JP5850405B2 - Surface coated cutting tool with excellent chipping resistance, peel resistance and wear resistance - Google Patents
Surface coated cutting tool with excellent chipping resistance, peel resistance and wear resistance Download PDFInfo
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この発明は、高熱発生を伴うとともに、切刃に対して断続的・衝撃的負荷が作用するステンレス、炭素鋼等の高速断続切削加工において、硬質被覆層がすぐれた耐チッピング性、耐剥離性および耐摩耗性を発揮する表面被覆切削工具（以下、被覆工具という）に関するものである。 This invention is accompanied by high heat generation, and in high-speed intermittent cutting of stainless steel, carbon steel, etc. where intermittent / impact loads are applied to the cutting edge, chipping resistance, exfoliation resistance and The present invention relates to a surface-coated cutting tool that exhibits wear resistance (hereinafter referred to as a coated tool).
工具基体表面に、周期律表の４ａ、５ａ、６ａ族から選ばれた少なくとも１種以上の元素の炭化物、窒化物、炭窒化物等からなる硬質皮膜を下地層として成膜し、その上に、さらに上部層としての酸化アルミニウム層を化学蒸着で形成した被覆工具は、例えば、特許文献１に示すようによく知られているが、このような酸化アルミニウム層においては、熱膨張係数差等に起因し、層中に冷却クラックが生じることが知られている。
そして、冷却クラックの発生による問題を解決すべく、従来から、種々の提案がなされている。
例えば、特許文献２では、炭化タングステン（ＷＣ）基超硬合金または炭窒化チタン（ＴｉＣＮ）基サーメットからなる工具基体の表面に、下部層と上部層からなる硬質被覆層を被覆した被覆工具において、上部層として、化学蒸着形成した状態でκ型またはθ型の結晶構造を有する酸化アルミニウムに加熱処理を施して結晶構造をα型結晶構造に変態してなると共に、加熱変態生成クラックが分布した組織および１〜１５μｍの平均層厚を有する加熱変態α型酸化アルミニウム層を層基体とし、前記層基体中に存在する樹枝状不連続クラックの分布形態を、前記層基体表面に対するショットブラスト処理で網目状連続クラックとした状態で、これに前記層基体との合量に占める割合で０．５〜５質量％の窒化チタンを化学蒸着充填してなるクラック充填加熱変態α型酸化アルミニウム層を被覆形成してなる被覆工具が提案されており、この被覆工具が、例えば各種の鋼や鋳鉄などの高速断続切削ですぐれた耐チッピング性を示すことも知られている。
A hard film made of carbide, nitride, carbonitride, or the like of at least one element selected from groups 4a, 5a, and 6a of the periodic table is formed on the surface of the tool base as an underlayer, and Furthermore, a coated tool in which an aluminum oxide layer as an upper layer is formed by chemical vapor deposition is well known, for example, as shown in Patent Document 1. However, in such an aluminum oxide layer, a difference in thermal expansion coefficient is caused. This is known to cause cooling cracks in the layer.
Various proposals have been made to solve the problems caused by the occurrence of cooling cracks.
For example, in Patent Document 2, in a coated tool in which a hard coating layer composed of a lower layer and an upper layer is coated on the surface of a tool base composed of tungsten carbide (WC) -based cemented carbide or titanium carbonitride (TiCN) -based cermet, As an upper layer, a structure in which heat treatment is applied to aluminum oxide having a κ-type or θ-type crystal structure in a state where chemical vapor deposition is formed to transform the crystal structure into an α-type crystal structure, and heat transformation generation cracks are distributed. And a heat-transformed α-type aluminum oxide layer having an average layer thickness of 1 to 15 μm as a layer substrate, and the distribution form of dendritic discontinuous cracks existing in the layer substrate is formed into a network by shot blasting on the surface of the layer substrate. In a state where continuous cracks are formed, a chemical vapor deposition filling of 0.5 to 5% by mass of titanium nitride in a proportion of the total amount with the layer base is performed. A coated tool formed by coating a heat-filled heat-transformed α-type aluminum oxide layer has been proposed, and this coated tool may exhibit excellent chipping resistance in high-speed intermittent cutting such as various steels and cast iron. Are known.
上記従来の被覆工具においては、これを通常条件の高速切削、断続切削に用いた場合には特段の支障はないが、特にこれを、高熱発生を伴い、切れ刃に断続的・衝撃的負荷が作用するステンレス、炭素鋼等の高速断続切削に用いた場合には、上記被覆工具では、溶着が生じたり、また、断続切削の衝撃によって切刃部にチッピングや剥離が発生するため、長期の使用にわたって十分に満足できる切削性能を発揮し得ないという問題があった。 In the above-mentioned conventional coated tool, there is no particular problem when it is used for high-speed cutting and intermittent cutting under normal conditions. However, this is accompanied by high heat generation, and intermittent and impact loads are applied to the cutting edge. When used for high-speed interrupted cutting of working stainless steel, carbon steel, etc., the above-mentioned coated tool will cause welding, and chipping and peeling will occur at the cutting edge due to the impact of interrupted cutting. There is a problem that the cutting performance that can be satisfactorily satisfied cannot be exhibited.
そこで、本発明者等は、耐チッピング性、耐剥離性にすぐれ、高速断続切削という厳しい条件下でも、長期の使用にわたってすぐれた耐摩耗性を発揮する被覆工具を提供すべく、鋭意研究を行ったところ、次のような知見を見出したのである。 Therefore, the present inventors have conducted intensive research to provide a coated tool that has excellent chipping resistance and peeling resistance, and exhibits excellent wear resistance over a long period of use even under severe conditions such as high-speed intermittent cutting. As a result, the following findings were found.
