０ｍｍ、厚さ５ｍｍの分析用直方体基板を真空装置内にセットし、それらの表面に、熱フィラメントＣＶＤ法により、約８μｍ厚さのダイヤモンド膜を成膜した。即ち、エンドミルの周辺に配置したタングステン製フィラメントに電流を流すことにより、これを約２５００℃に加熱し、これにＣＨ４／Ｈ２比が０．５〜３％のＣＨ４とＨ２の混合ガスを１０〜１５０ｃｍ３／ｍｉｎだけ流し、圧力１．３３〜１３．３ｋＰａ、基板温度９００〜１２００℃で成膜した。ｒｆプラズマＣＶＤ法により、真空装置内にＣ２Ｈ２ガスとＨ２とを流し、ガス圧１０．７Ｐａ、基板温度２００℃、基板バイアス８００Ｖで厚さ０．５μｍのＤＬＣ膜を成膜した。作製した試料のＸ線回折パターンは、各試料と一緒に成膜した上記の分析用基板を用いて評価した。理学電気（株）製のＸ線回折装置（ＲＵ−２００ＢＨ型）により、波長λが０．１５４０５ｎｍのＣｕＫα１線を用いて、２θ−θ走査法により測定した。２θの測定範囲は１０〜１４５度で、バックグランドノイズは装置に内蔵されたソフトにより除去した。表１に、各物質のＪＣＰＤＳファイルに記載されている２θ値（２θ０）、面指数及び本発明例１のＸ線回折測定結果と実測２θの標準２θ０からのシフト量Δ２θ（２θ−２θ０）もあわせて示す。表１から、ダイヤモンドの（４００）Ｘ線回折ピーク位置と六方晶グラファイトの（００８）Ｘ線回折ピーク位置のシフト量が特に大きいことがわかる。ＤＬＣ膜はアモルファス状であるため、明確なＸ線回折ピークは検出されなかったが、ＤＬＣ膜が実際に成膜されていることは、ラマンスペクトルで１５８０ｃｍ−１付近と１３６０ｃｍ−１付近にブロードなピークが検出されることから確認した。
【００１１】
【表１】
表２に実施例１によって作製した本発明例２〜１９の硬質炭素膜被覆工具のＸ線回折測定結果と工具寿命とをまとめて示す。
【００１３】
【表２】
表２より、本発明例２〜１９のいずれの試料も、ダイヤモンドの（４００）Ｘ線回折ピークのシフト量Δ２θが正の値を示し、高角側に０．１度以上シフトしていることがわかる。六方晶グラファイトの（００８）Ｘ線回折ピークのシフト量Δ２θが負の値を示し、低角側にシフトしていることがわかる。ここで、９００〜１２００℃の範囲内で成膜時の基板温度を高めるにつれてダイヤモンドの（４００）Ｘ線回折ピークがより高角側へシフトし、グラファイトの（００８）Ｘ線回折ピークはより低角側へシフトした。また、０．５〜３％の範囲内で成膜ガスのＣＨ４／Ｈ２比を下げるにつれてダイヤモンドの（４００）Ｘ線回折ピークの高角側へのシフト量や、グラファイトの（００８）Ｘ線回折ピークの低角側へのシフト量が小さくなった。本発明例２〜１９の工具寿命は、作製した本発明例の各３本を用いて、グラファイト材を下記の条件で切削し、外周刃の刃先の逃げ面摩耗量が０．１ｍｍに達するまでに切削した切削長さにより示した。
被削材：グラファイト（ＨＳ９５）
工具形状：ボールエンドミル（φ６、二枚刃）
工具回転数：１００００回転／ｍｉｎ
切削速度：１８８ｍ／ｍｉｎ
送り速度：２０００ｍｍ／ｍｉｎ（０．１ｍｍ／ｔｏｏｔｈ）
切り込み：０．３ｍｍ×０．３ｍｍ
切削油：使用せず
ショアー硬さＨＳ９５のグラファイト材を被削材に用いることにより、工具の耐摩耗性を早期に評価できるようにした。逃げ面摩耗量は倍率１００の実体顕微鏡と分解能１μｍのスライドテーブルを用いて測定した。表２より、本発明例２〜１９は、いずれも切削可能長が７１０ｍ以上と長く、工具寿命が優れていることがわかる。また、ダイヤモンドの（４００）Ｘ線回折ピークのシフト量が高角側に０．５〜２．０度であるとき、切削可能長が１４３０ｍ以上と２倍以上長く、優れた工具寿命が得られ、１．０〜１．５度の時は切削可能長が２５９０ｍ以上と更に１．８以上倍長く、更に優れた工具寿命が得られることがわかる。また、六方晶グラファイトの（００８）Ｘ線回折ピークのシフト量が低角側に−０．１〜−１．５度であるとき、切削可能長が１４３０ｍ以上と２倍長く、優れた工具寿命が得られ、−０．５〜−１．０度の時は切削可能長が２１５０ｍ以上と更に１．５倍以上長く、更に優れた工具寿命が得られることがわかる。
【００１５】
（実施例２）
