JP4763146B2 - Cutting tool made of sintered silicon nitride - Google Patents
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- JP4763146B2 JP4763146B2 JP2001109155A JP2001109155A JP4763146B2 JP 4763146 B2 JP4763146 B2 JP 4763146B2 JP 2001109155 A JP2001109155 A JP 2001109155A JP 2001109155 A JP2001109155 A JP 2001109155A JP 4763146 B2 JP4763146 B2 JP 4763146B2
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Description
【0001】
【発明の属する技術分野】
本発明は、窒化珪素製切削工具に関し、更に詳しくは、耐欠損性及び耐摩耗性に優れる窒化珪素製切削工具に関する。
【0002】
【従来の技術】
従来より、窒化珪素質焼結体は、高強度、高靭性であり、耐摩耗性、耐熱衝撃性、耐欠損性に優れることが知られている。また、窒化珪素の成形体を焼結と同時に超塑性加工(以下、超塑性鍛造焼結ともいう。)すると高強度、高靭性の窒化珪素焼結体が得られることが知られている(例えば、第2923781号公報、第2944953号、及び特開平5−221738号公報等)。しかし、これらの焼結体は切削工具を目的とするものではい。更に、この焼結体は、強度の弱い面を有しており、どのように使用すれば切削工具材料として有用であるかということは全く知られていなかった。
【0003】
また、焼成中に塑性流動させて粒子を配向させるといった記載はないが、強度、靭性、耐チッピング性の向上を目的とした切削工具として、特開平8−112705号公報等が挙げられる。この切削工具は、柱状で粗大なβ窒化珪素粒子の軸を切削工具のすくい面に対して平行方向に2次元配向させることで、上記の性能を向上させている。しかし、粒子の配向方法が粗大な柱状のβ窒化珪素粒子を添加して焼成前に配向させているため、残留ポア、残留応力の影響により強度が1100MPa程度で停滞してしまい、切り込み量を増やした場合、耐欠損性に劣ってしまう。このため、耐欠損性、耐摩耗性等に優れ、より高寿命な切削工具が望まれていた。
【0004】
【発明が解決しようとする課題】
本発明は、上記実情に鑑みてなされたものであり、耐欠損性及び耐摩耗性のいずれにも優れる窒化珪素質焼結体製切削工具を提供するものである。
【0005】
【課題を解決するための手段】
本発明者等は、耐欠損性及び耐摩耗性のいずれにも優れる窒化珪素質焼結体製切削工具について検討した結果、本発明を完成するに至った。
即ち、予備成形体を超塑性鍛造焼結により残留ポアを除去すること、及び/又は切削工具のすくい面を特定方向に設定すること、並びに結晶粒子の配向度を設定することによって、特定方向の強度、靭性を向上させることができ、切削工具とした場合に優れた耐欠損性及び耐摩耗性が得られることを見出したものである。
【0006】
本発明の窒化珪素質焼結体製切削工具は、窒化珪素系原料粉末を圧粉成形してなる予備成形体を圧縮焼成により、結晶粒を塑性流動させて結晶粒の配向方向を特定方向に制御した窒化珪素系焼結体からなり、圧縮軸方向に対して垂直となる面をすくい面とし、それ以外の面を逃げ面とする切削工具であって、上記すくい面において、下記式(1)で表されるX線回折ピークの強度比Rが0.90〜1であり、且つ上記逃げ面の少なくとも一方において、該強度比Rが0.10〜0.80であることを特徴とする。
R=I (200) /(I (200) +I (002) ) (1)
[但し、I (200) 、I (002) は、それぞれβ窒化珪素及び/又はβサイアロンの(200)面、(002)面の反射強度を示す。]
【0007】
上記「窒化珪素系原料粉末」は、特に限定されるものではないが、焼結体の結晶粒が異方粒成長する必要があるという点から、焼成温度域で超塑性変形させるために液相焼結するものが好ましい。通常、α窒化珪素粉末、αサイアロン粉末、β窒化珪素粉末、及びβサイアロン粉末のうちの少なくとも1種と、焼結助剤粉末とが用いられる。
上記α窒化珪素粉末、αサイアロン粉末、β窒化珪素粉末、及びβサイアロン粉末の平均粒径は0.1〜2μmであることが好ましい。また、これらの粉末の比表面積は5〜15g/m2であることが好ましい。
【0008】
上記焼結助剤粉末は、特に限定されるものではなく、焼結温度域で液相を形成する化合物であればよい。通常、金属元素を含む酸化物(例えば、酸化イットリウム、酸化アルミニウム、酸化マグネシウム及び酸化ジルコニウム等)、炭化物(例えば、炭化ジルコニウム、炭化チタン及び炭化タングステン等)、及び窒化物(例えば、窒化アルミニウム、窒化チタン及び窒化イットリウム等)等の粉末が用いられる。
これらの焼結助剤粉末の比表面積は5〜35g/m2であることが好ましい。これらの焼結助剤粉末は、単独で用いてもよいし、2種以上を混合して用いてもよい。
【0009】
上記「予備成形体」は、所定の窒化珪素系原料粉末を圧粉成形して得られる。上記圧粉成形は、原料粉末を加圧すればよく、この加圧方法としては、例えば、CIP(冷間静水圧プレス)、金型プレス及びラバープレス等が挙げられる。圧粉成形する際の温度、圧力等の成形条件は原材料の種類、所望の形状等により適宜調整される。更に、射出成形、鋳込み成形等、原料粉末をそのまま成形できる方法であれば適宜調製される。
【0010】
上記「窒化珪素系焼結体」は、上記予備成形体を焼結と同時に圧縮して塑性流動(超塑性鍛造焼結)させて得られるものであり、結晶粒の配向方向が特定方向に制御されたものである。このため、圧縮面に対して針状又は柱状粒子の長軸が平行に配向され、長軸の配向がランダムな組織の焼結体より圧縮面の強度、靭性を飛躍的に向上させることができる。更に、粗大なβ窒化珪素粒子を焼結前に添加して配向させて作製した焼結体より粒径が小さく、且つ残留ポアが除去され、高強度、高靭性のものが得られ、耐欠損性に優れる切削工具とすることができる。
【0011】
上記超塑性鍛造焼結する方法としては、熱間圧縮加工、熱間圧延加工及び熱間押出し加工等が挙げられる。この際、上記予備成形体は、側面の拘束がない状態、若しくは一組以上の側面の変形が拘束されるように型に入れられる。また、超塑性鍛造焼結する際の温度、圧力等の成型条件は予備成形体の形状、所望の形状等により適宜調整される。