即ち、炭化タングステン基超硬合金、炭窒化チタン基サーメットからなる工具基体表面上に、下地層として周期律表の４ａ、５ａ、６ａ族、ＡｌおよびＳｉから選ばれる少なくとも一種以上の元素の炭化物、窒化物、炭窒化物、炭酸化物および炭窒酸化物を含有する硬質被覆層を化学蒸着または物理蒸着によって被覆形成した後に、硬質被覆層としての酸化アルミニウム層を被覆形成するにあたり、化学蒸着（ＣＶＤ）法により酸化アルミニウム層を下層として形成し、下層表面に所定の凹部を形成した上で、該下層の表面に凹部を埋め込むようにゾル−ゲル法により非晶質酸化シリコン層を被覆形成した場合には、上層は、平滑かつ潤滑性にすぐれ、しかも、下層との密着性が大であることにより、耐チッピング性、耐剥離性、耐摩耗性に優れた硬質被覆層を成膜し得ることを見出したのである。 That is, a carbide of at least one element selected from the group 4a, 5a, 6a, Al and Si of the periodic table as an underlayer on the surface of a tool substrate made of tungsten carbide-based cemented carbide, titanium carbonitride-based cermet, After the hard coating layer containing nitride, carbonitride, carbonate and carbonitride oxide is coated by chemical vapor deposition or physical vapor deposition, the chemical vapor deposition (CVD) is performed to coat the aluminum oxide layer as the hard coating layer. ) When an aluminum oxide layer is formed as a lower layer by the method, a predetermined recess is formed on the lower surface, and an amorphous silicon oxide layer is formed by a sol-gel method so that the recess is embedded in the lower surface. In addition, the upper layer is smooth and has excellent lubricity, and also has high adhesion to the lower layer, thereby improving chipping resistance, peeling resistance, and abrasion resistance. It was found that the hard coating layer may be deposited.
つまり、従来の化学蒸着（ＣＶＤ）法で成膜した結晶質酸化アルミニウム層では、その表面の潤滑性や平滑性が足りないために溶着などにより、チッピング、剥離等の異常損傷やクレーター摩耗が短時間で発生するものの、これを下層とし、その上層としてゾル−ゲル法で成膜した非晶質酸化シリコン層を成膜した場合には、潤滑性、平滑性、切屑排出性が向上し、高い耐摩耗性を発揮し得ること、さらに、上層と下層の界面が凹形状となっているため、衝撃的負荷が作用する高速断続切削においても、アンカー効果により上層が剥離しにくくなること、加えて、硬質被覆層の摩耗が進行した際にも、凹部に上層の非晶質酸化シリコン層が充填されるように成膜されているために、上層の潤滑性と下層の耐摩耗性を、長期間にわたって同時に発揮することができるということを見出したのである。 In other words, the crystalline aluminum oxide layer formed by the conventional chemical vapor deposition (CVD) method has insufficient lubricity and smoothness on the surface, so that abnormal damage such as chipping and peeling and crater wear are short due to welding. Although it occurs over time, when this is used as the lower layer and an amorphous silicon oxide layer formed by the sol-gel method as the upper layer is formed, the lubricity, smoothness, and chip discharge properties are improved and high. In addition to being able to demonstrate wear resistance, and because the interface between the upper layer and the lower layer has a concave shape, the upper layer is difficult to peel off due to the anchor effect even in high-speed interrupted cutting where an impact load acts. Since the upper amorphous silicon oxide layer is filled in the recess even when wear of the hard coating layer proceeds, the lubricity of the upper layer and the wear resistance of the lower layer are increased. Simultaneously over a period It was found that it is possible to volatilization.
この発明は、上記知見に基づいてなされたものであって、
「（１） 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工具基体の表面に形成された下地層、及び該下地層上に、酸化アルミニウムからなる下層と酸化シリコンからなる上層とから構成される硬質被覆層が形成された表面被覆切削工具において、
（ａ）該下地層は、１．０〜１５．０μｍの平均層厚を有する周期律表の４ａ、５ａ、６ａ族、ＡｌおよびＳｉから選ばれる少なくとも一種以上の元素の炭化物、窒化物、炭窒化物、炭酸化物および炭窒酸化物層であって、
（ｂ）下層は、０．８〜１０．０μｍの平均層厚を有する結晶質酸化アルミニウム層、
（ｃ）上層は、０．２〜４．０μｍの平均層厚を有する非晶質酸化シリコン層であって、
（ｄ）下層の結晶質酸化アルミニウム層の表面には、凹部が形成されており、上層の非晶質酸化シリコン層は、下層の上記凹部を埋め込むように充填成膜されており、
（ｅ）下層に形成された凹部の平均深さは、０．５〜１０．０μｍの範囲（但し、下層の平均層厚以下）であり、
（ｆ）下層に形成された凹部の平均アスペクト比は、１．０〜４０の範囲であり、
（ｇ）下層に形成された凹部相互の平均水平間隔は、０．５〜１５μｍの範囲であることを特徴とする表面被覆切削工具。
（２） 下層の酸化アルミニウムはκ型の結晶構造を有することを特徴とする前記（１）に記載の表面被覆切削工具。」
を特徴とするものである。
This invention has been made based on the above findings,
"(1) tungsten carbide based cemented carbide or underlayer made form the surface of the tool substrate made of titanium carbonitride based cermet, and on the underlayer, and a top layer consisting of a lower layer and a silicon oxide consisting of aluminum oxide In the surface-coated cutting tool in which the hard coating layer is formed ,
(A) The underlayer is composed of carbide, nitride, charcoal of at least one element selected from Group 4a, 5a, 6a, Al and Si in the periodic table having an average layer thickness of 1.0 to 15.0 μm. A nitride, carbonate and carbonitride layer,
(B) The lower layer is 0 . A crystalline aluminum oxide layer having an average layer thickness of 8 to 10.0 μm;
(C) The upper layer is an amorphous silicon oxide layer having an average layer thickness of 0.2 to 4.0 μm,
(D) A concave portion is formed on the surface of the lower crystalline aluminum oxide layer, and the upper amorphous silicon oxide layer is filled to fill the lower concave portion,
(E) The average depth of the recesses formed in the lower layer is in the range of 0.5 to 10.0 μm (however, below the average layer thickness of the lower layer),
(F) The average aspect ratio of the recesses formed in the lower layer is in the range of 1.0 to 40,
(G) The surface-coated cutting tool, wherein the average horizontal interval between the recesses formed in the lower layer is in the range of 0.5 to 15 μm.
(2) The surface-coated cutting tool according to (1), wherein the lower layer aluminum oxide has a κ-type crystal structure. "
It is characterized by.
以下、本発明について、詳細に説明する。 Hereinafter, the present invention will be described in detail.