超硬合金材の表面にダイヤモンド膜を形成し、更にＤＬＣ膜を被覆する影響を明らかにするため、実施例１と同一ロットで作製したボールエンドミルの切削工具用超硬合金基体と分析用直方体基板を真空装置内にセットし、実施例１と同じ条件でダイヤモンド膜を成膜し、その表面にＤＬＣ膜を成膜しない従来例２０を作製した。従来例２０のラマンスペクトルは１３３２ｃｍ−１付近のダイヤモンドの鋭いピークと１５８０ｃｍ−１付近のグラファイトの鋭いピークのみが検出され、両ピーク付近にブロードなピークを示すＤＬＣは観察されなかった。また、ダイヤモンド成分の（４００）Ｘ線回折ピーク位置は高角側に０．１度シフトし、六方晶グラファイト成分の（００８）Ｘ線回折ピーク位置はシフトしていなかった。従来例２０のボールエンドミル３本を用いて実施例１と同一の条件で工具寿命を評価した結果、３００ｍ以内で外周刃の刃先摩耗量が０．０５ｍｍに達した。この結果、ダイヤモンド成分の（４００）Ｘ線回折ピーク位置と六方晶グラファイトの（００８）Ｘ線回折ピーク位置の両シフト量が同じであるダイヤモンド膜の表面にＤＬＣ膜を形成した本発明例２よりも工具寿命が１／２以下と短く、工具として劣っていることがわかった。即ち、ダイヤモンド膜の表面にＤＬＣ膜を形成した本発明例２〜１９は、同じダイヤモンド膜の表面にＤＬＣ膜を形成していない従来例２０に比べて、２倍以上、工具寿命が優れていることがわかった。
【００１６】
（実施例３）
超硬合金材の表面にダイヤモンド膜を形成し、更にＤＬＣ膜が被覆されている場合、このダイヤモンド膜が、（４００）面指数のＸ線回折ピークの２θ値が高角側にシフトしているダイヤモンド成分と、（００８）面指数のＸ線回折ピークの２θ値が低角側にシフトしている六方晶グラファイトとの両者の含有の有無による、工具寿命への影響を明らかにするために、従来例２１として、実施例１と同一の組成と形状よりなるボールエンドミルの切削工具用超硬合金基体と分析用直方体基板とを真空装置内にセットし、それらの表面に、熱フィラメントＣＶＤ法により約８μｍ厚さの硬質炭素膜を成膜した。その成膜条件は、タングステン製フィラメント温度が約２３００℃、炭素濃度が４％のＣＨ４とＨ２の混合ガス流量１５０ｃｍ３／ｍｉｎ、圧力１３．３ｋＰａ、基板温度８００℃である。この表面に実施例１と同一の条件で、厚さ０．５μｍのＤＬＣ膜を成膜した。従来例２１のダイヤモンド膜は、ダイヤモンド成分の（４００）面指数Ｘ線回折ピークの２θ値が１１９．５度であり、高角側へのシフト量が０．１度未満と小さく、高角側へのシフトは観察されなかった。また、ＤＬＣ膜が実際に成膜されていることの確認は、分析用試料のラマンスペクトルに１５８０ｃｍ−１付近と１３６０ｃｍ−１付近にブロードなピークが検出されることから確認した。また、切削テスト後に、皮膜断面をＳＥＭ−ＥＤＸにより分析し、結晶性の高いダイヤモンド膜の表面にアモルファス状の炭素膜が形成されていることからも確認した。従来例２１のボールエンドミル３本を用いて実施例１と同一の条件で工具寿命を評価した結果、４６０ｍ以内で外周刃の刃先摩耗量が０．０５ｍｍに達し、工具寿命が本発明例２の２／３以下にとどまった。本発明例２と従来例２１とを比較することにより、（４００）面指数のＸ線回折ピークの２θ値が０．１度以上高角側にシフトしているダイヤモンド膜の表面にＤＬＣ膜を形成した本発明例２の工具は、シフト量が０．１度以下であるダイヤモンド膜の表面にＤＬＣ膜を形成した従来例２１の工具に比べて工具寿命が１．６倍以上優れていることがわかった。
【００１７】
（実施例４）
ＷＣ：９５．５質量％、Ｃｏ：４．５質量％の組成よりなる直径６ｍｍ、２枚刃のスクエアエンドミル型の切削工具用超硬合金基体と、１０ｍｍ×１０ｍｍ、厚さ５ｍｍの分析用直方体基板とを真空装置内にセットし、それらの表面に、熱フィラメントＣＶＤ法により、約８μｍ厚さのダイヤモンド膜を成膜した。即ち、エンドミルの周辺に配置したタングステン製フィラメントに電流を流すことにより、これを約２５００℃に加熱し、これにＣＨ４／Ｈ２比が０．５〜３％のＣＨ４とＨ２の混合ガスを１０〜１５０ｃｍ３／ｍｉｎだけ流し、圧力１．３３〜１３．３ＫＰａ、基板温度９００〜１２００℃で成膜した。ｒｆプラズマＣＶＤ法により、真空装置内にＣ２Ｈ２ガスとＨ２とを流し、ガス圧１０．７Ｐａ、基板温度２００℃、基板バイアス８００Ｖで厚さ０．３μｍのＤＬＣ膜を成膜した。スクエアエンドミルの刃先先端にある平坦部を試料面にして、Ｘ線回折パターンを、実施例１と同一の条件で測定した。スクエアエンドミルの刃先先端の平坦部は面積が少ないため、平坦部以外は出来るだけ加工で除去するとともに、ビニールテープで覆うことにより、Ｘ線回折パターンに影響しないように工夫した。表３に実施例４によって作製した本発明例２２〜３８の硬質炭素膜被覆工具のＸ線回折測定結果と工具寿命とをまとめて示す。
