JPS6299467A - Surface-coated sintered hard alloy - Google Patents

Abstract

PURPOSE:To obtain a surface-coated sintered hard alloy which is remarkably increased in impact resistance, peeling resistance and deposition resistance by coating a conventional base material consisting of a JISP series and M series sintered hard alloys used for steel cutting with a CVD process wherein an organic CN compd. is made to a reaction gas. CONSTITUTION:A base material of the following sintered hard alloy is prepared which consists of 5-16wt% boding phase constituted in a proportion of group 6a/(group ba + group Fc metal) = 0.05-0.25, the balance (W, Ti, Ta, Nb)C solid solution having WC- and B1-type crystal structure as a hard phase formation component and the inevitable impurities. A coating having 0.5-5.0mum thickness of TiCN and TiN regulated to <=0.5mum each grain size is performed by applying a CVD process wherein an organic CN compd. is made to a reaction gas to the base material. Thereby the following surface-coated sintered hard alloy is obtained wherein the above-mentioned characteristics are increased and also the peeling and the dropping of a film due to mechanical shock in milling are reduced.

Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、特に転削工具として用いた場合、優れた切削
性能を示す表面被覆超硬合金に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a surface-coated cemented carbide that exhibits excellent cutting performance, especially when used as a milling tool.

〔従来の技術〕[Conventional technology]

一般に鋼、鋳物などのフライス切削に際して高速切削化
及び高能率切削化に対／、２．；するため、１其材料と
しては超硬合金のＷＣ粒度をより粗粒にし強度を向上さ
せ、　　（Ｗ、　７１’　ｉ　、ゴｔｒ　、　Ｎ　＋１
）　Ｃ相を微細に分散させ耐衝撃性を向１−シ、さらに
これらにＴｉＣＮやＴｉＮ等の硬質物質を被覆した表面
被覆超硬合金が使用されている。表面被覆超硬合金にお
いては、切刃の食いつき時の機械的衝撃によるチッピン
グ、欠損、皮膜の剥離などにより使用条件が制限されて
いる。In general, for high-speed cutting and high-efficiency cutting when milling steel, castings, etc./2. ; In order to do this, as a material, the WC grain size of the cemented carbide is made coarser to improve the strength, and (W, 71' i , Gotr , N +1
) A surface-coated cemented carbide is used in which the C phase is finely dispersed to improve impact resistance, and the C phase is further coated with a hard substance such as TiCN or TiN. Surface-coated cemented carbide has limited usage conditions due to chipping, breakage, and peeling of the coating due to mechanical impact when the cutting edge bites.

〔発明が解決しようとする問題点〕[Problem that the invention seeks to solve]

超硬合金への被覆は従来化学蒸着法、物理蒸着法が行わ
れている。化学蒸着法は主として旋削用として用いられ
、物理蒸着法は主としてエンドミルに用いられている。Conventionally, chemical vapor deposition and physical vapor deposition have been used to coat cemented carbide. The chemical vapor deposition method is mainly used for turning, and the physical vapor deposition method is mainly used for end mills.

両者はその特徴を生かした用途に実用化されているがフ
ライス工具として適用した場合、化学蒸着法は脱炭層に
よる強度不足、物理蒸着法は密着性が悪く、長寿命化に
効果が少ないため、実用化されるに至っていない。Both have been put to practical use in applications that take advantage of their characteristics, but when applied to milling tools, the chemical vapor deposition method lacks strength due to the decarburized layer, and the physical vapor deposition method has poor adhesion and is not effective in extending tool life. It has not yet been put into practical use.

」二連のように、表面被覆超硬合金によるフライス切削
では食いつき、離脱に伴う機械的衝撃のため十分満足す
る切削性能を有するまでには至っていない。表面被覆超
硬合金において、その切削領域。In milling using a surface-coated cemented carbide, as in the case of two series, it has not been possible to achieve sufficiently satisfactory cutting performance due to the mechanical impact caused by biting and separation. In surface-coated cemented carbide, its cutting area.

用途の拡大には、皮膜の安定性（特に耐剥離性）を向上
させる必要がある。To expand the range of applications, it is necessary to improve the stability (especially peeling resistance) of the film.