本発明の被覆工具は、炭化タングステン基超硬合金、炭窒化チタン基サーメットからなる工具基体の表面に下地層として周期律表の４ａ、５ａ、６ａ族、ＡｌおよびＳｉから選ばれる少なくとも一種以上の元素の炭化物、窒化物、炭窒化物、炭酸化物および炭窒酸化物を含有する硬質被覆層を化学蒸着または物理蒸着によって被覆形成し、上述した結晶質酸化アルミニウム層からなる下層と非晶質酸化シリコン層からなる上層とを該下地層上に被覆形成する。
また、上記下層の結晶質酸化アルミニウム層は下地層との密着力が優れるκ型酸化アルミニウムであることが望ましい。
結晶質酸化アルミニウムは超硬基体上、またはサーメット基体上に直接成膜した場合、密着性が低く、基体が酸化することによる性能劣化が起こるために、下地層は必要であり、該下地層の具体例としては、例えば、化学蒸着によって形成したＴｉＮ層、ＴｉＣＮ層、ＴｉＣＯ層、ＴｉＣＮＯ層等のＴｉ化合物層、物理蒸着によって形成したＴｉとＡｌの複合窒化物層、ＣｒとＡｌの複合窒化物層等を挙げることができる。
The coated tool of the present invention comprises at least one or more selected from the group 4a, 5a, 6a of the periodic table, Al and Si as an underlayer on the surface of a tool base made of tungsten carbide base cemented carbide or titanium carbonitride base cermet. A hard coating layer containing elemental carbides, nitrides, carbonitrides, carbonates and carbonitrides is formed by chemical vapor deposition or physical vapor deposition. An upper layer made of a silicon layer is formed on the base layer.
The lower crystalline aluminum oxide layer is preferably κ-type aluminum oxide having excellent adhesion to the underlayer.
When crystalline aluminum oxide is formed directly on a cemented carbide substrate or a cermet substrate, the adhesion is low, and performance deterioration due to oxidation of the substrate occurs. Specific examples include, for example, Ti compound layers such as TiN layers, TiCN layers, TiCO layers, and TiCNO layers formed by chemical vapor deposition, Ti and Al composite nitride layers formed by physical vapor deposition, and Cr and Al composite nitrides. A layer etc. can be mentioned.
図１に、本発明の被覆工具の硬質被覆層縦断面の構成図を、また、図２に、本発明被覆工具の硬質被覆層の縦断面模式図を示す。
図１に示される本発明の被覆工具は、炭化タングステン基超硬合金からなる工具基体上に下地層を形成した後、化学蒸着で形成された０．８〜１０．０μｍの平均層厚を有する結晶質酸化アルミニウム層からなる下層が被覆形成され、この上に、０．２〜４．０μｍの平均層厚を有する非晶質酸化シリコン層からなる上層が被覆形成されている。
また、図２に示すように、下層の結晶質酸化アルミニウム層の表面には、凹部が形成されており、上層の非晶質酸化シリコン層は、下層の凹部を埋め込むように充填成膜されている。
FIG. 1 is a configuration diagram of a longitudinal section of a hard coating layer of the coated tool of the present invention, and FIG. 2 is a schematic longitudinal sectional view of a hard coating layer of the coated tool of the present invention.
The coated tool of the present invention shown in FIG. 1 has an average layer thickness of 0.8 to 10.0 μm formed by chemical vapor deposition after forming an underlayer on a tool substrate made of a tungsten carbide base cemented carbide. A lower layer made of a crystalline aluminum oxide layer is coated, and an upper layer made of an amorphous silicon oxide layer having an average layer thickness of 0.2 to 4.0 μm is coated thereon.
Further, as shown in FIG. 2, a recess is formed on the surface of the lower crystalline aluminum oxide layer, and the upper amorphous silicon oxide layer is filled and formed so as to fill the lower recess. Yes.
ここで、下層の平均層厚を０．８〜１０．０μｍと定め、また、上層の平均層厚を０．２〜４．０μｍと定めているが、その理由は、それぞれの層厚が下限値（０．８μｍ，０．２μｍ）を下回った場合には、長期の使用に亘って十分な耐摩耗性を発揮することができず、一方、上限値（１０．０μｍ，４．０μｍ）を超える場合には、チッピングを発生しやすくなるということによる。 Here, the average layer thickness of the lower layer is defined as 0.8 to 10.0 μm, and the average layer thickness of the upper layer is defined as 0.2 to 4.0 μm, because the respective layer thickness is the lower limit. When the value is less than 0.8 μm or 0.2 μm, sufficient wear resistance cannot be exhibited over a long period of use, while the upper limit (10.0 μm, 4.0 μm) is not reached. If it exceeds, chipping is likely to occur.
また、下層の表面に形成されている凹部について述べる。
まず、下層の凹部の平均深さ（図１参照）は、０．５〜１０．０μｍ、上層の潤滑性と下層の耐摩耗性を同時に発揮できる最適範囲と非晶質酸化シリコンの焼成時の熱膨張を考慮すると、凹部深さはより好ましくは２．０〜７．０μｍの範囲内にあり、下層の凹部の平均深さが０．５μｍ未満である場合には、下層表面がほぼ平坦となり、下層−上層間でのアンカー効果が小さくなるため、上層が剥離しやすくなることから、凹部の平均深さは０．５μｍ以上必要である。一方、下層の最大平均層厚が１０．０μｍなのであるから、下層の凹部の最大平均深さは、自ずと１０．０μｍとなる。
Moreover, the recessed part currently formed in the surface of a lower layer is described.
First, the average depth of the recesses in the lower layer (see FIG. 1) is 0.5 to 10.0 μm, the optimum range in which the upper layer lubricity and the lower layer wear resistance can be exhibited at the same time, and when the amorphous silicon oxide is fired. In consideration of thermal expansion, the depth of the recess is more preferably in the range of 2.0 to 7.0 μm. When the average depth of the recess in the lower layer is less than 0.5 μm, the surface of the lower layer becomes almost flat. Since the anchor effect between the lower layer and the upper layer becomes small and the upper layer is easily peeled off, the average depth of the recesses is required to be 0.5 μm or more. On the other hand, since the maximum average layer thickness of the lower layer is 10.0 μm, the maximum average depth of the recesses of the lower layer is naturally 10.0 μm.