例えば、熱間圧縮加工による場合、焼結温度1500〜2000℃、成形圧力2〜100MPa、窒素気圧1〜10atmの条件で超塑性鍛造焼結を行うことができる
この窒化珪素系焼結体の相対密度は、通常、97〜100%(好ましくは98〜100%)である。
【0012】
本発明の切削工具は、塑性流動させる際の圧縮軸方向に垂直となる面を、すくい面とする。この場合、切削工具が欠損する際のクラック進展方向と結晶粒の軸とが垂直になるため、耐欠損性を向上させることができる。
【0013】
他の本発明の窒化珪素質焼結体製切削工具は、窒化珪素質焼結体からなる切削工具であって、該切削工具のすくい面における結晶粒の長軸が、該すくい面に対して平行方向に制御されており、上記すくい面において、下記式(1)で表されるX線回折ピークの強度比Rが0.90〜1であり、且つ該すくい面以外の面を逃げ面としたときに該逃げ面の少なくとも一方において、該強度比Rが0.10〜0.80であることを特徴とする。
R=I (200) /(I (200) +I (002) ) (1)
[但し、I (200) 、I (002) は、それぞれβ窒化珪素及び/又はβサイアロンの(200)面、(002)面の反射強度を示す。]
【0014】
上記切削工具は、すくい面における結晶粒の長軸が、このすくい面に対して平行方向に制御されている。このため、切削工具が欠損する際のクラック進展方向と結晶粒の長軸が垂直になり、耐欠損性が向上させることができる。
また、上記焼結体は、切削工具とした場合に、すくい面における結晶粒の長軸が、このすくい面に対して平行方向に制御されている。この焼結体は、前述の窒化珪素系原料粉末等を用いることができ、例えば、前述の超塑性鍛造焼結により作製することができる。
【0015】
上記本発明と、上記他の本発明の両発明における、上記すくい面において、下記式(1)に示すX線回折ピークの強度比Rが0.90〜1(より好ましくは0.95〜1)であり、且つ少なくとも逃げ面の一方において、強度比Rが0.10〜0.80(より好ましくは0.15〜0.75)である。
R=I(200)/(I(200)+I(002)) (1)
[但し、I(200)、I(002)は、それぞれβ窒化珪素及び/又はβサイアロンの(200)面、(002)面の反射強度を示す。]
この強度比Rが1の場合はβ窒化珪素及び/又はβサイアロン結晶の長軸(以下c軸ともいう)が測定面に対して全ての粒子において平行であることを意味し、Rが0の場合は、β窒化珪素結晶のc軸が測定面に対して全ての粒子において垂直であることを意味している。
【0016】
このすくい面の強度比Rが0.90未満であると、すくい面に対してc軸が垂直となるβ窒化珪素及び/又はβサイアロンの粒子数が増加するため、すくい面の強度が低下し、耐欠損性も低下する。また、少なくとも一方の逃げ面の強度比Rが0.80より大きいと、逃げ面とc軸が平行となるβ窒化珪素及び/又はβサイアロンの粒子数が増加し、その逃げ面と垂直方向のすくい面強度が低下するため耐欠損性が低下することがある。また、一方の逃げ面の強度比Rが0.10未満であると、他方の逃げ面におけるc軸が平行となるβ窒化珪素及び/又はβサイアロンの粒子数が増加し、その逃げ面と平行方向のすくい面強度が低下し、耐欠損性が低下することがある。
【0017】
また、両発明の切削工具は、断面が高さ3mm、幅4mmの曲げ試験片を用いたスパン16mmの3点曲げ強度試験法において、上記すくい面の強度が1200MPa以上、(好ましくは1300MPa以上、より好ましくは1400MPa以上)とすることができる。
更には、試験片の形状、スパンの長さ等が異なる他の3点曲げ或いは4点曲げ強度試験(例えば、JIS R 1601の曲げ強度試験)においても、有効体積換算に基づき、本強度試験法の強度と同等若しくはそれ以上のものとすることができる。尚、有効体積は下記数式(2)を用いて求めることができ、更に下記数式(3)を用いることで、本発明における強度試験法による有効体積(V1)及び強度(σ1)と、上記他の方法による有効体積(V2)及び強度(σ2)との相関を求めることができる。
【0018】
【数1】
【0019】
[但し、VE:有効体積、b:試験片の幅、h:(試験片の高さ)/2、L1:(外スパン−内スパン)/2、L2:内スパン、m:ワイブル係数を示す。]
【0020】
【数2】
【0021】
[但し、σ1,σ2:平均強度、V1,V2:有効体積、m:ワイブル係数を示す。]
【0022】
更に、両発明の切削工具は、下記実施例の耐欠損性を評価する切削試験において、加工山数が10個以上(好ましくは14個以上)であるものとすることができる。
【0023】
また、両発明の切削工具は、常圧焼結及びガス圧焼結により作製される同一組成の切削工具の耐摩耗量を1とした場合に、この耐摩耗量が0.95以下(好ましくは0.90以下、より好ましくは0.70以下)であるものとすることができる。但し、耐摩耗量は下記実施例の評価方法によるものとする。
【0024】
【発明の実施の形態】
以下、実施例により、本発明を更に詳しく説明する。
実施例1
(1)窒化珪素質焼結体製切削工具(実験例1、2、4及び5)
原料粉末としてα窒化珪素粉末(宇部興産株式会社製、「E−10」、比表面積;10m2/g、平均粒径;0.5μm)と、焼結助剤成分粉末[酸化イットリウム(比表面積;10m2/g)、酸化アルミニウム(比表面積;13m2/g)、酸化マグネシウム(比表面積;30m2/g)、酸化セリウム(比表面積;10m2/g)、酸化ジルコニウム(比表面積;10m2/g)]とを、表1の所定の量比となるように配合し、エタノール中でボールミルを用いて40時間湿式粉砕混合を行った。
得られたスラリーを500メッシュのふるいを通し、溶媒を除去し粉末を回収した後、50メッシュのふるいを用い、造粒粉を得た。これを一軸加圧成形した後、196MPaでCIP(冷間静水圧プレス)処理を行い、40×20×30mmの予備成形体を得た。得られた予備成形体を、一組の側面が変形を拘束するように底面60×20mmのカーボンダイスに入れ、焼結と同時に圧縮加工した。熱間圧縮加工は、1650〜1750℃、窒素9atm下、圧縮荷重36kN(最終圧力30MPa)の条件で、3時間行った。得られた焼結体は約60×20×10mmで、密度は理論密度比で95〜99%程度であった。
その後、焼結体から圧縮軸に垂直な面(以下、N面という。)がすくい面、塑性流動した方向に垂直な面(以下、E面という。)と変形を拘束した面(以下、T面という。)とが逃げ面になるように、所定の工具形状(ISO SNGN432型、サイズ;縦12.7mm、横12.7mm、高さ4.76mm)に加工した。
【0025】
(2)窒化珪素質焼結体製切削工具(実験例3及び6)