〔問題点を解決するための手段〕[Means for solving problems]

以上の点より本発明は、従来の表面被覆超硬合金より安
定した性能を発揮させるため、被覆相に着目し、特に皮
膜の耐剥離性、密着性、脱炭相の低減、微粒化を計った
ものである。Based on the above points, the present invention focuses on the coating phase and particularly aims to improve the peeling resistance, adhesion, reduction of decarburized phase, and atomization of the coating in order to exhibit more stable performance than conventional surface-coated cemented carbide. It is something that

従って、本発明等は機械的衝撃に優れ、かつ化学蒸着法
と同程度の密着性を有する被覆法を検討した結果、７０
０〜９００℃で蒸着する化学蒸着法により達成する事が
できるとの知見を得た。Therefore, as a result of studying a coating method that is excellent in mechanical impact and has adhesion comparable to that of chemical vapor deposition, the present invention has developed a coating method with 70%
It has been found that this can be achieved by a chemical vapor deposition method that performs vapor deposition at a temperature of 0 to 900°C.

本発明は上記知見に基づき、Ｆｅ族金属の１種又は２種
以上及び６ａ族を含有し、その比が６ａ族／（６ａ族＋
Ｆｅ族金属）＝５／１００−２５／１００で構成された
結合相；５〜１６ｗｔ％。Based on the above findings, the present invention contains one or more Fe group metals and 6a group, and the ratio is 6a group/(6a group +
Binding phase composed of Fe group metal) = 5/100-25/100; 5-16 wt%.

硬質相形成成分として炭化タングステン及びＢ１型の結
晶構造を有する（　Ｗ　、　Ｔ　ｊ、　、　Ｔ　ａ　、
　Ｎ　ｂ　）Ｃ固溶体及び不可避不純物；残りからなる
組成を有し、Ｔ　ｊ、　ＣＮ及び又はＴｉＮを０．５〜
５．０μｍ被覆した表面被覆超硬合金において、その被
覆層（ＴｉＣＮ及び又はＴｉＮ）の粒子径が０．５μｍ
以下である事を特徴とする表面被覆超硬合金である。It has tungsten carbide as a hard phase forming component and a B1 type crystal structure (W, Tj, , Ta,
Nb) C solid solution and unavoidable impurities; has a composition consisting of the remainder, Tj, CN and or TiN from 0.5 to
In surface-coated cemented carbide coated with a thickness of 5.0 μm, the particle size of the coating layer (TiCN and/or TiN) is 0.5 μm.
This is a surface coated cemented carbide characterized by the following:

以下に数値限定した理由を説明する。The reason for the numerical limitations will be explained below.

■結合相の含有量 その含有量が５％未満では、所望の優れた強度を合金に
付与する事ができず、一方１６％を超えると相対的にＷ
Ｃなどの硬質相の含有量が低下し、ＷＣなどの持つ優れ
た耐摩耗性、耐塑性変形性がなくなるため、その含有量
が５〜１６％と限定した。■ Content of binder phase If the content is less than 5%, the desired excellent strength cannot be imparted to the alloy, while if it exceeds 16%, the relative W
Since the content of hard phases such as C decreases and the excellent wear resistance and plastic deformation resistance of WC and the like are lost, the content is limited to 5 to 16%.

■結合相中の６８族の含有に ６ａ族／（６ａ族十Ｆｅ族）＝５／１００−２５／１０
０の構成としたのは５　／　’１．　ＯＯ未ｈ×１では
所望の優れた耐熱性、耐酸化性、耐塑性変形性。■Inclusion of group 68 in the binder phase: 6a group/(6a group, 10 Fe groups) = 5/100-25/10
The configuration of 0 was 5/'1. OO-H×1 has the desired excellent heat resistance, oxidation resistance, and plastic deformation resistance.

耐溶着性を合金に付与する事ができず、２５／１００を
超えると硬質相がＭ、Ｃタイプの複炭化物を生成し、靭
性を低下させるためである。This is because it is not possible to impart adhesion resistance to the alloy, and when the ratio exceeds 25/100, the hard phase forms M and C type double carbides, reducing toughness.

■硬質相の被覆及び膜厚 本発明の表面被覆超硬合金への被覆は、有機ＣＮ化合物
を反応ガスとするＣＶＤ　（Ｃｈｅｍｉｃａｌ　　ｖａ
ｐｏｒ　　ｄｅｐｏｓｉｔｉ、ｏｎ）法が適用される。■Hard phase coating and film thickness The coating on the surface-coated cemented carbide of the present invention is carried out by chemical vapor deposition (CVD) using an organic CN compound as a reaction gas.
por deposit, on) method is applied.

