JP4815925B2 - Coated sintered alloy - Google Patents
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Description
本発明は焼結合金の基材に被膜を被覆した被覆焼結合金に関する。その中でも、特にチップ、ドリル、エンドミルに代表される切削工具や各種の耐摩耗工具、耐摩耗部品に好適な被覆焼結合金に関する。 The present invention relates to a coated sintered alloy obtained by coating a sintered alloy substrate with a coating. In particular, the present invention relates to a coated sintered alloy suitable for cutting tools represented by chips, drills, end mills, various wear-resistant tools, and wear-resistant parts.
焼結合金の基材の表面にＴｉＣ、ＴｉＣＮ、ＴｉＮ、（Ｔｉ，Ａｌ）Ｎ、Ａｌ2Ｏ3などの被膜を被覆してなる被覆焼結合金は、基材の高強度、高靱性と被膜の耐摩耗性、耐酸化性、潤滑性、耐溶着性などを兼備しているため、切削工具や耐摩耗工具，耐摩耗部品として多用されている。これまで、被膜の特性を十分に発揮させるために、被膜と基材との間の密着性について改善がなされてきた。このような被覆部材の従来技術としては、炭化タングステン基超硬合金または炭窒化チタン基サーメットからなる基体の表面に、窒化チタンからなる密着性物理蒸着被覆層を介して、ＴｉとＡｌの複合窒化物からなる耐摩耗性物理蒸着被覆層を形成してなる表面被覆サーメット製切削工具がある（例えば、特許文献１参照。）。しかし、これは層間での剥離を起因とする突発的なチッピングや欠損が生じ短寿命になる場合があり、さらなる密着性の改善が求められている。 A coated sintered alloy obtained by coating the surface of a sintered alloy base material with a coating such as TiC, TiCN, TiN, (Ti, Al) N, Al 2 O 3, etc. has a high strength and high toughness of the base material. Because of its wear resistance, oxidation resistance, lubricity, and welding resistance, it is widely used as a cutting tool, wear-resistant tool, and wear-resistant part. Until now, in order to fully exhibit the characteristics of the coating, the adhesion between the coating and the substrate has been improved. As a prior art of such a covering member, composite nitriding of Ti and Al is performed on the surface of a substrate made of tungsten carbide-based cemented carbide or titanium carbonitride-based cermet via an adhesive physical vapor deposition coating layer made of titanium nitride. There is a surface-covered cermet cutting tool formed by forming a wear-resistant physical vapor deposition coating layer made of a material (see, for example, Patent Document 1). However, this may cause sudden chipping or chipping due to delamination between layers, resulting in a short life, and further improvement in adhesion is demanded.
近年、高速度、高送りの過酷な切削条件の要求が増えており、切削中に連続切削から断続切削へと大きく変化する加工条件なども増えている。また製造現場においては無人化が進み、長時間安定した加工ができる工具の要求が多くなっている。そのため信頼性の高く長時間加工できる工具が求められている。そこで本発明は、耐欠損性や耐チッピング性に優れ、長時間安定した加工が可能な被覆焼結合金の提供を目的とする。 In recent years, demands for severe cutting conditions of high speed and high feed are increasing, and machining conditions that greatly change from continuous cutting to intermittent cutting during cutting are also increasing. In addition, unmanned manufacturing is progressing at manufacturing sites, and there is an increasing demand for tools that can perform stable machining for a long time. Therefore, a highly reliable tool that can be processed for a long time is required. Accordingly, an object of the present invention is to provide a coated sintered alloy that is excellent in fracture resistance and chipping resistance and can be processed stably for a long time.
本発明者らは、長年に亘り、被覆焼結合金について研究したところ、被覆前の基材の表面処理を最適化し、基材と被膜との界面における結合相の形状を凸状にすることで、基材と被膜間の剥離が生じにくくなり、その結果、耐欠損性、耐チッピング性が向上し、安定した長寿命加工が可能になることを見出した。 The present inventors have studied the coated sintered alloy for many years. By optimizing the surface treatment of the substrate before coating and making the shape of the binder phase at the interface between the substrate and the coating convex. It has been found that peeling between the substrate and the film is less likely to occur, and as a result, chipping resistance and chipping resistance are improved, and stable long-life processing becomes possible.