上記(1)と同様の原料粉末を用いて、上記(1)と同様に予備成形体を作製し、1650〜1700℃、窒素ガス中で常圧焼結した後、更に1600℃〜1800℃、窒素75atm下でガス圧焼結して得られた焼結体を所定の工具形状(ISO SNGN432型)となるように加工した。
【0026】
【表1】
【0027】
(3)切削工具の評価(実験例1〜6)
上記(1)及び(2)で得られた各々の切削工具の耐欠損性及び耐摩耗性を以下の条件による切削試験により評価した。これらの結果をそれぞれ表1に併記した。
(耐欠損性の評価方法)
各々の切削工具の逃げ面にチャンファー0.07mmの面取り加工を施し、両端面に鋳砂の残った「FC200」を被削材として、乾式下、切削速度;150mm/min、切り込み;2.0mm、送り速度;1.3mm/revの条件にて切削を同様の条件で3回行った。加工山数は最大15とした。欠損が生じるまでの加工山数が、10個以下を「×」、11〜14個を「○」、15個(欠損が生じず)を「◎」とした。
(耐摩耗性の評価方法)
各々の切削工具の逃げ面にチャンファー0.2mmの面取り加工を施し、両端面に鋳砂の残った「FC200」を被削材として、乾式下、切削速度;300mm/min、切り込み;1.5mm、送り速度;0.34mm/minの条件にて切削を行い、フランク最大摩耗量を測定し、これを逃げ面摩耗量(mm)とした。
【0028】
(4)評価結果(実験例1〜6)
表1によれば、常圧焼結及びガス圧焼結により作製した窒化珪素質焼結体を用いた、実験例3及び実験例6では、それぞれ加工山数が3回とも3個及び2個以下で、耐欠損性が「×」であった。
これに対して、超塑性鍛造焼結により作製した焼結体を用い、前逃げ面となる面をE面とした実験例1及び実験例4、及び前逃げ面となる面をT面とした実験例2及び実験例5では、すべてにおいて加工山数が3回とも15個で欠損せず、耐欠損性が「◎」と優れていた。
また、同一組成である実験例1〜3のフランク摩耗量を比較してみると、本発明の範囲外の実験例3では2.32mmであるのに対して、本発明の範囲内の実験例1、2では、それぞれ1.46mm(実験例3の耐摩耗量:実験例1の耐摩耗量=1:0.63)、2.18mm(実験例3の耐摩耗量:実験例2の耐摩耗量=1:0.94)と耐摩耗性に優れていた。
更に、同一組成である実験例4〜6のフランク摩耗量を比較してみても、と、本発明の範囲外の実験例6では、1.03mmであるのに対して、本発明の範囲内の実験例4、5では、それぞれ0.41mm(実験例6の耐摩耗量:実験例4の耐摩耗量=1:0.40)、0.9mm(実験例6の耐摩耗量:実験例5の耐摩耗量=1:0.88)と耐摩耗性に優れていた。
上記のことから、実験例1、2、4及び5は、耐欠損性及び耐摩耗性の両方の性能において優れていることが分かった。
【0029】
実施例2
(1)窒化珪素質焼結体製切削工具の作製(実験例7〜11)
β窒化珪素の配向による影響を確認するため、実施例1の実験例4と同一組成、同一方法で調製した粉末を用いて、表2に示す形状の予備成形体を作製し、熱間圧縮加工してβ窒化珪素及び/又はβサイアロンの配向度の異なる焼結体(形状;N方向60mm、T方向20mm、E方向6.5〜15mm)を得た。得られた焼結体を所定の工具形状(ISO SNGN432型)となるように加工した。
【0030】
(2)窒化珪素質焼結体製切削工具の作製(実験例12及び13)
上記(1)と同一組成の造粒子を用いて、表2に示す形状の予備成形体を作製し、1600〜1700℃、窒素ガス中で常圧焼結した後、更に1600℃〜1800℃、窒素75atm下でガス圧焼結した焼結体(形状;N方向32mm、T方向16mm、E方向24mm)と、粉末から1700℃でホットプレス焼結した焼結体(形状;N方向60mm、T方向20mm、E方向10mm)を作製し、得られた焼結体を所定の工具形状(ISO SNGN432型)となるように加工した。
【0031】
【表2】
【0032】
(3)切削工具の評価(実験例7〜13)
上記(1)及び(2)で得られた各々の切削工具の耐欠損性、3点曲げ強度、及びX線強度比を以下の条件により測定し、評価した。これらの結果をそれぞれ表2に併記した。更に、実験例9のX線強度比を示すX線チャートを図1に示した。
(耐欠損性の評価方法)
上記実施例1の(3)と同様に評価した。
(3点曲げ強度の評価方法)
すくい面を引張面とし、前逃げ面方向を引張軸とした3×4×20(mm)の試料を切り出して作製し、断面が高さ3mm、幅4mm、スパン16mmの3点曲げ強度を評価した。
【0033】
(X線強度比の測定方法)
β窒化珪素及び/又はβサイアロンの結晶粒の配向度は、以下の条件によるX線回折によって得られたβ窒化珪素及び/又はβサイアロンの(200)面及び(002)面のX線回折ピークの強度比Rを用いて示した。
X線回折装置(理学電機工業社製、「RU−200T」)を使用し、X線源として、CuKα線を用い、X線出力は40kV、100mAとした。測定方法はFT法を用い、スキャンスピード2°/min、ステップ0.02°とした。スリットは、発散スリット0.5degree、散乱スリット0.5degree、受光スリット0.15mmを用いた。ピーク強度は、Kα1とKα2の分離後、Kα1の強度を用いた。
【0034】
(4)評価結果(実験例7〜13)
表2によれば、X線強度比RがN面0.84、T面0.59、E面0.59であり、粉末ホットプレス焼結により作製した窒化珪素質焼結体を用いた実験例12、及びX線強度比が全ての面で0.72であり、常圧焼結及びガス圧焼結により作製した窒化珪素質焼結体を用いた実験例13では、それぞれ加工山数が3回とも5個又は3個以下で、耐欠損性が「×」であった。また、3点曲げ強度においては、実験例12は1400MPaであったが、実験例13では1160MPaと低い値であった。
【0035】
これに対して、超塑性鍛造焼結により作製した焼結体を用いた実験例10(X線強度比R;N面1、T面0.75、E面0.15)及び実験例11(X線強度比R;N面1、T面0.80、E面0.10)では、前逃げ面がE面である場合は、加工山数が3回とも15個で欠損せず、前逃げ面がT面である場合は、加工山数が11〜15個であり、耐欠損性が「○」又は「◎」と優れていた。また、3点曲げ強度は、実験例10では1900MPa(前逃げ面;E面)、1310MPa(前逃げ面;T面)であり、実験例11では、1920MPa(前逃げ面;E面)、1210MPa(前逃げ面;T面)と優れた強度を示し、耐欠損性に優れていることが分かった。
【0036】