本方法は蒸着温度が７００〜９００℃と従来のＣＶＤ法
に比較して低く、■拡散速度が遅いため脱炭層の生成が
少なく、■膜質が微細であり、■従来のＣＶＤ法との併
用が可能なことなどのメリットを有する。This method has a deposition temperature of 700 to 900°C, which is lower than that of conventional CVD methods, ■ has a slow diffusion rate, resulting in less decarburized layer formation, ■ has a fine film quality, and ■ cannot be used in combination with conventional CVD methods. It has the advantage of being possible.

膜厚を０．５〜５．０μｍとしたのは、０．５μｍ未満
では十分な耐摩耗性を付与することが出来ず、５．０μ
ｍを超えて厚くすると密着性が劣化するためである。The reason why the film thickness is set to 0.5 to 5.0 μm is because if it is less than 0.5 μm, sufficient wear resistance cannot be imparted.
This is because if the thickness exceeds m, the adhesion will deteriorate.

さらに被覆層の粒子径を０．５μｍ以下としたのは、耐
衝撃性、耐摩耗性を向上させ、かつフライス切削におけ
る機械的衝撃による皮膜の剥離。Furthermore, the particle size of the coating layer is set to 0.5 μm or less to improve impact resistance and abrasion resistance, and to prevent the coating from peeling off due to mechanical impact during milling.

脱落などを少なくするためである。This is to reduce the possibility of falling off.

以下、実施例について説明する。Examples will be described below.

〔実施例〕〔Example〕

実施例Ｉ ＪＩＳ　　Ｐ３０相当の合金を製造するため（Ｗ。 Example I To manufacture alloys equivalent to JIS P30 (W.

Ｔｉ）Ｃ（平均粒度１．Ｏ〜ｌ−，５μｍ）（Ｔａ。Ti) C (average particle size 1.0-1-, 5 μm) (Ta.

Ｎｂ）Ｃ粉末（同１．２／ｊｍ）、ＷＣ粉末（平均粒度
４μｍ）及びＣｏ粉末（同１．７ｚｍ）、Ｎｉ粉末（同
１μｍ）を用意し、これらを第１−表に示す組成に配合
し、ボールミル中で湿式粉砕、混合を９６時間行ない、
乾燥処理後ＩＴｏｎ／ｆｆｌの圧力でプレス成形した。Nb)C powder (average particle size 1.2/jm), WC powder (average particle size 4μm), Co powder (average particle size 1.7zm), and Ni powder (average particle size 1μm) were prepared, and these were made into the composition shown in Table 1. Blend, wet grind and mix in a ball mill for 96 hours,
After drying, it was press-molded at a pressure of Iton/ffl.

次に真空中１４００℃で焼結し、本発明の超硬合金を製
造した。次にこれらの硬さ及び抗折力を測定した結果も
第１表に合せて記入した。Next, it was sintered at 1400° C. in vacuum to produce the cemented carbide of the present invention. Next, the results of measuring their hardness and transverse rupture strength are also entered in Table 1.

次に上記合金へ有機ＣＮ化合物を反応ガスとするＣＶＤ
法によりＴｉＣＮ２μｍを被覆した。次に被覆後の抗折
力を測定するため、３面を研削し被覆層を抗折力試験片
の引張応力側にセットし、測定した。その結果も表１に
併記する。Next, the above alloy is subjected to CVD using an organic CN compound as a reaction gas.
2 μm of TiCN was coated by the method. Next, in order to measure the transverse rupture strength after coating, three sides were ground, the coating layer was set on the tensile stress side of the transverse rupture strength test piece, and the measurement was performed. The results are also listed in Table 1.

表１より従来のＣＶＤ法に比較し、膜厚が同一の場合、
被覆後の抗折力は向−１ニし、強度低下の少第１表 ■、ＣＶＤ法（ハロゲンガス使用）による被ｇ　（Ｔｊ
ＣＮ２μｍ）ないことが分かる。From Table 1, compared to the conventional CVD method, when the film thickness is the same,
The transverse rupture strength after coating is -12, and there is little decrease in strength.
It can be seen that there is no CN2μm).