本発明は、結合相と硬質相とからなる焼結合金の基材の表面に周期律表４ａ、５ａ、６ａ族元素、Ａｌ、Ｓｉの炭化物、窒化物およびこれらの相互固溶体の中から選ばれた少なくとも１種の被膜を被覆した被覆焼結合金において、被覆焼結合金の断面組織を観察したときに、基材の結合相と被膜との界面の少なくとも１部に、凸状結合相が形成されている被覆焼結合金である。 The present invention is selected from periodic table 4a, 5a, 6a group elements, Al, Si carbides, nitrides and their mutual solid solutions on the surface of a sintered alloy base material comprising a binder phase and a hard phase. Further, in the coated sintered alloy coated with at least one kind of coating, when the cross-sectional structure of the coated sintered alloy is observed, a convex bonded phase is formed in at least a part of the interface between the bonded phase of the substrate and the coated film. It is a coated sintered alloy.
本発明の被覆焼結合金の基材は、Ｃｏ、Ｎｉ、Ｆｅなどの鉄族金属を主成分とする結合相と周期律表４ａ、５ａ、６ａ族元素の炭化物、窒化物およびこれらの相互固溶体の中から選ばれた少なくとも１種の硬質相とからなる焼結合金である。硬質相は、周期律表４ａ、５ａ、６ａ族元素の炭化物、窒化物およびこれらの相互固溶体の中から選ばれた少なくとも１種からなり、ＷＣ、ＴｉＣＮなどを挙げることができる。なお、結合相には、硬質相の成分、すなわち金属元素およびＣ，Ｎが微量固溶することができる。結合相への固溶量は、元素によって異なるが、２０重量％以下である。 The base material of the coated sintered alloy of the present invention includes a binder phase mainly composed of an iron group metal such as Co, Ni, Fe, carbides, nitrides of periodic table elements 4a, 5a, 6a, and mutual solid solutions thereof. Is a sintered alloy composed of at least one hard phase selected from among the above. The hard phase is composed of at least one selected from carbides, nitrides, and mutual solid solutions of Group 4a, 5a, and 6a elements of the periodic table, and examples thereof include WC and TiCN. In the binder phase, the components of the hard phase, that is, metal elements and C, N can be dissolved in a small amount. The amount of solid solution in the binder phase varies depending on the element, but is 20% by weight or less.
本発明の被覆焼結合金は、焼結合金の基材の表面に、周期律表４ａ、５ａ、６ａ族元素、Ａｌ、Ｓｉの炭化物、窒化物およびこれらの相互固溶体の中から選ばれた少なくとも１種の被膜を被覆したもので、被覆焼結合金の断面組織を観察したときに、基材の結合相と被膜との界面の少なくとも１部、すなわち、基材の結合相と被膜との界面の全部またはその一部に凸状結合相が形成されている。凸状結合相が形成されると被膜と基材との密着性が向上する。なお、本発明において断面組織とは、被覆焼結合金の基材の表面に対して任意の垂直断面を観察したときの断面組織をいう。本発明の被覆焼結合金の一実施例の断面組織の概略図を図１に示す。本発明の被覆焼結合金の結合相と被膜との界面の一部には、略三角状の凸状結合相が形成されていることが分かる。 The coated sintered alloy of the present invention is at least selected from the periodic table 4a, 5a, 6a group elements, Al, Si carbides, nitrides and their mutual solid solutions on the surface of the sintered alloy base material. When the cross-sectional structure of the coated sintered alloy is observed, it is at least part of the interface between the binder phase of the substrate and the coating, that is, the interface between the binder phase of the substrate and the coating. A convex binder phase is formed on all or a part thereof. When the convex binder phase is formed, the adhesion between the coating and the substrate is improved. In the present invention, the cross-sectional structure refers to a cross-sectional structure when an arbitrary vertical cross section is observed with respect to the surface of the base material of the coated sintered alloy. A schematic diagram of a cross-sectional structure of an embodiment of the coated sintered alloy of the present invention is shown in FIG. It can be seen that a substantially triangular convex binder phase is formed at a part of the interface between the binder phase and the coating film of the coated sintered alloy of the present invention.