更に、超塑性鍛造焼結により作製した焼結体を用いた実験例7(X線強度比R;N面0.95、T面0.50、E面0.48)、実験例8(X線強度比R;N面0.99、T面0.63、E面0.30)及び実験例9(X線強度比R;N面1、T面0.66、E面0.23)では、すべてにおいて加工山数が3回とも15個で欠損せず、前逃げ面に影響されること無く耐欠損性が「◎」とより優れていた。また、3点曲げ強度は、実験例7では1600MPa(前逃げ面;E面)、1580MPa(前逃げ面;T面)、実験例8では、1720MPa(前逃げ面;E面)、1620MPa(前逃げ面;T面)であり、且つ実験例9では、1830MPa(前逃げ面;E面)、1430MPa(前逃げ面;T面)と優れた強度を示し、これらが耐欠損性により優れていることが分かった。
【0037】
特に、すくい面のX線強度比が0.95〜1であり、逃げ面の強度比Rが0.15〜0.75の場合、3点曲げ強度における前逃げ面の違いによる差が少なく、非常に優れた耐欠損性が得られた。
尚、本発明においては、上記実施例に示されたものに限られず、目的、用途に応じて種々変更した実施例とすることができる。
例えば、高い耐欠損性を求められる耐熱合金切削用の工具にも好適である。
【0038】
【発明の効果】
本発明の窒化珪素質焼結体製切削工具は、圧粉成形された予備成形体を超塑性鍛造焼結して得られた、結晶粒の配向方向が制御された焼結体からなることで、特定方向の強度、靭性を向上させることができ、優れた耐欠損性及び耐摩耗性を有する。
他の本発明の窒化珪素質焼結体製切削工具は、窒化珪素質焼結体からなり、切削工具のすくい面における結晶粒の長軸が、すくい面に対して平行方向に制御されているため、特定方向の強度、靭性を向上させることができ、優れた耐欠損性及び耐摩耗性を有する。
【図面の簡単な説明】
【図1】実験例9のN面、T面及びE面の各X線強度比を示すX線チャート図である。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a silicon nitride cutting tool, and more particularly to a silicon nitride cutting tool having excellent fracture resistance and wear resistance.
[0002]
[Prior art]
Conventionally, it is known that a silicon nitride sintered body has high strength and high toughness, and is excellent in wear resistance, thermal shock resistance, and fracture resistance. It is also known that a silicon nitride sintered body having high strength and high toughness can be obtained by superplastic working (hereinafter also referred to as superplastic forging sintering) simultaneously with sintering of a silicon nitride shaped body (for example, No. 2923781, No. 2944953, and Japanese Patent Laid-Open No. 5-221738). However, these sintered bodies are not intended for cutting tools. Furthermore, this sintered body has a weak surface, and it has never been known how to use it as a cutting tool material.
[0003]
Moreover, although there is no description that the particles are oriented by plastic flow during firing, JP-A-8-112705 or the like is cited as a cutting tool for the purpose of improving strength, toughness, and chipping resistance. In this cutting tool, the above-mentioned performance is improved by two-dimensionally orienting the axes of columnar and coarse β silicon nitride particles in a direction parallel to the rake face of the cutting tool. However, since the columnar β-silicon nitride particles are added in a coarse orientation method and oriented before firing, the strength is stagnant at about 1100 MPa due to the effects of residual pores and residual stress, and the amount of cut increases. In such a case, the chipping resistance is inferior. For this reason, a cutting tool which is excellent in fracture resistance, wear resistance and the like and has a longer life has been desired.
[0004]
[Problems to be solved by the invention]
The present invention has been made in view of the above circumstances, and provides a cutting tool made of a silicon nitride sintered body that is excellent in both fracture resistance and wear resistance.