【００１８】
【表３】
表３より、本発明例２２〜３８のいずれの試料も、硬質炭素膜が（４００）面指数のＸ線回折ピークの２θ値が高角側に０．１度以上シフトしているダイヤモンド成分と（００８）面指数のＸ線回折ピークの２θ値が低角側に０．１度以上シフトしている六方晶グラファイトの両者より成っていることがわかる。また、ＤＬＣ膜が実際に成膜されていることは、分析用試料のラマンスペクトルに１５８０ｃｍ−１付近と１３６０ｃｍ−１付近にブロードなピークが検出されることから確認した。また、切削テスト後に、皮膜断面をＳＥＭ−ＥＤＸにより分析し、結晶性の高いダイヤモンド膜の表面にアモルファス状の炭素膜が形成されていることからも確認した。作製した本発明例２２〜３８のスクエアエンドミル各３本を用いて、本発明例の工具寿命を下記の条件で評価した。
被削材：Ａｌ−９質量％Ｓｉ合金
工具形状：スクエアエンドミル（φ６、二枚刃）
工具回転数：２００００回転／分
切削速度：５００ｍ／分
送り速度：７．２ｍ／分（０．１８ｍｍ／刃）
切り込み：Ａｄ１５ｍｍ×Ｒｄ０．８ｍｍ
切削油：使用せず
工具寿命は、刃先の逃げ面摩耗量が０．０５ｍｍに達するまでに切削した切削長さで示した。表３中に工具寿命を併記する。表３より、本発明例２２〜３８は、いずれも切削可能長が１８０ｍ以上と長く、工具寿命が優れていることがわかる。また、ダイヤモンドの（４００）Ｘ線回折ピークのシフト量が高角側に０．５〜２．０度であるとき切削可能長が２７０ｍ以上と１．５倍長い、優れた工具寿命が得られ、１．０〜１．５度の時は切削可能長が４９８ｍ以上と更に１．８倍以上長く、更に優れた工具寿命が得られることがわかる。また、六方晶グラファイトの（００８）Ｘ線回折ピークのシフト量が低角側に０．１〜１．５度であるとき切削可能長が２７０ｍ以上と長く、優れた工具寿命が得られ、０．５〜１．０度の時は切削可能長が４５０ｍ以上と更に１．６倍以上長く、更に優れた工具寿命が得られることがわかった。
【００２０】
（実施例５）
超硬合金材の表面にダイヤモンド膜を形成し、ＤＬＣ膜を被覆する影響を明らかにするため、従来例３９として、実施例４と同一ロットで作製したスクエアエンドミル型の切削工具用超硬合金基体と分析用直方体基板を真空装置内にセットし、実施例４と同じ条件でダイヤモンド膜を成膜した後、その表面にＤＬＣ膜を成膜しないせず、製作した。従来例３９のラマンスペクトルは１３３２ｃｍ−１付近のダイヤモンドの鋭いピークと１５８０ｃｍ−１付近のグラファイトの鋭いピークのみが検出され、両ピーク付近にブロードなピークを示すＤＬＣは観察されなかった。また、ダイヤモンド成分の（４００）Ｘ線回折ピーク位置は高角側に０．１度シフトし、六方晶グラファイト成分の（００８）Ｘ線回折ピーク位置はシフトしていなかった。従来例３９のスクエアエンドミル３本の用いて実施例４と同一の条件で工具寿命を評価した結果、８５ｍ以内で外周刃の刃先摩耗量が０．０５ｍｍに達した。この結果、ダイヤモンド成分の（４００）Ｘ線回折ピーク位置と六方晶グラファイトの（００８）Ｘ線回折ピーク位置の両シフト量が同じであるダイヤモンド膜の表面にＤＬＣ膜を形成した本発明例２２よりも工具寿命が１／２以下と短く、工具として劣っていることがわかった。即ち、ダイヤモンド膜の表面にＤＬＣ膜を形成した本発明例２２〜３８は、同じダイヤモンド膜の表面にＤＬＣ膜を形成していない従来例３９に比べて、２倍以上工具寿命が優れていることがわかった。
【００２１】
【発明の効果】
本発明を適用することによって、結晶性が良く耐摩耗性の優れたダイヤモンド膜表面の摺動性が高まることにより、耐摩耗性と摺動性の両者が優れ、格段に工具寿命の長い硬質炭素膜被覆工具を実現できる。[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a tool coated with a hard carbon film.