次に、本発明では凹部の平均アスペクト比を凹部最大深さに対する基体水平方向における凹部の最大幅の比として定義し、該平均アスペクト比が１．０〜４０、より好ましくは５．０〜２５の範囲内にある方が焼成時の上層と下層の熱膨張係数差による凹部における応力の影響が小さくなるため、密着性が高まり、下層の凹部は長方形に近い方がアンカー効果が高く、アスペクト比が４０を超えると、硬質皮膜の上部では非晶質酸化シリコンの割合が多くなり、下部では結晶質酸化アルミニウムの割合が少なくなるため、非晶質酸化シリコンの潤滑性と結晶質酸化アルミニウムの耐摩耗性を長期にわたって両立させることができない。一方、アスペクト比が１．０未満であると、上層と下層の異なる機械的・熱的特性に起因して凹部の付け根から異常損傷を起こしやすくなり、アンカー効果が小さくなるために上層が剥離しやすくなり、結果的に潤滑性が不足するために大きな発熱が生じる。 Next, in the present invention, the average aspect ratio of the recesses is defined as the ratio of the maximum width of the recesses in the horizontal direction of the substrate to the maximum depth of the recesses, and the average aspect ratio is 1.0 to 40, more preferably 5.0 to 25. When the ratio is within the range, the influence of stress in the recess due to the difference in thermal expansion coefficient between the upper and lower layers during firing is reduced, so the adhesion is improved, and the anchor effect is higher when the recess in the lower layer is closer to a rectangle. Exceeds 40, the proportion of amorphous silicon oxide increases in the upper part of the hard film and the proportion of crystalline aluminum oxide decreases in the lower part. Therefore, the lubricity of amorphous silicon oxide and the resistance of crystalline aluminum oxide are reduced. Abrasion cannot be achieved over a long period of time. On the other hand, if the aspect ratio is less than 1.0, abnormal damage tends to occur from the root of the recess due to the different mechanical and thermal characteristics of the upper layer and the lower layer, and the anchor effect is reduced, so the upper layer peels off. As a result, a large amount of heat is generated due to insufficient lubricity.
また、下層に形成された凹部相互の平均水平間隔は、０．５〜１５μｍ、より好ましくは、２．０〜１０μｍの範囲内にある方が、比較的靭性が低下する凹部に焼成時負荷される応力に十分耐えうる形成密度となるために密着性が高く、下層に形成された凹部相互の平均水平間隔が０．５μｍ未満であると、下層の結晶質酸化アルミニウムが相対的に少なくなるために高い耐摩耗性を発揮することができず、一方、平均水平間隔が１５μｍを超えると、非晶質酸化シリコンが相対的に少なくなるために、潤滑性を十分に発揮することができないばかりか、アンカー効果も低下してくるため上層−下層間での密着強度が低下することから、下層に形成された凹部相互の平均水平間隔は、０．５〜１５μｍの範囲と定めた。 Further, the average horizontal interval between the recesses formed in the lower layer is 0.5 to 15 μm, and more preferably within the range of 2.0 to 10 μm. Since the formation density can sufficiently withstand the stress, the adhesion is high, and when the average horizontal interval between the recesses formed in the lower layer is less than 0.5 μm, the lower layer of crystalline aluminum oxide is relatively reduced. On the other hand, if the average horizontal distance exceeds 15 μm, the amount of amorphous silicon oxide becomes relatively small, so that the lubricity cannot be sufficiently exhibited. Further, since the anchoring effect is also lowered and the adhesion strength between the upper layer and the lower layer is lowered, the average horizontal interval between the recesses formed in the lower layer is determined to be in the range of 0.5 to 15 μm.
次に、本発明の被覆工具を得るための硬質被覆層の成膜法の一例について、以下に述べる。 Next, an example of a method for forming a hard coating layer for obtaining the coated tool of the present invention will be described below.
まず、工具基体表面と下層間に介在形成する下地層、即ち、周期律表の４ａ、５ａ、６ａ族、ＡｌおよびＳｉから選ばれる少なくとも一種以上の元素の炭化物、窒化物、炭窒化物、炭酸化物および炭窒酸化物を含有する下地層、については、従来から知られている化学蒸着法または物理蒸着法によって形成すれば良く、特段、成膜法を限定するものではない。 First, an underlayer formed between the tool base surface and the lower layer, that is, carbide, nitride, carbonitride, carbonic acid of at least one element selected from groups 4a, 5a, 6a, Al and Si in the periodic table The underlayer containing the fluoride and oxycarbonitride may be formed by a conventionally known chemical vapor deposition method or physical vapor deposition method, and the film forming method is not particularly limited.
次に、結晶質酸化アルミニウムからなる下層については、これも従来から知られている化学蒸着法で、０．８〜１０．０μｍの平均層厚を有する結晶質酸化アルミニウム層を蒸着成膜すればよい。
この蒸着により、請求項１に規定される所定の凹部が下層に形成されている場合には、この上に、後記する成膜法によって上層を形成するが、蒸着成膜した結晶質酸化アルミニウム層に、所定の凹部が形成されていない場合には、例えば、エッチング処理工程とブラスト処理工程からなる凹部形成処理を成膜後に施すことにより、下層に所定の凹部を形成することができる。
凹部形成処理におけるエッチング処理工程は、結晶質酸化アルミニウム層上にレジスト膜を成膜し、所望の凹パターンを有するマスクを使用し、露光、現像を行い、凹部を形成させたい部分のみレジスト膜を除去する。その後、例えば反応性イオンエッチング法により、該結晶質酸化アルミニウム膜をエッチングし、凹部を形成する。残存するレジスト膜除去には剥離液を使用し、エッチングの際に発生するデポ物も除去することが望ましい。
また、凹部を強調するために、エッチング処理工程後にブラスト処理工程を行うことが望ましく、特に、ブラスト投射角度：３０〜７０度、ブラスト投射圧力：８０〜２００ｋＰａ、ショットの粒径：０．０５〜０．１５ｍｍ、の条件にて鋼球をブラストするショットブラスト処理が望ましい。
なお、下層に所定の凹部を形成するための手段は、上記エッチング処理やブラスト処理ばかりでなく、成膜後の熱処理や化学蒸着条件の調整によって行うことも勿論可能である。
Next, for a lower layer made of crystalline aluminum oxide, if a crystalline aluminum oxide layer having an average layer thickness of 0.8 to 10.0 μm is vapor deposited by a conventionally known chemical vapor deposition method, Good.