さらに写真１に示すように本被覆法によれば極めて微細
な皮膜が得られ、かつ断面を研磨し、ラップした後、村
」二試薬でエツチングし、観察した結果、写真３に示す
ように脱炭層（ＭｇＣ）は観察されなかった。なお、脱
炭層は皮膜と超硬合金の界面に生成し、写真の場合、黒
色として観察される。写真２．写真４には従来のＣＶＤ
法の場合を示す。Furthermore, as shown in Photo 1, an extremely fine film was obtained using this coating method, and after polishing and lapping the cross section, etching with Murakami's reagent and observation revealed that the film was removed as shown in Photo 3. No carbon layer (MgC) was observed. Note that the decarburized layer forms at the interface between the film and the cemented carbide, and is observed as black in the photograph. Photo 2. Photo 4 shows conventional CVD
Indicates the case of law.

実施例２ 実施例１の合金を用いて、下記の条件で切削試験を行な
い、その性能を評価した。Example 2 Using the alloy of Example 1, a cutting test was conducted under the following conditions to evaluate its performance.

■寿命試験 被剛材　　　Ｓ　ＣＭ４４０ チップ　　　５ＰＧＮ４２２ 切削速度　　２００ｍ／ｍｉｎ 送り　　　　０　、２　ｍｍ　／刃 切削時間　　１０ｍ１ｎ の条件で正面フライスによる切削試験を行ない、逃げ面
摩耗を測定した。■ Life test material S CM440 Chip 5PGN422 A cutting test was conducted using a face mill under the conditions of cutting speed: 200 m/min, feed: 0, 2 mm/blade cutting time: 10 m1n, and flank wear was measured.

第２表 第３表 これらの測定結果を第３表に示す。Table 2 Table 3 The results of these measurements are shown in Table 3.

第３表に示される結果より、本発明合金はｗｃ基超超硬
合金靭性を保ちなかｔ″Ｉにり高速切削、高送り切削に
優れた性能を示す１１Ｆが明らかである。From the results shown in Table 3, it is clear that the alloy of the present invention maintains the toughness of the WC-based cemented carbide and exhibits excellent performance in high-speed cutting and high-feed cutting due to t''I.

実施例３ 実施例１と同様の工Ｐ、）で試料番ｒ３．　Ｂの合金を
用いて、これに実施例１で用いたＣＶＤ法によりＴｊＣ
Ｎ又は及びＴ　ｉ　Ｎを中層、複層に被覆した。Example 3 Sample number r3. Using the alloy B, TjC was applied to it by the CVD method used in Example 1.
The middle layer and multiple layers were coated with N or TiN.

その膜厚、膜質及び抗折力を測定した結果も第３表に合
せて記入した。さらに耐熱性、耐ＷＲ撃性を評価するた
め切削試験用チップを製造し、被削材　　　Ｓ　Ｋ　Ｄ
　６１ チップ　　　５ＰＣＮ／ｌ　２ＴＲ−Ａ３切削速度　　
１００　ｍ　／　ｍｊ、ｎ送り　　　　Ｏｉ、５ｍｍ／
刃 の条件で正面フライスによる切削試験を行ない、１０分
切削後の逃げ面摩耗を測定した。その結果も合せて記入
する。第３表から明らかなように被覆層の微細化、脱炭
層の低減などの相乗効果により耐熱性、耐摩耗性、耐溶
着性に優れ高速切削に対応した優れた性能を示した。さ
らに実施例３により、本発明が広い汎用性を持っている
ことも明らかである。The results of measuring the film thickness, film quality, and transverse rupture strength are also entered in Table 3. Furthermore, in order to evaluate heat resistance and WR impact resistance, cutting test chips were manufactured and the workpiece material S K D
61 Tip 5PCN/l 2TR-A3 cutting speed
100 m/mj, n feed Oi, 5mm/
A cutting test was conducted using a face milling cutter under the conditions of the blade, and flank wear was measured after 10 minutes of cutting. Also enter the results. As is clear from Table 3, due to the synergistic effects of the finer coating layer and the reduction of the decarburized layer, it exhibited excellent heat resistance, wear resistance, and welding resistance, and exhibited excellent performance suitable for high-speed cutting. Furthermore, it is clear from Example 3 that the present invention has wide versatility.