さらに断面組織の拡大した図２に示すように、略三角形状の凸状結合相の高さＨｎ（ｎ＝１，２…）および間隔Ｌｎ（ｎ＝１，２…）を測定し、それらの平均高さＨと平均間隔Ｌを求めたとき、平均高さＨは、０．０５μｍ＜Ｈ＜０．５０μｍの範囲にあり、平均間隔Ｌは、０．０５μｍ＜Ｌ＜０．５０μｍの範囲にあると、基材と被膜との密着性が高くなるため好ましい。なお、Ｈが０．５０μｍ以上になると被膜表面に凹凸を生じ、その凹凸を起点として損傷が進行しやすくなり、Ｈが０．０５μｍ以下であると密着性を向上させる効果が低くなる。Ｌが０．０５μｍ以下では、凸状結合相自体の強度が低下し、Ｌが０．５０μｍ以上であると密着性を向上させる効果が低くなる。 Further, as shown in FIG. 2 in which the cross-sectional structure is enlarged, the height Hn (n = 1, 2,...) And the interval Ln (n = 1, 2,...) Of the substantially triangular convex binder phase are measured. When the average height H and the average interval L were obtained, the average height H was in the range of 0.05 μm <H <0.50 μm, and the average interval L was in the range of 0.05 μm <L <0.50 μm. When it exists, since the adhesiveness of a base material and a film becomes high, it is preferable. When H is 0.50 μm or more, unevenness is generated on the surface of the coating, and damage is likely to proceed starting from the unevenness. When H is 0.05 μm or less, the effect of improving the adhesiveness is reduced. When L is 0.05 μm or less, the strength of the convex binder phase itself decreases, and when L is 0.50 μm or more, the effect of improving the adhesion is reduced.
本発明の被覆焼結合金の被膜は（Ｔｉ，Ａｌ）Ｎを含むと、耐摩耗性に優れることからさらに好ましい。 When the coating of the coated sintered alloy of the present invention contains (Ti, Al) N, it is more preferable because it has excellent wear resistance.
本発明の被覆焼結合金の表面の算術平均粗さＲａが０．０２μｍ＜Ｒａ＜０．３０μｍであるとき、表面の凹凸を起点とする損傷が低減し、より安定した加工が可能となるため好ましい。鏡面処理による焼結合金の表面粗さＲａが０．０２μｍとなり、それ以上の精度での制御が難しいため下限値を０．０２μｍ超とした。またＲａが０．３０μｍ以上になると表面の凹凸が大きくなり、それを起点とした損傷が大きくなるため上限値を０．３０μｍ未満とした。 When the arithmetic average roughness Ra of the surface of the coated sintered alloy according to the present invention is 0.02 μm <Ra <0.30 μm, damage caused by surface irregularities is reduced, and more stable processing is possible. preferable. The surface roughness Ra of the sintered alloy by the mirror treatment is 0.02 μm, and control with higher accuracy is difficult, so the lower limit is set to more than 0.02 μm. Further, when Ra is 0.30 μm or more, the unevenness of the surface becomes large, and damage starting from that becomes large. Therefore, the upper limit value is set to less than 0.30 μm.
本発明の被覆焼結合金は、熱フィラメントプラズマ源によるスパッタ法での基材の表面処理が可能な電極を装備したアークイオンプレーティング装置を用いて作製することができる。すなわち、基材をアークイオンプレーティング装置に装入し、熱フィラメントプラズマ源によるガスイオンボンバード処理と、それとプラズマ密度が異なるアーク放電方式による金属ボンバード処理を組み合わせて、それぞれのボンバード処理における基材への印加電圧、時間を調整することで、基材の結合相の表面形状を制御することができる。熱フィラメントプラズマ源によるボンバード処理として、具体的にはＡｒボンバード処理などを挙げることができる。また、アーク放電方式によるボンバード処理として、具体的には、Ｔｉボンバード処理、ＴｉＡｌボンバード処理、Ｎｂボンバード処理、Ｚｒボンバード処理などの金属ボンバード処理を挙げることができる。 The coated sintered alloy of the present invention can be produced using an arc ion plating apparatus equipped with an electrode capable of surface treatment of a substrate by sputtering using a hot filament plasma source. That is, the base material is inserted into an arc ion plating apparatus, and a gas ion bombard process using a hot filament plasma source and a metal bombard process using an arc discharge method having a different plasma density are combined to form a base material in each bombard process. The surface shape of the binder phase of the substrate can be controlled by adjusting the applied voltage and time. Specific examples of the bombardment process using a hot filament plasma source include an Ar bombard process. Specific examples of the bombardment treatment by the arc discharge method include Ti bombardment treatment, TiAl bombardment treatment, Nb bombardment treatment, Zr bombardment treatment, and the like.