When the predetermined concave portion defined in claim 1 is formed in the lower layer by this vapor deposition, an upper layer is formed thereon by a film formation method described later. In addition, when the predetermined concave portion is not formed, for example, the predetermined concave portion can be formed in the lower layer by performing a concave portion forming process including an etching process step and a blasting step after the film formation.
In the etching process in the recess forming process, a resist film is formed on the crystalline aluminum oxide layer, a mask having a desired concave pattern is used, and exposure and development are performed. Remove. Thereafter, the crystalline aluminum oxide film is etched by, for example, a reactive ion etching method to form a recess. For removing the remaining resist film, it is desirable to use a stripping solution to remove deposits generated during etching.
Moreover, in order to emphasize a recessed part, it is desirable to perform a blasting process after an etching process, especially a blast projection angle: 30-70 degree | times, a blast projection pressure: 80-200 kPa, a shot particle size: 0.05- Shot blasting is preferred in which steel balls are blasted under the condition of 0.15 mm.
Of course, the means for forming the predetermined recesses in the lower layer can be performed not only by the etching process and the blasting process, but also by a heat treatment after film formation and adjustment of chemical vapor deposition conditions.
次に、結晶質酸化アルミニウムからなる下層の表面に０．２〜４．０μｍの平均層厚を有する非晶質酸化シリコン層を成膜する。成膜方法としては、凹部に欠陥等なく充填させるよう成膜するためには、ゾル−ゲル法による成膜が望ましい。
ゾル−ゲル法による非晶質酸化シリコン層の形成は、調製及び保持を施したシリカゾルを下層の表面に塗布し、これを乾燥・焼成することによって成膜することができる。
この工程を、より具体的に述べれば、以下のとおりである。
Next, an amorphous silicon oxide layer having an average layer thickness of 0.2 to 4.0 μm is formed on the surface of the lower layer made of crystalline aluminum oxide. As a film forming method, film formation by a sol-gel method is desirable in order to form a film so as to fill the recess without defects.
The formation of the amorphous silicon oxide layer by the sol-gel method can be performed by applying the prepared and retained silica sol to the surface of the lower layer, and drying and baking it.
More specifically, this process is as follows.
シリカゾルの調製：
まず、シリコンのアルコキシド（例えば、テトラエトキシシラン）にアルコール（例えば、１−ブタノール）を添加し、さらに、所定濃度の酸（例えば、塩酸）を添加した後、２０〜４０℃以下の温度範囲にて１〜３時間攪拌することによってシリカゾルを調整する。
Preparation of silica sol:
First, an alcohol (for example, 1-butanol) is added to a silicon alkoxide (for example, tetraethoxysilane), and an acid (for example, hydrochloric acid) with a predetermined concentration is added. The silica sol is prepared by stirring for 1 to 3 hours.
シリカゾルの保持：
次いで、上記シリカゾルについて、ゾル中で起きている加水分解・縮合反応が平衡状態に至るまで待つ目的で２０〜８０℃の温度範囲にて１２時間以上保持する。
Silica sol retention:
Next, the silica sol is held at a temperature range of 20 to 80 ° C. for 12 hours or more for the purpose of waiting until the hydrolysis / condensation reaction occurring in the sol reaches an equilibrium state.
乾燥・焼成：
上記シリカゾルを、下地層上に被覆形成した下層上に塗布し、それに続き７０〜２００℃での乾燥処理を繰り返し行い、次いで、３００〜７００℃の温度範囲で焼成処理を行って、０．２〜４．０μｍの平均層厚を有する非晶質酸化シリコン層を成膜する。
Drying and firing:
The silica sol is applied onto a lower layer coated on the underlayer, followed by repeated drying at 70 to 200 ° C., followed by firing at a temperature in the range of 300 to 700 ° C., 0.2 An amorphous silicon oxide layer having an average layer thickness of ˜4.0 μm is formed.
上記非晶質酸化シリコン層の層厚は、シリカゾルの塗布厚さおよび塗布回数に依存するが、層厚が０．２μｍ未満では、長期の使用にわたってすぐれた耐摩耗性を発揮することができず、一方、層厚が４．０μｍを越えると剥離、チッピングが生じやすくなることから、上記非晶質酸化シリコン層からなる上層の平均層厚は０．２〜４．０μｍとする。 The layer thickness of the amorphous silicon oxide layer depends on the silica sol coating thickness and the number of coatings. However, if the layer thickness is less than 0.2 μm, excellent wear resistance cannot be exhibited over a long period of use. On the other hand, if the layer thickness exceeds 4.0 μm, peeling and chipping are likely to occur. Therefore, the average layer thickness of the upper layer made of the amorphous silicon oxide layer is set to 0.2 to 4.0 μm.
本発明の被覆工具によれば、下地層を介して、特定の凹形状を有する結晶質酸化アルミニウム層が下層として形成され、さらにその上に、ゾル−ゲル法により形成された非晶質酸化シリコン層が設けられていることから、硬質被覆層の潤滑性、平滑性が向上し、高い耐摩耗性を有するとともに、上層と下層の密着性が大で剥離が生じにくいことから、高熱発生を伴うとともに、断続的・衝撃的負荷が作用する高速断続切削に用いた場合でも、長期の使用に亘ってすぐれた耐摩耗性を発揮することができるのである。 According to the coated tool of the present invention, a crystalline aluminum oxide layer having a specific concave shape is formed as a lower layer through an underlayer, and further amorphous silicon oxide formed by a sol-gel method thereon. Since the layer is provided, the lubricity and smoothness of the hard coating layer are improved, it has high wear resistance, and the adhesion between the upper layer and the lower layer is large, so that it is difficult to peel off, resulting in high heat generation. At the same time, even when used for high-speed intermittent cutting in which intermittent and impact loads act, excellent wear resistance can be exhibited over a long period of use.
つぎに、この発明を実施例により具体的に説明する。 Next, the present invention will be specifically described with reference to examples.