上記実施例では、被覆層としてＴｊＣ，ＴｊＣＮ等の炭
化物、炭窒化物を使用しているが、さらに金属ハロゲン
ガス、Ｈ２ガス、炭化水素ガス又は酸化物のガスを反応
ガスとするＣＶＤ法との絹合せによりＴｉＣ，ＡＱ２０
３などとの多層被覆した場合でも優れた効果が得られる
。In the above embodiments, carbides and carbonitrides such as TjC and TjCN are used as the coating layer, but it is also possible to use a CVD method using metal halogen gas, H2 gas, hydrocarbon gas, or oxide gas as the reaction gas. TiC, AQ20 by silk combination
Excellent effects can be obtained even in the case of multilayer coating such as 3.

〔発明の効果〕〔Effect of the invention〕

本願表面被覆超硬合金は、従来の鋼切削用のＪＩＳＰ系
９Ｍ系（Ｗ　Ｃ−Ｔ　ｊ、　Ｃ−Ｔ　ａ　Ｃ−Ｃ。The surface-coated cemented carbide of the present application is a JISP 9M series (W C-Tj, C-T a C-C) for conventional steel cutting.

／　Ｎ　ｉ系）の超硬合金を基体とし、有機ＣＮ化合物
を反応ガスとするＣＶＤ法で被覆することにより、従来
不十分であった耐ｗｊｔ撃性、耐剥離性、耐溶着性が大
１】に向」ニし、そのため機械的衝撃を伴うフライス切
削工具用材料として好適なものである。/Ni-based) cemented carbide as a base and coated with a CVD method using an organic CN compound as a reaction gas, the conventionally insufficient wjt impact resistance, peeling resistance, and welding resistance are greatly improved. ] Therefore, it is suitable as a material for milling cutting tools that are subject to mechanical impact.

−１，１−-1,1-

【図面の簡単な説明】[Brief explanation of drawings]

写真１は、本発明の皮膜最外層のＳＥＭ観察結果（倍率
Ｘ　３０００）を示す。写真２は、ハロゲンガス使用の
ＣＶＤ法の皮膜最外層のＳＥＭ観察結果を示す。写真３
は、写真１の断面観察（倍率×１５００）を示す。写真
４は、写真２の断面観察の結果を示す。 特許出願人　　日立超硬株式会社 屈面の０書・：内容に変更なし） 手続補正帯（方式） 昭和６１年４月４日Photo 1 shows the results of SEM observation (magnification: X 3000) of the outermost layer of the film of the present invention. Photo 2 shows the results of SEM observation of the outermost layer of the film obtained by CVD using halogen gas. Photo 3
shows the cross-sectional observation of Photo 1 (magnification x 1500). Photo 4 shows the results of cross-sectional observation of Photo 2. Patent Applicant Hitachi Choukou Co., Ltd. Kumen No. 0: No change in content) Procedural Amendment Band (Method) April 4, 1986

Claims (1)

【特許請求の範囲】[Claims] １）Ｆｅ族金属の１種又は２種以上及び６ａ族を含有し
、その比が６ａ族／（６ａ族＋Ｆｅ族金属）＝５／１０
０−２５／１００で構成された結合相；５〜１６ｗｔ％
、硬質相形成成分として炭化タングステン及びＢ１型の
結晶構造を有する（Ｗ、Ｔｉ、Ｔａ、Ｎｂ）Ｃ固溶体及
び不可避不純物；残りからなる組成を有し、ＴｉＣＮ及
び又はＴｉＮを０．５〜５．０μｍ被覆した表面被覆超
硬合金において、その被覆層（ＴｉＣＮ及び／又はＴｉ
Ｎ）の粒子径が０．５μｍ以下である事を特徴とする表
面被覆超硬合金。1) Contains one or more Fe group metals and 6a group, the ratio of which is 6a group/(6a group + Fe group metal) = 5/10
Bonded phase composed of 0-25/100; 5-16wt%
, tungsten carbide as a hard phase forming component, a (W, Ti, Ta, Nb)C solid solution having a B1 type crystal structure, and unavoidable impurities; In the surface-coated cemented carbide coated with a thickness of 0 μm, the coating layer (TiCN and/or Ti
A surface-coated cemented carbide characterized in that the particle size of N) is 0.5 μm or less.