[0005]
[Means for Solving the Problems]
The inventors of the present invention have studied the cutting tool made of a silicon nitride sintered body that is excellent in both fracture resistance and wear resistance. As a result, the present invention has been completed.
That is, by removing residual pores by superplastic forging and sintering the preform and / or setting the rake face of the cutting tool in a specific direction and setting the degree of orientation of crystal grains, It has been found that the strength and toughness can be improved, and excellent chipping resistance and wear resistance can be obtained when a cutting tool is used.
[0006]
The cutting tool made of a silicon nitride based sintered body of the present invention compresses and fires a preform formed by compacting a silicon nitride-based raw material powder to plastically flow the crystal grains so that the crystal grains are oriented in a specific direction. Ri Do from the control the silicon nitride sintered body, and the surface from the rake face perpendicular to the compression axis direction, a cutting tool that flank the other side, in the rake face, the following formula ( The intensity ratio R of the X-ray diffraction peak represented by 1) is 0.90 to 1, and at least one of the flank faces, the intensity ratio R is 0.10 to 0.80, To do.
R = I (200) / (I (200) + I (002) ) (1)
[However, I (200) and I (002) indicate the reflection intensity of (200) plane and (002) plane of β silicon nitride and / or β sialon, respectively. ]
[0007]
The above-mentioned “silicon nitride-based raw material powder” is not particularly limited, but from the viewpoint that the crystal grains of the sintered body need to grow anisotropically, the liquid phase is used for superplastic deformation in the firing temperature range. What is sintered is preferred. Usually, at least one of α silicon nitride powder, α sialon powder, β silicon nitride powder, and β sialon powder and a sintering aid powder are used.
The average particle size of the α silicon nitride powder, α sialon powder, β silicon nitride powder, and β sialon powder is preferably 0.1 to 2 μm. Moreover, it is preferable that the specific surface area of these powders is 5-15 g / m < 2 >.
[0008]
The sintering aid powder is not particularly limited as long as it is a compound that forms a liquid phase in the sintering temperature range. Usually, an oxide containing a metal element (for example, yttrium oxide, aluminum oxide, magnesium oxide, and zirconium oxide), carbide (for example, zirconium carbide, titanium carbide, and tungsten carbide), and nitride (for example, aluminum nitride, nitride) Powders such as titanium and yttrium nitride) are used.
The specific surface area of these sintering aid powders is preferably 5 to 35 g / m 2 . These sintering aid powders may be used alone or in admixture of two or more.
[0009]
The “preliminary body” is obtained by compacting a predetermined silicon nitride-based raw material powder. The compacting may be performed by pressurizing the raw material powder. Examples of the pressurizing method include CIP (cold isostatic pressing), die press, rubber press and the like. Molding conditions such as temperature and pressure when compacting are appropriately adjusted according to the type of raw material, desired shape, and the like. Furthermore, any method that can form the raw material powder as it is, such as injection molding or cast molding, is prepared as appropriate.
[0010]
The above-mentioned “silicon nitride sintered body” is obtained by compressing the preform simultaneously with sintering and plastic flow (superplastic forging sintering), and the crystal grain orientation direction is controlled to a specific direction. It has been done. For this reason, the long axis of needle-like or columnar particles is oriented in parallel to the compression surface, and the strength and toughness of the compression surface can be dramatically improved over a sintered body having a structure in which the long axis orientation is random. . In addition, coarse β-silicon nitride particles are added prior to sintering and oriented to make the particle size smaller, and the residual pores are removed, resulting in high strength and high toughness. It can be set as the cutting tool excellent in property.
[0011]
Examples of the superplastic forging and sintering method include hot compression, hot rolling, and hot extrusion. At this time, the preform is placed in a mold so that side surfaces are not constrained, or deformation of one or more sets of side surfaces is constrained. Further, the molding conditions such as temperature and pressure at the time of superplastic forging and sintering are appropriately adjusted according to the shape of the preform, the desired shape, and the like.
For example, in the case of hot compression processing, relative to this silicon nitride-based sintered body capable of performing superplastic forging sintering under conditions of a sintering temperature of 1500 to 2000 ° C., a molding pressure of 2 to 100 MPa, and a nitrogen pressure of 1 to 10 atm. The density is usually 97 to 100% (preferably 98 to 100%).
[0012]
In the cutting tool of the present invention, a surface perpendicular to the compression axis direction when plastically flowing is a rake surface. In this case, the crack propagation direction when the cutting tool is chipped and the axis of the crystal grain are perpendicular to each other, so that the chipping resistance can be improved.
[0013]
Another cutting tool made of a silicon nitride-based sintered body according to the present invention is a cutting tool made of a silicon nitride-based sintered body, and the major axis of crystal grains in the rake face of the cutting tool is relative to the rake face. In the rake face, the intensity ratio R of the X-ray diffraction peak represented by the following formula (1) is 0.90 to 1, and a face other than the rake face is defined as a flank face. The strength ratio R is 0.10 to 0.80 on at least one of the flank surfaces .
R = I (200) / (I (200) + I (002) ) (1)
[However, I (200) and I (002) indicate the reflection intensity of (200) plane and (002) plane of β silicon nitride and / or β sialon, respectively. ]
[0014]
In the cutting tool, the major axis of crystal grains on the rake face is controlled in a direction parallel to the rake face. For this reason, the crack propagation direction when the cutting tool is chipped and the major axis of the crystal grains are perpendicular to each other, and the chipping resistance can be improved.
Further, the sintered body, when a cutting tool, the long axis of the crystal grains on the rake face, that is controlled in a direction parallel to the rake face. As this sintered body, the aforementioned silicon nitride-based raw material powder or the like can be used, and for example, it can be produced by the aforementioned superplastic forging and sintering.
[0015]
The intensity ratio R of the X-ray diffraction peak represented by the following formula (1) is 0.90 to 1 (more preferably 0.95 to 1) on the rake face in both the present invention and the other inventions of the present invention. And at least one of the flank faces, the strength ratio R is 0.10 to 0.80 (more preferably 0.15 to 0.75).