[0002]
[Prior art]
With the high hardness and light weight of the workpiece, there is an increasing trend to utilize cutting tools and wear-resistant members coated with a diamond film having high hardness and high thermal conductivity. In particular, diamond-coated tools are promising for processing aluminum alloys and graphite materials, and are being actively studied. Patent Documents 1 to 4 below disclose diamond coated tools.
[Patent Document 1] JP-A-8-259391 (Table 1 on page 9, Table 2 on page 10)
[Patent Document 2] JP-A-2001-179504 (Table 5 on page 5, Table 7 on page 7)
[Patent Document 3] JP-A-2001-328007 (Table 6 on page 6, Table 3 on page 7)
[Patent Document 4] JP-A-2003-25117 (page 2, claims 1 and 2)
[0003]
Patent Literature 1 discloses that the surface of the film is smoothed by using diamond having an X-ray diffraction peak intensity of (220) which is stronger than other peaks, thereby improving the slidability. However, when the crystallinity and slidability of only these diamond components are modified, a good balance of wear resistance and slidability of the entire hard film is not sufficiently achieved, and a sufficient tool as a coated tool is not obtained. There was a drawback that the life could not be obtained. Patent Literatures 2 and 3 disclose coating a hard carbon film containing both diamond having a strong (400) plane orientation and hexagonal graphite having a strong (008) plane index with an X-ray diffraction peak intensity. Tools with excellent tool life are disclosed. Patent Document 4 discloses a coated cutting tool combining a diamond coating film and a protective film having lubricity, and discloses a technique using a hard carbon film as the protective film.
[0004]
[Problems to be solved by the invention]
The problem to be solved by the present invention is to realize a coated tool having both excellent wear resistance and slidability by enhancing the slidability of the diamond film surface having good crystallinity and excellent wear resistance, An object of the present invention is to provide a hard carbon film-coated tool having a significantly longer tool life than conventional tools.
[0005]
[Means for Solving the Problems]
The inventors of the present invention have made intensive studies to solve the above-mentioned problems. As a result, the surface of a cemented carbide material is coated with a diamond film, and the 2θ value of the X-ray diffraction peak of the (400) plane index of the diamond film is 0. The diamond film surface is coated with a diamond-like carbon film, and the 2θ value of the X-ray diffraction peak of the (008) plane index of the diamond film is low by 0.1 degree or more. The present inventors have found that a tool having an excellent tool life can be realized by using a hard carbon film-coated tool characterized by containing a hexagonal graphite component shifted to the corner side, and reached the present invention.
BEST MODE FOR CARRYING OUT THE INVENTION
[0006]
The present invention is a hard carbon film-coated tool characterized in that a diamond film is formed on a surface of a cemented carbide material and then the surface is coated with a diamond-like carbon (hereinafter referred to as DLC) film. As a result, a diamond film having high hardness and particularly excellent wear resistance is formed on the surface of a cemented carbide material having excellent toughness and wear resistance, and DLC having high sliding characteristics is formed on the surface. By forming the film, a hard carbon film-coated tool having excellent cutting characteristics and a long tool life can be realized. Generally, since the DLC film is formed at a low temperature of around 200 ° C., it has low adhesion to a substrate and a lower layer film, and has a disadvantage that it is easily peeled off when used as a cutting tool. However, in the present invention, the DLC film is formed on the surface of the diamond film made of the same carbon, so that the DLC film has excellent adhesion to the underlayer film, and the DLC film does not come off during the cutting process, and has particularly excellent sliding characteristics. Show. The formation of a diamond film, a DLC film, or the like on the substrate surface can be analyzed by X-ray diffraction, electron beam diffraction, Raman spectroscopy, or the like. Further, when the cross section of the film is analyzed by a scanning electron microscope-energy dispersive X-ray analyzer (SEM-EDX), it can be confirmed from the fact that an amorphous carbon film is formed on the surface of the highly crystalline diamond film. .