原料粉末として、平均粒径０．８μｍの微粒ＷＣ粉末、平均粒径２〜３μｍの中粒ＷＣ粉末といずれも１〜３μｍの平均粒径を有するＴｉＣＮ粉末、ＺｒＣ粉末、ＴａＣ粉末、ＮｂＣ粉末、Ｃｒ3Ｃ2粉末およびＣｏ粉末を用意し、これら原料粉末を、表１に示す所定の配合組成に配合し、さらにワックスを加えてアセトン中で２４時間ボールミル混合し、減圧乾燥した後、９８ＭＰａの圧力で所定形状の圧粉体にプレス成形し、この圧粉体を５Ｐａの真空中、１４００℃の温度に１時間保持の条件で真空焼結し、焼結後、切刃部にＲ：０．０５ｍｍのホーニング加工を施すことによりＩＳＯ・ＣＮＭＧ１２０４０８に規定するインサート形状をもったＷＣ基超硬合金製の工具基体Ａ，Ｂ，Ｃ，Ｄ（工具基体Ａ，Ｂ，Ｃ，Ｄという）を製造した。 As raw material powder, fine WC powder having an average particle diameter of 0.8 μm, medium WC powder having an average particle diameter of 2 to 3 μm, and TiCN powder, ZrC powder, TaC powder, NbC powder each having an average particle diameter of 1 to 3 μm, Cr 3 C 2 powder and Co powder were prepared, and these raw material powders were blended in the prescribed blending composition shown in Table 1, further added with wax, ball mill mixed in acetone for 24 hours, and dried under reduced pressure. The green compact was press-molded into a green compact of a predetermined shape, and the green compact was vacuum sintered in a vacuum of 5 Pa at a temperature of 1400 ° C. for 1 hour. Manufacture tool bases A, B, C, D (tool bases A, B, C, D) made of WC-base cemented carbide with insert shape specified in ISO / CNMG120408 by honing process of .05mm did
ついで、上記工具基体Ａ〜Ｄに対して、下層を形成した。
なお、下層の形成にあたり、上記工具基体Ａ及びＢについては、化学蒸着装置に装入し、表２に示す成膜条件を用いて、粒状結晶組織を有するＴｉＮ層、ＴｉＣＮ層、ＴｉＣＯ層、ＴｉＣＮＯ層、縦長成長結晶組織のＴｉＣＮ層（以下、ｌ−ＴｉＣＮで示す）からなるＴｉ化合物層を表４に示す皮膜構成にて下地層を予め形成した。
一方、上記工具基体Ｃについては、物理蒸着装置の一種であるアークイオンプレーティング装置に装入し、表４に示す膜厚のＴｉ０．５Ａｌ０．５Ｎ層からなる下地層を予め形成した。
また、上記工具基体Ｄについては、同じくアークイオンプレーティング装置に装入し、表４に示す膜厚のＡｌ０．７Ｃｒ０．３Ｎ層からなる下地層を予め形成した。
Next, a lower layer was formed on the tool bases A to D.
In forming the lower layer, the tool bases A and B are charged into a chemical vapor deposition apparatus, and the TiN layer, TiCN layer, TiCO layer, TiCNO having a granular crystal structure are formed using the film formation conditions shown in Table 2. A Ti compound layer composed of a TiCN layer (hereinafter referred to as 1-TiCN) having a vertically elongated crystal structure was formed in advance with a coating composition shown in Table 4.
On the other hand, the tool base C is inserted into an arc ion plating apparatus which is a kind of physical vapor deposition apparatus, and an underlayer composed of a Ti 0.5 Al 0.5 N layer having a film thickness shown in Table 4 is formed in advance. did.
Further, the tool base D was similarly inserted into an arc ion plating apparatus, and an underlayer composed of an Al 0.7 Cr 0.3 N layer having a thickness shown in Table 4 was formed in advance.
ついで、下地層を形成した上記工具基体Ａ〜Ｄに対して、化学蒸着装置を用いて、所定目標層厚になるまで表２に示す成膜条件で結晶質酸化アルミニウム層を蒸着することにより下層を形成した。
なお、工具基体Ａ〜Ｄに形成された結晶質酸化アルミニウム層においては、蒸着したままの状態では、本発明で規定する凹部の形状、サイズが得られていなかったので、表３に示す条件で凹部形成処理を行い、本発明で規定する範囲内の凹部形状、サイズを形成した。エッチングガスはＣＦ４−ＣＨＦ３−Ａｒを用いた。
さらに、工具基体Ａ〜Ｄの下層に形成されている凹部について、走査型電子顕微鏡を用いた縦断面観察により、凹部の平均深さを測定するとともに、凹部のアスペクト比を凹部最大深さに対する凹部最大幅の比と定義して５点測定したのち、該アスペクト比の平均を本発明の凹部の平均アスペクト比として算出した。また、それと同様に、凹部の中心を凹部最大幅を示す線分の中点とし、凹部相互の平均水平間隔を該中心間の距離として走査型電子顕微鏡を用いて測定した結果を表４に示す。（但し、いずれの測定も、凹部形成処理実施後の測定である。）
Next, a lower layer is formed by depositing a crystalline aluminum oxide layer on the tool bases A to D on which the base layer has been formed by using a chemical vapor deposition apparatus under the film formation conditions shown in Table 2 until a predetermined target layer thickness is reached. Formed.
In the crystalline aluminum oxide layer formed on the tool bases A to D, the shape and size of the recesses defined in the present invention were not obtained in the vapor deposited state. A recess forming process was performed to form a recess shape and size within the range defined by the present invention. As the etching gas, CF 4 —CHF 3 —Ar was used.
Furthermore, about the recessed part currently formed in the lower layer of tool base | substrate A-D, while measuring the average depth of a recessed part by longitudinal cross-section observation using a scanning electron microscope, the recessed part is made into the recessed part with respect to the recessed part maximum depth. After measuring five points by defining the ratio of the maximum width, the average of the aspect ratios was calculated as the average aspect ratio of the recesses of the present invention. Similarly, Table 4 shows the results of measurement using a scanning electron microscope with the center of the recess as the midpoint of the line segment indicating the maximum width of the recess and the average horizontal interval between the recesses as the distance between the centers. . (However, all measurements are measurements after the recess formation process is performed.)