R = I (200) / (I (200) + I (002) ) (1)
[However, I (200) and I (002) indicate the reflection intensity of (200) plane and (002) plane of β silicon nitride and / or β sialon, respectively. ]
When the intensity ratio R is 1, it means that the major axis (hereinafter also referred to as c-axis) of β silicon nitride and / or β sialon crystal is parallel to the measurement surface in all particles, and R is 0. In this case, it means that the c-axis of the β silicon nitride crystal is perpendicular to all the grains with respect to the measurement surface.
[0016]
If the strength ratio R of the rake face is less than 0.90, the number of β silicon nitride and / or β sialon particles whose c-axis is perpendicular to the rake face increases, so the strength of the rake face decreases. Further, the chipping resistance is also lowered. Further, when the intensity ratio R of at least one flank is larger than 0.80, the number of particles of β silicon nitride and / or β sialon in which the flank and the c-axis are parallel increases, and the flank is perpendicular to the flank. Since the rake face strength is reduced, the chipping resistance may be reduced. If the intensity ratio R of one flank is less than 0.10, the number of β silicon nitride and / or β sialon particles whose c-axis is parallel to the other flank increases and is parallel to the flank. The rake face strength in the direction may be reduced, and the fracture resistance may be reduced.
[0017]
Further, in the cutting tools of both inventions, in the three-point bending strength test method having a span of 16 mm using a bending test piece having a height of 3 mm and a width of 4 mm, the strength of the rake face is 1200 MPa or more (preferably 1300 MPa or more, More preferably, it can be set to 1400 MPa or more.
Furthermore, in the other three-point bending or four-point bending strength test (for example, the bending strength test of JIS R 1601) in which the shape of the test piece, the span length, etc. are different, this strength test method is based on the effective volume conversion. The strength can be equal to or greater than The effective volume can be determined by using the following formula (2), and further by using the following formula (3), the effective volume (V 1 ) and strength (σ 1 ) according to the strength test method in the present invention, The correlation between the effective volume (V 2 ) and the strength (σ 2 ) by the other method can be obtained.
[0018]
[Expression 1]
[0019]
[However, V E : Effective volume, b: Specimen width, h: (Test piece height) / 2, L 1 : (Outer span-Inner span) / 2, L 2 : Inner span, m: Weibull Indicates the coefficient. ]
[0020]
[Expression 2]
[0021]
[However, σ 1 , σ 2 : Average intensity, V 1 , V 2 : Effective volume, m: Weibull coefficient. ]
[0022]
Further, the cutting tools of both inventions can have 10 or more (preferably 14 or more) processing ridges in a cutting test for evaluating fracture resistance in the following examples.
[0023]
The cutting tools of both inventions have a wear resistance of 0.95 or less (preferably, when the wear resistance of a cutting tool of the same composition produced by atmospheric pressure sintering and gas pressure sintering is 1. 0.90 or less, more preferably 0.70 or less). However, the wear resistance is determined by the evaluation method of the following example.
[0024]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, the present invention will be described in more detail by way of examples.
Example 1
(1) Cutting tool made of silicon nitride sintered body (Experimental Examples 1, 2, 4 and 5)
As a raw material powder, α silicon nitride powder (manufactured by Ube Industries, “E-10”, specific surface area: 10 m 2 / g, average particle size: 0.5 μm) and sintering aid component powder [yttrium oxide (specific surface area) 10 m 2 / g), aluminum oxide (specific surface area; 13 m 2 / g), magnesium oxide (specific surface area; 30 m 2 / g), cerium oxide (specific surface area; 10 m 2 / g), zirconium oxide (specific surface area; 10 m) 2 / g)] was mixed so as to have a predetermined quantitative ratio shown in Table 1, and wet pulverized and mixed for 40 hours using a ball mill in ethanol.
The obtained slurry was passed through a 500 mesh sieve, the solvent was removed and the powder was recovered. Then, a granulated powder was obtained using a 50 mesh sieve. After this was uniaxially pressed, a CIP (cold isostatic pressing) process was performed at 196 MPa to obtain a 40 × 20 × 30 mm preform. The obtained preform was put into a carbon die having a bottom surface of 60 × 20 mm so that a set of side surfaces constrains deformation, and was compressed simultaneously with sintering. The hot compression processing was performed for 3 hours under conditions of 1650 to 1750 ° C., 9 atm of nitrogen, and a compression load of 36 kN (
Thereafter, a plane perpendicular to the compression axis (hereinafter referred to as N plane) from the sintered body is a rake face, a plane perpendicular to the direction of plastic flow (hereinafter referred to as E plane), and a plane restraining deformation (hereinafter referred to as T plane). And a predetermined tool shape (ISO SNGN432 type, size: length 12.7 mm, width 12.7 mm, height 4.76 mm).
[0025]
(2) Cutting tool made of silicon nitride sintered body (Experimental Examples 3 and 6)
Using the same raw material powder as in the above (1), a preform is prepared in the same manner as in the above (1), and after sintering at 1650 to 1700 ° C. in nitrogen gas at atmospheric pressure, further 1600 ° C. to 1800 ° C., A sintered body obtained by gas pressure sintering under nitrogen at 75 atm was processed to have a predetermined tool shape (ISO SNGN432 type).
[0026]
[Table 1]
[0027]
(3) Evaluation of cutting tool (Experimental examples 1 to 6)
The cutting resistance and wear resistance of each cutting tool obtained in the above (1) and (2) were evaluated by a cutting test under the following conditions. These results are also shown in Table 1.
(Evaluation method for fracture resistance)
1. Chamfer 0.07mm chamfering is performed on the flank face of each cutting tool, and "FC200" with cast sand remaining on both end faces is used as a work material under a dry process, cutting speed: 150 mm / min, cutting; Cutting was performed three times under the same conditions at 0 mm, feed rate: 1.3 mm / rev. The maximum number of processing peaks was 15. The number of processed ridges until a defect occurs was defined as “x” when 10 or less, “◯” when 11-14, and “◎” when 15 (no defect).