[0007]
In the tool coated with a hard carbon film of the present invention, it is necessary that the 2θ value of the X-ray diffraction peak of the (400) plane index of the diamond film is shifted to a higher angle side by 0.1 degree or more. By doing so, the slidability of the diamond film is enhanced, and a hard carbon film-coated tool having excellent cutting characteristics can be realized in combination with the excellent wear resistance inherent in diamond. This is considered because the 2θ value of the X-ray diffraction peak of the (400) plane index was shifted to the higher angle side by 0.1 degree or more, so that the bondability with the DLC component and the hexagonal graphite component was increased. When the shift amount of the 2θ value is less than 0.1 degree, a disadvantage that the tool characteristics are deteriorated appears. This is probably because the bonding force between the diamond component and the DLC component or the hexagonal graphite component is reduced.
[0008]
The hard carbon film-coated tool of the present invention contains a hexagonal graphite component in which the 2θ value of the X-ray diffraction peak of the (008) plane index of the diamond film is shifted to the lower angle side by 0.1 ° or more. Is preferred. By doing so, the diamond film contains a hexagonal graphite component having excellent slidability and also has an excellent bonding property with the diamond component, so that wear resistance and sliding resistance are improved. The hard carbon film-coated tool, which is particularly excellent in both properties and is stable and has more excellent cutting characteristics, can be realized. This is because the 2θ value of the X-ray diffraction peak of the (008) plane index of the hexagonal graphite component is shifted to the lower angle side by 0.1 degree or more, and therefore, the atomic It is considered that there is interference such as sharing, and a strong bonding force acts between the diamond component and the graphite component. For this reason, both excellent wear resistance, which is a characteristic of diamond, and excellent sliding characteristics, which is a characteristic of graphite, are simultaneously obtained, and it is judged that excellent tool characteristics are exhibited. When the shift amount of the hexagonal graphite component is less than 0.1 degree, there is a disadvantage in that the tool characteristics are deteriorated. This is thought to be due to a decrease in the bonding force between the diamond component and the hexagonal graphite component.
An example of a hard carbon film-coated end mill which is a typical example of the hard carbon film-coated tool in the present invention will be described. In the coated tool of the present invention, the X-ray diffraction peak of diamond is identified using the X-ray diffraction data file No. 6-0675 of the JCPDS file, and the X-ray diffraction peak of hexagonal graphite is identified using the same file number 25-284. Was performed using the above data. In order to manufacture the diamond film of the coated tool of the present invention, a known CVD method such as a hot filament CVD method, a microwave CVD method, an rf plasma CVD method, and an ECR plasma CVD method can be used. Must be adjusted appropriately. In the study of the present inventors, the diamond (400) X-ray diffraction peak shifts to a higher angle side and the (008) X-ray diffraction peak of graphite shifts to a lower angle side as the substrate temperature during film formation is increased. I do. Further, as the CH 4 / H 2 ratio of the film forming gas is lowered, the amount of shift of the (400) X-ray diffraction peak of diamond toward the high angle side and the amount of shift of the (008) X-ray diffraction peak of graphite toward the low angle side are reduced. Has been found to be smaller. In order to manufacture the DLC film of the coated tool of the present invention, an rf plasma CVD method using a gas reaction, a microwave CVD method, an ECR plasma CVD method, or a physical vapor deposition (PVD) method using a carbon target is used. Although it can be used, it is preferable to form the film by a CVD method because higher adhesion can be obtained between the diamond film and the DLC film. The application of the present invention is not limited to a solid end mill type cutting tool, but may be an end mill type cutting tool, a milling tool, or a turning tool using a throw-away insert. Further, a wear-resistant material, a mold, a molten metal part, or the like coated with a hard carbon film may be used. In the coated tool of the present invention, the component of the hard carbon film is not limited to only carbon. It is permissible to include inevitable additives and impurities such as Co and W, for example, up to about several mass% within a range where the effects of the present invention are not lost. Next, the coated tool of the present invention will be specifically described with reference to examples, but the present invention is not limited to these examples.