このとき、基材のスパッタ率が、熱フィラメントプラズマ源によるボンバード処理よりもアーク放電方式によるボンバード処理が２倍以上になるように印加電圧を調整する。その際、印加電圧が小さいとエッチング速度が遅くなり作業効率が著しく低下し、印加電圧を大きくしすぎると、制御可能な時間が極端に短くなるため、具体的には、熱フィラメントプラズマ源によるボンバード処理では印加電圧を１５０Ｖ〜３５０Ｖ、アーク放電方式では印加電圧を６００Ｖ〜１０００Ｖにすると好ましく、基材の形状や個数によって処理時間を調整すると、本発明品を製造することができる。 At this time, the applied voltage is adjusted so that the sputtering rate of the base material is twice or more in the bombarding process by the arc discharge method than in the bombarding process by the hot filament plasma source. At that time, if the applied voltage is small, the etching rate is slowed down and the working efficiency is remarkably reduced.If the applied voltage is too large, the controllable time becomes extremely short. In the treatment, the applied voltage is preferably 150 V to 350 V, and in the arc discharge method, the applied voltage is preferably 600 V to 1000 V. The product of the present invention can be produced by adjusting the treatment time depending on the shape and number of base materials.
本発明の被覆焼結合金は、被膜と基材との高い密着性が安定して得られるため、突発的な欠損やチッピングが抑えられ、安定した長寿命加工が可能になる。そのため無人化作業での信頼性が向上し、作業効率の向上が可能となる。 In the coated sintered alloy of the present invention, high adhesion between the coating and the substrate can be obtained stably, so that sudden breakage and chipping are suppressed, and stable long-life processing is possible. Therefore, the reliability in the unmanned work is improved, and the work efficiency can be improved.
基材としてＫ２０相当超硬合金製チップＳＤＫＮ１２０３ＡＥＴＮを用意し、熱フィラメントによるＡｒボンバードが可能な電極および４極のターゲット着装が可能なアークイオンプレーティング装置（以下、ＡＩＰ装置という。）を使用した。基材をＡＩＰ装置内に装入して１×１０-3Ｐａの真空とし、ＡＩＰ装置内のヒーターで５００℃まで加熱した後、表１に示す条件で基材の表面処理をおこなった。その後、表２に示す構成の被膜をコーティングした。被膜は、各被膜の金属成分のターゲットを用い、必要に応じてＮ2またはＣＨ4を雰囲気として導入し、圧力：２．６６Ｐａ、バイアス電圧：５０Ｖという条件で被覆した。 A K20 equivalent cemented carbide chip SDKN1203AETN was prepared as a substrate, and an arc ion plating apparatus (hereinafter referred to as an AIP apparatus) capable of mounting an Ar bombardment with a hot filament and a four-pole target was used. The base material was charged into the AIP apparatus to make a vacuum of 1 × 10 −3 Pa, heated to 500 ° C. with a heater in the AIP apparatus, and then the base material was surface-treated under the conditions shown in Table 1. Then, the film of the structure shown in Table 2 was coated. The coating was performed under the conditions of pressure: 2.66 Pa and bias voltage: 50 V using a target of the metal component of each coating, introducing N 2 or CH 4 as an atmosphere as necessary.
試料番号１〜１９の被覆焼結合金工具について、基材表面に対して任意の垂直断面を鏡面研磨して断面組織をＦＥ−ＳＥＭで観察した。断面組織を組成像で観察すると、結合相と被膜との界面が容易に観察できる。界面に凸状結合相の存在する場合、凸状結合相の平均高さＨと平均間隔Ｌを測定し、表２に併記した。さらに、被覆焼結合金工具の表面の算術平均粗さＲａを測定し、表２に併記した。 For the coated sintered alloy tools of sample numbers 1 to 19, an arbitrary vertical cross section was mirror-polished with respect to the substrate surface, and the cross-sectional structure was observed with FE-SEM. When the cross-sectional structure is observed with a composition image, the interface between the binder phase and the coating can be easily observed. When a convex binder phase was present at the interface, the average height H and average interval L of the convex binder phase were measured and listed in Table 2. Further, the arithmetic average roughness Ra of the surface of the coated sintered alloy tool was measured and listed in Table 2.
試料番号１〜１９の被覆焼結合金工具を用いて、被削材：ＳＣＭ４４０、切削速度：２００ｍ／ｍｉｎ、切り込み：２．０ｍｍ、送り：０．２ｍｍ／ｔｏｏｔｈの条件で乾式フライス試験を行った。工具寿命は、逃げ面摩耗量ＶＢ＝０．３ｍｍに達するまでとした。切削長４ｍまでに逃げ面摩耗量ＶＢ＝０．３ｍｍに達しない場合は、切削長４ｍ時の逃げ面摩耗量ＶＢを測定した。これらの結果を表３に示す。 Using the coated sintered alloy tools of Sample Nos. 1 to 19, dry milling tests were performed under the conditions of work material: SCM440, cutting speed: 200 m / min, cutting depth: 2.0 mm, feed rate: 0.2 mm / tooth. . The tool life was set to reach the flank wear amount VB = 0.3 mm. When the flank wear amount VB did not reach 0.3 mm by the cutting length of 4 m, the flank wear amount VB at the cutting length of 4 m was measured. These results are shown in Table 3.