(Abrasion resistance evaluation method)
Chamfer 0.2mm chamfering is performed on the flank face of each cutting tool, and "FC200" with cast sand remaining on both end faces is used as a work material under a dry process, cutting speed: 300 mm / min, cutting; Cutting was performed under the conditions of 5 mm, feed rate: 0.34 mm / min, the maximum flank wear was measured, and this was defined as the flank wear (mm).
[0028]
(4) Evaluation results (Experimental examples 1 to 6)
According to Table 1, in the experimental example 3 and the experimental example 6 using the silicon nitride sintered body produced by atmospheric pressure sintering and gas pressure sintering, the number of processed ridges is 3 and 2 respectively for 3 times. In the following, the fracture resistance was “x”.
On the other hand, using a sintered body produced by superplastic forging sintering, Experimental Example 1 and Experimental Example 4 in which the surface serving as the front flank is the E surface, and the surface serving as the front flank is the T surface In Experimental Example 2 and Experimental Example 5, in all cases, the number of processed ridges was 15 in all, and no chipping occurred, and the chipping resistance was excellent as “◎”.
Further, when comparing the flank wear amounts of Experimental Examples 1 to 3 having the same composition, it is 2.32 mm in Experimental Example 3 outside the scope of the present invention, whereas Experimental Examples within the scope of the present invention. 1 and 2, respectively, 1.46 mm (Abrasion resistance in Experimental Example 3: Abrasion resistance in Experimental Example 1 = 1: 0.63), 2.18 mm (Abrasion resistance in Experimental Example 3: resistance to abrasion in Experimental Example 2) Abrasion amount = 1: 0.94) and excellent wear resistance.
Furthermore, even when the flank wear amounts of Experimental Examples 4 to 6 having the same composition are compared, in Experimental Example 6 outside the scope of the present invention, it is 1.03 mm, but within the scope of the present invention. In Experimental Examples 4 and 5, 0.41 mm (Abrasion resistance in Experimental Example 6: Abrasion resistance in Experimental Example = 1: 0.40), 0.9 mm (Abrasion resistance in Experimental Example 6: Experimental example) No. 5 wear resistance = 1: 0.88) and excellent wear resistance.
From the above, it was found that Experimental Examples 1, 2, 4, and 5 were excellent in both the fracture resistance and the wear resistance.
[0029]
Example 2
(1) Production of cutting tool made of silicon nitride based sintered body (Experimental Examples 7 to 11)
In order to confirm the influence due to the orientation of β silicon nitride, a preform having the shape shown in Table 2 was prepared using the same composition and the same method as in Experimental Example 4 of Example 1, and hot compression processing was performed. As a result, sintered bodies having different orientation degrees of β silicon nitride and / or β sialon (shape:
[0030]
(2) Production of cutting tool made of silicon nitride sintered body (Experimental Examples 12 and 13)
Using the granulated particles having the same composition as the above (1), a preform having the shape shown in Table 2 was prepared, sintered at 1600 to 1700 ° C. under normal pressure in nitrogen gas, and further 1600 to 1800 ° C. Sintered body sintered under gas pressure under nitrogen at 75 atm (shape: 32 mm in N direction, 16 mm in T direction, 24 mm in E direction) and sintered body sintered at 1700 ° C. from powder (shape: 60 mm in N direction,
[0031]
[Table 2]
[0032]
(3) Evaluation of cutting tool (Experimental Examples 7 to 13)
The fracture resistance, the three-point bending strength, and the X-ray strength ratio of each cutting tool obtained in the above (1) and (2) were measured and evaluated under the following conditions. These results are also shown in Table 2. Furthermore, an X-ray chart showing the X-ray intensity ratio of Experimental Example 9 is shown in FIG.
(Evaluation method for fracture resistance)
Evaluation was performed in the same manner as in Example 3 (3).
(Evaluation method of 3-point bending strength)
A 3 x 4 x 20 (mm) sample with the rake face as the tensile surface and the front flank direction as the tensile axis was cut out and evaluated for three-point bending strength with a cross section of 3 mm in height, 4 mm in width, and 16 mm in span. did.
[0033]
(Measurement method of X-ray intensity ratio)
The orientation degree of crystal grains of β silicon nitride and / or β sialon is the X-ray diffraction peak of (200) plane and (002) plane of β silicon nitride and / or β sialon obtained by X-ray diffraction under the following conditions. The intensity ratio R is shown.
An X-ray diffractometer (manufactured by Rigaku Corporation, “RU-200T”) was used, CuKα rays were used as the X-ray source, and the X-ray output was 40 kV and 100 mA. The measurement method was the FT method, with a scan speed of 2 ° / min and a step of 0.02 °. As the slit, a divergence slit of 0.5 degree, a scattering slit of 0.5 degree, and a light receiving slit of 0.15 mm were used. Peak intensity, after separation K [alpha 1 and K [alpha 2, with a strength of K [alpha 1.
[0034]
(4) Evaluation results (Experimental examples 7 to 13)
According to Table 2, the X-ray intensity ratio R is N plane 0.84, T plane 0.59, E plane 0.59, and an experiment using a silicon nitride sintered body produced by powder hot press sintering. In Example 12 and Experimental Example 13 using a silicon nitride-based sintered body produced by atmospheric pressure sintering and gas pressure sintering, the X-ray intensity ratio was 0.72 on all surfaces, The number of defects was 5 or 3 in all, and the chipping resistance was “x”. In addition, in the three-point bending strength, Experimental Example 12 was 1400 MPa, but Experimental Example 13 was a low value of 1160 MPa.
[0035]
On the other hand, Experimental Example 10 (X-ray intensity ratio R; N-plane 1, T-plane 0.75, E-plane 0.15) and Experimental Example 11 (using a sintered body produced by superplastic forging and sintering) X-ray intensity ratio R; N plane 1, T plane 0.80, E plane 0.10), when the front flank is E plane, the number of processed ridges is 15 in all three times, and the front When the flank face was a T-face, the number of processed ridges was 11 to 15, and the fracture resistance was excellent as “◯” or “◎”. The three-point bending strength is 1900 MPa (front flank; E plane) and 1310 MPa (front flank; T plane) in Experimental Example 10, and 1920 MPa (front flank; E plane) and 1210 MPa in Experimental Example 11. (Front flank; T-plane) and excellent strength, it was found that the fracture resistance is excellent.