[0010]
【Example】
(Example 1)
WC: 94% by mass, Co: 6% by mass, cemented carbide substrate for cutting tool of 6 mm in diameter, 2-flute ball end mill type cutting tool manufactured by sintering in the same lot, 10 mm x 10 mm, thickness A 5 mm rectangular parallelepiped substrate for analysis was set in a vacuum apparatus, and a diamond film having a thickness of about 8 μm was formed on the surface thereof by hot filament CVD. That is, by flowing an electric current through a tungsten filament disposed around the end mill, the tungsten filament is heated to about 2500 ° C. and mixed with CH 4 and H 2 having a CH 4 / H 2 ratio of 0.5 to 3%. A gas was flowed at a flow rate of 10 to 150 cm 3 / min, and a film was formed at a pressure of 1.33 to 13.3 kPa and a substrate temperature of 900 to 1200 ° C. By a rf plasma CVD method, C 2 H 2 gas and H 2 were flowed in a vacuum apparatus, and a DLC film having a thickness of 0.5 μm was formed at a gas pressure of 10.7 Pa, a substrate temperature of 200 ° C., and a substrate bias of 800 V. The X-ray diffraction patterns of the prepared samples were evaluated using the above-mentioned analysis substrate formed together with each sample. The X-ray diffraction apparatus manufactured by Rigaku Denki (Ltd.) (RU-200BH type), the wavelength λ by using the CuKa 1 line of 0.15405 nm, was determined by 2 [Theta]-theta scan technique. The measurement range of 2θ was 10 to 145 degrees, and the background noise was removed by software built in the apparatus. Table 1, 2 [Theta] value listed in the JCPDS file of each substance (2 [Theta] 0), the shift amount Δ2θ from standard 2 [Theta] 0 in plane index and the present invention Example 1 X-ray diffraction measurements and the measured 2θ (2θ-2θ 0 ) is also shown. Table 1 shows that the amount of shift between the (400) X-ray diffraction peak position of diamond and the (008) X-ray diffraction peak position of hexagonal graphite is particularly large. Since the DLC film is amorphous, but definite X-ray diffraction peaks were detected, the DLC film is actually deposited is broad near 1580 cm -1 and near 1360 cm -1 in the Raman spectrum It was confirmed from the fact that a peak was detected.
[0011]
[Table 1]
Table 2 summarizes the results of X-ray diffraction measurement and the tool life of the hard carbon film-coated tools of Examples 2 to 19 of the present invention produced in Example 1.
[0013]
[Table 2]
From Table 2, it can be seen that the shift amount Δ2θ of the (400) X-ray diffraction peak of diamond shows a positive value in all the samples of Invention Examples 2 to 19, and is shifted by 0.1 ° or more to the high angle side. Understand. The shift amount Δ2θ of the (008) X-ray diffraction peak of hexagonal graphite shows a negative value, indicating that the peak is shifted to the lower angle side. Here, the diamond (400) X-ray diffraction peak shifts to a higher angle side as the substrate temperature at the time of film formation is increased within the range of 900 to 1200 ° C., and the graphite (008) X-ray diffraction peak shifts to a lower angle. Shifted to the side. Further, as the CH 4 / H 2 ratio of the film-forming gas is lowered within the range of 0.5 to 3%, the shift amount of the (400) X-ray diffraction peak of diamond toward the high angle side and the (008) X-ray of graphite are increased. The shift amount of the diffraction peak to the lower angle side became smaller. The tool life of each of the inventive examples 2 to 19 is such that the graphite material is cut under the following conditions using each of the three inventive examples manufactured until the flank wear of the cutting edge of the outer peripheral edge reaches 0.1 mm. This is indicated by the cutting length.
Work material: Graphite (HS95)
Tool shape: Ball end mill (φ6, 2 flutes)
Tool rotation speed: 10,000 rotations / min
Cutting speed: 188m / min
Feeding speed: 2000 mm / min (0.1 mm / tooth)
Cut: 0.3mm × 0.3mm
Cutting oil: Abrasion resistance of a tool can be evaluated at an early stage by using a graphite material having a Shore hardness of HS95 as a work material without using it. The flank wear was measured using a stereo microscope with a magnification of 100 and a slide table with a resolution of 1 μm. From Table 2, it can be seen that Examples 2 to 19 of the present invention all have a long cuttable length of 710 m or more, and have excellent tool life. Further, when the shift amount of the (400) X-ray diffraction peak of diamond is 0.5 to 2.0 degrees on the high angle side, the cuttable length is 1430 m or more, twice or more, and an excellent tool life is obtained, When the angle is 1.0 to 1.5 degrees, the cuttable length is 2590 m or more, which is 1.8 times or more, which indicates that a more excellent tool life can be obtained. Further, when the shift amount of the (008) X-ray diffraction peak of hexagonal graphite is −0.1 to −1.5 degrees on the low angle side, the cuttable length is 1430 m or more, twice as long, and excellent tool life is obtained. When -0.5 to -1.0 degrees, the cuttable length is 2150 m or more, which is 1.5 times or more longer, indicating that a more excellent tool life can be obtained.
[0015]
(Example 2)
In order to clarify the effect of forming a diamond film on the surface of a cemented carbide material and further covering the DLC film, a cemented carbide substrate for a cutting tool of a ball end mill and a rectangular parallelepiped substrate for analysis were manufactured in the same lot as in Example 1. Was set in a vacuum apparatus, a diamond film was formed under the same conditions as in Example 1, and a conventional example 20 in which a DLC film was not formed on the surface was produced. Raman spectra of the conventional example 20 is only sharp peak of graphite near sharp peaks and 1580 cm -1 of the diamond near 1332 cm -1 is detected, DLC showing a broad peak in the vicinity of both peaks were observed. The position of the (400) X-ray diffraction peak of the diamond component was shifted by 0.1 degree to the higher angle side, and the position of the (008) X-ray diffraction peak of the hexagonal graphite component was not shifted. The tool life was evaluated under the same conditions as in Example 1 using three ball end mills of Conventional Example 20, and as a result, the wear amount of the outer peripheral edge reached 0.05 mm within 300 m. As a result, the DLC film was formed on the surface of the diamond film having the same shift amount between the (400) X-ray diffraction peak position of the diamond component and the (008) X-ray diffraction peak position of the hexagonal graphite. It was also found that the tool life was as short as 1/2 or less, which was inferior as a tool. That is, Examples 2 to 19 of the present invention in which the DLC film was formed on the surface of the diamond film had a tool life more than twice as long as that of Conventional Example 20 in which the DLC film was not formed on the surface of the same diamond film. I understand.