ついで、それぞれ下層を被覆形成した上記工具基体Ａ〜Ｄに対して、次の（イ）〜（ハ）の工程で、非晶質酸化シリコン層をゾルーゲル法で被覆形成した。
（イ）まず、反応原料における各成分の溶液組成はモル比で、
（テトラエトキシシラン）：（水）：（１−ブタノール）：（塩酸）
＝１：５０〜２００：５〜１０：０．１〜０．５
になるよう添加して、恒温槽中３０℃で攪拌を行い、さらに、６０℃で１２時間保持させることで、攪拌を継続し、シリカゾルを調製した。
（ロ）ついで、上記工具基体Ａ〜Ｄの下層表面に上記シリカゾルを塗布した。
（ハ）ついで、上記塗布したシリカゾルを、大気中１５０℃で０．５時間の乾燥処理を行い、さらに塗布と乾燥を所定層厚になるまで繰り返した後、大気中６００℃で１時間の焼成処理を行うことにより、表４に示す本発明の被覆工具１〜１２（本発明工具１〜１２という）を製造した。
Subsequently, an amorphous silicon oxide layer was formed by a sol-gel method in the following steps (a) to (c) on the tool bases A to D each having a lower layer formed thereon.
(A) First, the solution composition of each component in the reaction raw material is a molar ratio,
(Tetraethoxysilane): (water): (1-butanol): (hydrochloric acid)
= 1: 50-200: 5-10: 0.1-0.5
Then, the mixture was stirred at 30 ° C. in a thermostatic bath, and further kept at 60 ° C. for 12 hours, whereby stirring was continued to prepare a silica sol.
(B) Next, the silica sol was applied to the lower layer surfaces of the tool bases A to D.
(C) Next, the applied silica sol is dried in air at 150 ° C. for 0.5 hours, and further, coating and drying are repeated until a predetermined layer thickness is obtained, followed by baking in air at 600 ° C. for 1 hour. By carrying out the treatment, coated tools 1 to 12 (referred to as present invention tools 1 to 12) of the present invention shown in Table 4 were produced.
上記本発明工具１〜１２について、下層、上層の結晶構造を透過電子顕微鏡により、制限電子回折による構造解析を行ったところ、下層は明瞭な電子回折パターンが得られ、αまたはκ型の結晶構造を有する酸化アルミニウム、また、上層はハローパターンが得られたことから非晶質酸化シリコンで構成されていることが確認され、また、透過電子顕微鏡を用いた縦断面観察を行い、凹部近傍の下層と上層との界面を詳細に観察したところ、下層の凹部に上層の非晶質酸化シリコンがポア等なく埋め込まれたような状態で充填されていることが確認された。また、同時に上層、下層の平均層厚を透過型電子顕微鏡を用いて断面測定したところ、いずれも目標層厚と実質的に同じ平均値（５ヶ所の平均値）を示した。 Regarding the above-described tools 1 to 12 of the present invention, when the crystal structure of the lower layer and the upper layer was subjected to structural analysis by restricted electron diffraction using a transmission electron microscope, a clear electron diffraction pattern was obtained for the lower layer, and the α or κ type crystal structure The upper layer was confirmed to be composed of amorphous silicon oxide because the halo pattern was obtained, and the longitudinal section was observed using a transmission electron microscope, and the lower layer near the recess When the interface between the upper layer and the upper layer was observed in detail, it was confirmed that the upper layer of amorphous silicon oxide was filled in the recesses of the lower layer without being filled with pores. At the same time, when the average layer thicknesses of the upper layer and the lower layer were measured by cross-section using a transmission electron microscope, both showed the same average value (average value of 5 locations) as the target layer thickness.
次に、被覆工具の切削性能に及ぼす下層（結晶質酸化アルミニウム層）の平均層厚と凹部の形状・サイズの影響を調査するため、工具基体Ａ〜Ｄを用いて、下地層及び下層の平均層厚を変更するとともに、表３に示す種々の条件で凹部形成処理を施すことにより、１２種類の比較材１〜１２を作製した。
そして、その結果得られた比較材１〜１２に形成された下層の凹部形状・サイズを測定し、その平均値を求めた。
表５に、下層の平均層厚、凹部形成処理条件、また、その結果得られた下層の凹部形状・サイズの測定平均値を示す。
Next, in order to investigate the influence of the average layer thickness of the lower layer (crystalline aluminum oxide layer) and the shape and size of the recesses on the cutting performance of the coated tool, the average of the lower layer and the lower layer was used using the tool bases A to D. Twelve types of comparative materials 1 to 12 were produced by changing the layer thickness and performing a recess formation process under various conditions shown in Table 3.
And the recessed part shape and size of the lower layer formed in the comparative materials 1-12 obtained as a result were measured, and the average value was calculated | required.
Table 5 shows the average layer thickness of the lower layer, the recess formation processing conditions, and the measured average values of the recess shape and size of the lower layer obtained as a result.
ついで、上記比較材１〜１２に対して、前記（イ）〜（ハ）と同様な工程で、シリカゾルの調製、保持を行い、下層表面に塗布、乾燥、焼成を行うことで、表５に示す比較例の被覆工具１〜１２（比較例工具１〜１２という）を作製した。 Then, for the comparative materials 1 to 12, the silica sol is prepared and held in the same steps as in the above (a) to (c), and applied to the lower layer surface, dried and fired. Coated tools 1 to 12 (referred to as comparative example tools 1 to 12) of the comparative examples shown were produced.
上記比較例工具１〜１２について、下層、上層の結晶構造を透過電子顕微鏡を用いて構造解析したところ、下層はαまたはκ型の結晶構造を有する結晶質酸化アルミニウム、また、上層は非晶質酸化シリコンで構成されていることが確認されたが、同様に、透過電子顕微鏡を用いて凹部近傍の下層と上層との界面を観察したところ、一部の比較例工具では、下層の凹部に上層の非晶質酸化シリコンが十分に充填されておらず、ポアや密度の薄い部分が存在した。 Regarding the comparative tools 1 to 12, when the crystal structure of the lower layer and the upper layer was analyzed using a transmission electron microscope, the lower layer was crystalline aluminum oxide having an α or κ type crystal structure, and the upper layer was amorphous. Although it was confirmed that it was composed of silicon oxide, similarly, when the interface between the lower layer and the upper layer in the vicinity of the concave portion was observed using a transmission electron microscope, in some comparative tools, the upper layer was formed in the lower concave portion. The amorphous silicon oxide was not sufficiently filled, and there were pores and low density portions.
つぎに、上記本発明工具１〜１２、比較例工具１〜１２について、次の条件で湿式高速断続切削加工試験を行った。 Next, a wet high-speed intermittent cutting test was performed on the above-described inventive tools 1 to 12 and comparative tools 1 to 12 under the following conditions.