[0036]
Further, Experimental Example 7 (X-ray intensity ratio R; N plane 0.95, T plane 0.50, E plane 0.48) using a sintered body produced by superplastic forging sintering, Experimental Example 8 (X Line intensity ratio R: N plane 0.99, T plane 0.63, E plane 0.30) and Experimental Example 9 (X ray intensity ratio R; N plane 1, T plane 0.66, E plane 0.23) In all cases, the number of processed ridges was 15 at all three times, and the chip was not broken, and the fracture resistance was more excellent as “「 ”without being affected by the front flank. The three-point bending strength is 1600 MPa (front flank; E surface) and 1580 MPa (front flank; T surface) in Experimental Example 7, and 1720 MPa (front flank; E surface) and 1620 MPa (front) in Experimental Example 8. In Example 9, Experimental Example 9 shows excellent strengths of 1830 MPa (front flank; E surface) and 1430 MPa (front flank; T surface), which are more excellent in fracture resistance. I understood that.
[0037]
In particular, when the X-ray intensity ratio of the rake face is 0.95 to 1 and the flank intensity ratio R is 0.15 to 0.75, there is little difference due to the difference in the front flank in the three-point bending strength, Very good fracture resistance was obtained.
In addition, in this invention, it can be set as the Example variously changed according to the objective and use, without being restricted to what was shown by the said Example.
For example, it is also suitable for a tool for cutting a heat-resistant alloy that requires high fracture resistance.
[0038]
【The invention's effect】
The cutting tool made of a silicon nitride sintered body of the present invention is made of a sintered body in which the orientation direction of crystal grains is controlled, obtained by superplastic forging and sintering of a compacted preform. The strength and toughness in a specific direction can be improved, and it has excellent fracture resistance and wear resistance.
Another cutting tool made of a silicon nitride sintered body of the present invention is made of a silicon nitride sintered body, and the major axis of the crystal grains on the rake face of the cutting tool is controlled in a direction parallel to the rake face. Therefore, the strength and toughness in a specific direction can be improved, and the chip has excellent fracture resistance and wear resistance.
[Brief description of the drawings]
FIG. 1 is an X-ray chart showing the X-ray intensity ratios of N-plane, T-plane, and E-plane in Experimental Example 9;
Claims (5)
上記すくい面において、下記式(1)で表されるX線回折ピークの強度比Rが0.90〜1であり、且つ上記逃げ面の少なくとも一方において、該強度比Rが0.10〜0.80であることを特徴とする窒化珪素質焼結体製切削工具。
R=I (200) /(I (200) +I (002) ) (1)
[但し、I (200) 、I (002) は、それぞれβ窒化珪素及び/又はβサイアロンの(200)面、(002)面の反射強度を示す。] Compression fired preform silicon based raw nitride powder obtained by compacting, Ri grain Do from plastic flow is allowed by the crystal grains of silicon nitride-based sintered body of the orientation direction was controlled in a specific direction of a compression axis A cutting tool having a rake face as a plane perpendicular to the direction and a flank as the other face,
In the rake face, the intensity ratio R of the X-ray diffraction peak represented by the following formula (1) is 0.90 to 1, and in at least one of the flank faces, the intensity ratio R is 0.10 to 0. A cutting tool made of a sintered silicon nitride material, wherein the cutting tool is .80.
R = I (200) / (I (200) + I (002) ) (1)
[However, I (200) and I (002) indicate the reflection intensity of (200) plane and (002) plane of β silicon nitride and / or β sialon, respectively. ]
上記すくい面において、下記式(1)で表されるX線回折ピークの強度比Rが0.90〜1であり、且つ該すくい面以外の面を逃げ面としたときに該逃げ面の少なくとも一方において、該強度比Rが0.10〜0.80であることを特徴とする窒化珪素質焼結体製切削工具。
R=I (200) /(I (200) +I (002) ) (1)
[但し、I (200) 、I (002) は、それぞれβ窒化珪素及び/又はβサイアロンの(200)面、(002)面の反射強度を示す。] A cutting tool comprising a silicon nitride sintered body, wherein the major axis of crystal grains in the rake face of the cutting tool is controlled in a direction parallel to the rake face ,
In the rake face, the intensity ratio R of the X-ray diffraction peak represented by the following formula (1) is 0.90 to 1, and when a face other than the rake face is a flank face, at least the flank face On the other hand, the silicon nitride sintered body cutting tool, wherein the strength ratio R is 0.10 to 0.80 .
R = I (200) / (I (200) + I (002) ) (1)
[However, I (200) and I (002) indicate the reflection intensity of (200) plane and (002) plane of β silicon nitride and / or β sialon, respectively. ]
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| JP2001109155A JP4763146B2 (en) | 2001-04-06 | 2001-04-06 | Cutting tool made of sintered silicon nitride |
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| JP2001109155A JP4763146B2 (en) | 2001-04-06 | 2001-04-06 | Cutting tool made of sintered silicon nitride |
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| JP4763146B2 true JP4763146B2 (en) | 2011-08-31 |
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| CN101087670B (en) * | 2004-12-22 | 2011-07-20 | 日本特殊陶业株式会社 | Saran ceramic inserts and cutting tools equipped with such inserts |
| JP7451350B2 (en) * | 2020-08-24 | 2024-03-18 | 日本特殊陶業株式会社 | End mills and friction stir welding tools |
| CN119076989B (en) * | 2024-07-29 | 2025-04-15 | 岭南师范学院 | A grain-oriented SiAlON ceramic cutting blade and a preparation method thereof |
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| JPH08290972A (en) * | 1995-02-20 | 1996-11-05 | Sumitomo Electric Ind Ltd | Silicon nitride ceramic member and method for manufacturing the same |
| JP2923781B1 (en) * | 1998-06-22 | 1999-07-26 | 工業技術院長 | Sintering and molding method for silicon nitride ceramics |
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