[0016]
(Example 3)
In the case where a diamond film is formed on the surface of a cemented carbide material and further coated with a DLC film, the diamond film in which the 2θ value of the (400) plane index X-ray diffraction peak shifts to a higher angle side is obtained. In order to clarify the influence on the tool life due to the presence or absence of both the component and the hexagonal graphite in which the 2θ value of the X-ray diffraction peak of the (008) plane index shifts to the low angle side, In Example 21, a cemented carbide substrate for a cutting tool and a rectangular parallelepiped substrate for analysis of a ball end mill having the same composition and shape as in Example 1 were set in a vacuum apparatus, and the surfaces thereof were heated by a hot filament CVD method. A hard carbon film having a thickness of 8 μm was formed. The film formation conditions are a tungsten filament temperature of about 2300 ° C., a mixed gas flow rate of CH 4 and H 2 having a carbon concentration of 4% of 150 cm 3 / min, a pressure of 13.3 kPa, and a substrate temperature of 800 ° C. On this surface, a DLC film having a thickness of 0.5 μm was formed under the same conditions as in Example 1. In the diamond film of Conventional Example 21, the 2θ value of the (400) plane index X-ray diffraction peak of the diamond component was 119.5 degrees, the shift amount to the high angle side was less than 0.1 degree, and the shift amount to the high angle side was small. No shift was observed. Further, confirmation that the DLC film is actually deposited is a broad peak was confirmed to be detected around 1580 cm -1 and near 1360 cm -1 in the Raman spectrum of the sample for analysis. After the cutting test, the cross section of the film was analyzed by SEM-EDX, and it was confirmed from the fact that an amorphous carbon film was formed on the surface of the highly crystalline diamond film. The tool life was evaluated under the same conditions as in Example 1 using three ball end mills of Conventional Example 21. As a result, the wear amount of the outer peripheral edge reached 0.05 mm within 460 m, and the tool life of Example 2 of the present invention was reduced. It stayed below 2/3. By comparing Inventive Example 2 with Conventional Example 21, a DLC film was formed on the surface of a diamond film in which the 2θ value of the (400) plane index X-ray diffraction peak was shifted to the higher angle side by 0.1 ° or more. The tool of Example 2 of the present invention has a tool life 1.6 times or more superior to the tool of Conventional Example 21 in which a DLC film is formed on the surface of a diamond film having a shift amount of 0.1 degree or less. all right.
[0017]
(Example 4)
WC: 95.5% by mass, Co: 4.5% by mass, diameter: 6 mm, 2-flute square end mill type cemented carbide substrate for cutting tool, 10 mm × 10 mm, 5 mm thick rectangular solid for analysis The substrate and the substrate were set in a vacuum apparatus, and a diamond film having a thickness of about 8 μm was formed on the surface thereof by hot filament CVD. That is, by flowing an electric current through a tungsten filament disposed around the end mill, the tungsten filament is heated to about 2500 ° C. and mixed with CH 4 and H 2 having a CH 4 / H 2 ratio of 0.5 to 3%. A film was formed at a pressure of 1.33 to 13.3 KPa and a substrate temperature of 900 to 1200 ° C. by flowing a gas at a flow rate of 10 to 150 cm 3 / min. By a rf plasma CVD method, C 2 H 2 gas and H 2 were flowed in a vacuum apparatus, and a 0.3 μm thick DLC film was formed at a gas pressure of 10.7 Pa, a substrate temperature of 200 ° C., and a substrate bias of 800 V. The X-ray diffraction pattern was measured under the same conditions as in Example 1 using the flat part at the tip of the edge of the square end mill as the sample surface. Since the flat portion at the tip of the edge of the square end mill has a small area, the portion other than the flat portion is removed by processing as much as possible, and by covering with vinyl tape, it is devised so as not to affect the X-ray diffraction pattern. Table 3 summarizes the results of X-ray diffraction measurement and the tool life of the hard carbon film-coated tools of Examples 22 to 38 of the present invention produced in Example 4.