以上のように、基材の結合相と被膜との界面の結合相形状を制御した発明品は、比較品と比べて安定した長寿命加工が可能であった。 As described above, the inventive product in which the shape of the binder phase at the interface between the binder phase of the substrate and the coating was controlled was capable of stable long-life processing as compared with the comparative product.
基材としてＰ３０相当超硬合金製チップＷＰＭＴ０８０６１５ＺＳＲを用意した。基材をＡＩＰ装置内に装入して１×１０-3Ｐａの真空とし、ＡＩＰ装置内のヒーターで５００℃まで加熱した後、表４に示す条件で基材の表面処理をおこなった。その後、表５に示す構成の被膜をコーティングした。被膜は、各被膜の金属成分のターゲットを用い、雰囲気としてＮ2を導入し、圧力：２．６６Ｐａ、バイアス電圧：８０Ｖという条件で被覆した。 A P30 equivalent cemented carbide chip WPMT080615ZSR was prepared as a substrate. The base material was charged into the AIP apparatus to make a vacuum of 1 × 10 −3 Pa, heated to 500 ° C. with a heater in the AIP apparatus, and then the base material was surface treated under the conditions shown in Table 4. Then, the film of the structure shown in Table 5 was coated. The film was coated under the conditions of pressure: 2.66 Pa and bias voltage: 80 V using a target of the metal component of each film, introducing N 2 as an atmosphere.
試料番号２０〜２５の被覆焼結合金工具について、基材表面に対して任意の垂直断面を鏡面研磨して得られた断面組織をＦＥ−ＳＥＭで観察した。基材の結合相と被膜との界面に凸状結合相が存在する場合、凸状結合相の平均高さＨと平均間隔Ｌを測定し、表５に併記した。さらに、被覆焼結合金工具表面の算術平均粗さＲａを測定し、表５に併記した。 Regarding the coated sintered alloy tools of sample numbers 20 to 25, the cross-sectional structure obtained by mirror polishing an arbitrary vertical cross section with respect to the substrate surface was observed with an FE-SEM. When a convex binder phase was present at the interface between the binder phase of the substrate and the coating, the average height H and average interval L of the convex binder phase were measured and listed in Table 5. Further, the arithmetic average roughness Ra of the surface of the coated sintered alloy tool was measured and shown in Table 5.
試料番号２０〜２５の被覆焼結工具を用いて、被削材：ＳＫＤ１１、切削速度：１５０ｍ／ｍｉｎ、切り込み：１．０ｍｍ、送り：１．０ｍｍ／ｔｏｏｔｈの条件で乾式フライス試験を行った。工具寿命は、逃げ面摩耗量ＶＢ＝０．３ｍｍに達するまでとした。切削長４０ｍまでに逃げ面摩耗量ＶＢ＝０．３ｍｍに達しない場合は、切削長４０ｍ時の逃げ面摩耗量ＶＢを測定した。これらの結果を表６に示す。 Using the coated sintered tools of sample numbers 20 to 25, a dry milling test was performed under the conditions of a work material: SKD11, a cutting speed: 150 m / min, a cutting depth: 1.0 mm, and a feed rate: 1.0 mm / tooth. The tool life was set to reach the flank wear amount VB = 0.3 mm. When the flank wear amount VB did not reach 0.3 mm by the cutting length of 40 m, the flank wear amount VB at the cutting length of 40 m was measured. These results are shown in Table 6.
以上のように、基材の結合相と被膜との界面の結合相形状を制御した発明品は、比較品と比べて安定した長寿命加工が可能であった。 As described above, the inventive product in which the shape of the binder phase at the interface between the binder phase of the substrate and the coating was controlled was capable of stable long-life processing as compared with the comparative product.
１…被膜
２…結合相
３…硬質相
Ｈｎ…凸状結合相の高さ
Ｌｎ…凸状結合相の間隔
DESCRIPTION OF SYMBOLS 1 ...
Claims (3)
3. The coated sintered alloy according to claim 1, wherein the arithmetic average roughness Ra of the surface of the coated sintered alloy is 0.02 μm <Ra <0.30 μm.
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