[0018]
[Table 3]
As shown in Table 3, all of the samples of Examples 22 to 38 of the present invention have a diamond component in which the 2θ value of the X-ray diffraction peak of the (400) plane index is shifted by 0.1 degree or more toward the high angle side in the hard carbon film. 008) It can be seen that the 2θ value of the X-ray diffraction peak of the plane index is composed of both hexagonal graphites shifted to the lower angle side by 0.1 ° or more. Further, it is actually deposition DLC film, broad peak Raman spectra near 1580 cm -1 and near 1360 cm -1 of the analytical sample was confirmed to be detected. After the cutting test, the cross section of the film was analyzed by SEM-EDX, and it was confirmed from the fact that an amorphous carbon film was formed on the surface of the highly crystalline diamond film. The tool life of the example of the present invention was evaluated under the following conditions by using each of the manufactured three square end mills of examples 22 to 38 of the present invention.
Work material: Al-9 mass% Si alloy Tool shape: Square end mill (φ6, 2 flutes)
Tool rotation speed: 20000 revolutions / min Cutting speed: 500 m / min Feeding speed: 7.2 m / min (0.18 mm / tooth)
Cut: Ad15mm × Rd0.8mm
Cutting oil: The tool life was not used, and the tool life was indicated by the length of cutting until the flank wear of the cutting edge reached 0.05 mm. Table 3 also shows the tool life. From Table 3, it can be seen that Examples 22 to 38 of the present invention all have a long cuttable length of 180 m or more and have an excellent tool life. In addition, when the shift amount of the (400) X-ray diffraction peak of diamond is 0.5 to 2.0 degrees on the high angle side, the cuttable length is 270 m or more and 1.5 times longer, and an excellent tool life is obtained. When the angle is 1.0 to 1.5 degrees, the cuttable length is 498 m or more, which is 1.8 times or more, which indicates that a more excellent tool life can be obtained. When the shift amount of the (008) X-ray diffraction peak of hexagonal graphite is 0.1 to 1.5 degrees on the low angle side, the cuttable length is as long as 270 m or more, and excellent tool life is obtained. At 0.5 to 1.0 degree, the cuttable length is 450 m or more, which is 1.6 times or more longer, and it can be seen that a more excellent tool life can be obtained.
[0020]
(Example 5)
In order to clarify the effect of forming a diamond film on the surface of a cemented carbide material and covering the DLC film, as a conventional example 39, a cemented carbide substrate for a square end mill type cutting tool manufactured in the same lot as in Example 4 And a rectangular parallelepiped substrate for analysis were set in a vacuum apparatus, a diamond film was formed under the same conditions as in Example 4, and a DLC film was not formed on the surface of the diamond film. Raman spectra of conventional 39 only sharp peak of graphite near sharp peaks and 1580 cm -1 of the diamond near 1332 cm -1 is detected, DLC showing a broad peak in the vicinity of both peaks were observed. The position of the (400) X-ray diffraction peak of the diamond component was shifted by 0.1 degree to the higher angle side, and the position of the (008) X-ray diffraction peak of the hexagonal graphite component was not shifted. The tool life was evaluated under the same conditions as in Example 4 using three square end mills of Conventional Example 39, and as a result, the wear amount of the outer peripheral edge reached 0.05 mm within 85 m. As a result, the DLC film was formed on the surface of the diamond film having the same shift amount between the (400) X-ray diffraction peak position of the diamond component and the (008) X-ray diffraction peak position of the hexagonal graphite. It was also found that the tool life was as short as 1/2 or less, which was inferior as a tool. That is, Examples 22 to 38 of the present invention in which the DLC film was formed on the surface of the diamond film had a tool life twice or more superior to that of Conventional Example 39 in which the DLC film was not formed on the surface of the same diamond film. I understood.
[0021]
【The invention's effect】
By applying the present invention, the slidability of the diamond film surface, which has good crystallinity and excellent wear resistance, is enhanced, so that both the wear resistance and the slidability are excellent, and the hard carbon having a remarkably long tool life. A film-coated tool can be realized.
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| JP2003062702A JP2004268201A (en) | 2003-03-10 | 2003-03-10 | Hard carbon film-coated tool |
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| JP2003062702A JP2004268201A (en) | 2003-03-10 | 2003-03-10 | Hard carbon film-coated tool |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008229755A (en) * | 2007-03-19 | 2008-10-02 | Ookouchi Kinzoku Kk | Cutting tool having dlc coating and its manufacturing method |
| JP2015157338A (en) * | 2014-02-25 | 2015-09-03 | 神奈川県 | Cutting tool and cutting method |
-
2003
- 2003-03-10 JP JP2003062702A patent/JP2004268201A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008229755A (en) * | 2007-03-19 | 2008-10-02 | Ookouchi Kinzoku Kk | Cutting tool having dlc coating and its manufacturing method |
| JP2015157338A (en) * | 2014-02-25 | 2015-09-03 | 神奈川県 | Cutting tool and cutting method |
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