被削材：ＪＩＳ・ＳＵＳ４３０の長さ方向等間隔４本縦溝入り丸棒、
切削速度：１７０ｍ／ｍｉｎ．、
切り込み：１．２ ｍｍ、
送り：０．２３ｍｍ／ｒｅｖ．、
切削時間： ５ 分、
（通常の切削速度は、１２０ ｍ／ｍｉｎ．）
切削加工試験後の、それぞれの工具の摩耗状態について観察を行い、逃げ面摩耗量の測定を行うとともに、硬質被覆層の損傷状況を観察した。
表６に、これらの結果を示す。
Work material: JIS / SUS430 lengthwise equal 4 round bars with flutes,
Cutting speed: 170 m / min. ,
Cutting depth: 1.2 mm,
Feed: 0.23 mm / rev. ,
Cutting time: 5 minutes,
(Normal cutting speed is 120 m / min.)
After the cutting test, the wear state of each tool was observed, the flank wear amount was measured, and the damage state of the hard coating layer was observed.
Table 6 shows these results.
原料粉末として、いずれも０．５〜２μｍの平均粒径を有するＴｉＣＮ（質量比でＴｉＣ／ＴｉＮ＝５０／５０）粉末、Ｍｏ2Ｃ粉末、ＺｒＣ粉末、ＮｂＣ粉末、ＴａＣ粉末、ＷＣ粉末、Ｃｏ粉末、およびＮｉ粉末を用意し、これらを表７に示す所定の配合組成に配合し、ボールミルで２４時間湿式混合し、乾燥した後、９８ＭＰａの圧力で圧粉体にプレス成形し、この圧粉体を１．３ｋＰａの窒素雰囲気中、温度：１５４０℃に１時間保持の条件で焼結し、焼結後、切刃部分にＲ：０．０７ｍｍのホーニング加工を施すことによりＩＳＯ規格・ＣＮＭＧ１２０４１２のチップ形状をもったＴｉＣＮ基サーメット製の工具基体Ｅ，Ｆ，Ｇ，Ｈ（工具基体Ｅ〜Ｈという）を製造した。 As raw material powders, TiCN (mass ratio TiC / TiN = 50/50) powder, Mo 2 C powder, ZrC powder, NbC powder, TaC powder, WC powder, Co having an average particle diameter of 0.5 to 2 μm. Powders and Ni powders were prepared, blended in the prescribed blending composition shown in Table 7, wet-mixed for 24 hours with a ball mill, dried, and press-molded into compacts at a pressure of 98 MPa. The body was sintered in a nitrogen atmosphere of 1.3 kPa at a temperature of 1540 ° C. for 1 hour, and after sintering, the cutting edge portion was subjected to honing of R: 0.07 mm to achieve ISO standard / CNMG12041 Tool bases E, F, G, and H made of TiCN-based cermets having chip shapes (referred to as tool bases E to H) were manufactured.
ついで、上記工具基体Ｅ，Ｆについては化学蒸着法により、それぞれ、表８に示すＴｉ化合物下地層を形成し、工具基体Ｇについては、アークイオンプレーティング装置を用い、表８に示す膜厚のＴｉ０．５Ａｌ０．５Ｎ層からなる下地層を物理蒸着により予め被覆形成した。
また、上記工具基体Ｈについても、同じくアークイオンプレーティング装置で、表８に示す膜厚のＡｌ０．７Ｃｒ０．３Ｎ層からなる下地層を予め被覆形成した。
Next, a Ti compound base layer shown in Table 8 is formed for each of the tool bases E and F by chemical vapor deposition, and a film thickness shown in Table 8 is used for the tool base G using an arc ion plating apparatus. A base layer composed of a Ti 0.5 Al 0.5 N layer was previously formed by physical vapor deposition.
In addition, for the tool base H, a base layer made of an Al 0.7 Cr 0.3 N layer having a thickness shown in Table 8 was previously formed by coating using the same arc ion plating apparatus.
ついで、上記工具基体Ｅ〜Ｈに対して、ＣＶＤ装置を用い、所定目標膜厚になるまで表２に示す条件で結晶質酸化アルミニウム層を蒸着することにより下層を形成した。
なお、工具基体Ｅ〜Ｈに形成された結晶質酸化アルミニウム層においては、蒸着したままの状態では、本発明で規定する凹部の形状、サイズが得られていなかったので、表３に示す条件で凹部形成処理を施し、下層に、本発明で規定する範囲内の凹部形状、サイズを形成した。
表８に、工具基体Ｅ〜Ｈの下層に形成されている凹部について、縦断面の走査型電子顕微鏡観察において測定した凹部の形状、サイズの平均値を示す。（但し、いずれの測定も、凹部形成処理実施後の測定である。）
Next, a lower layer was formed by depositing a crystalline aluminum oxide layer on the tool bases E to H using a CVD apparatus under the conditions shown in Table 2 until a predetermined target film thickness was reached.
In addition, in the crystalline aluminum oxide layer formed on the tool bases E to H, since the shape and size of the recess defined in the present invention were not obtained in the state of being deposited, the conditions shown in Table 3 were used. Recess formation processing was performed, and the recess shape and size within the range specified by the present invention were formed in the lower layer.
Table 8 shows the average values of the shape and size of the recesses measured by scanning electron microscope observation of the longitudinal section of the recesses formed in the lower layers of the tool bases E to H. (However, all measurements are measurements after the recess formation process is performed.)
ついで、それぞれ下層を被覆形成した上記工具基体Ｅ〜Ｈに対して、実施例１の前記（イ）〜（ハ）と同様の処理を施すことにより、本発明の被覆工具１３〜２４（本発明工具１３〜２４という）を製造した。 Next, the above-mentioned tool bases E to H, each of which has a lower layer formed thereon, are subjected to the same treatment as in the above (a) to (c) of Example 1 to thereby provide the coated tools 13 to 24 (the present invention). Tools 13-24).
上記本発明工具１３〜２４について、下層、上層の結晶構造を透過電子顕微鏡を用いて構造解析を行ったところ下層はαまたはκ型の結晶構造を有する酸化アルミニウム、また、上層は非晶質酸化シリコンで構成されていることが確認され、また、同様に、透過電子顕微鏡を用いて凹部近傍の下層と上層との界面を観察したところ、下層の凹部に上層の非晶質酸化シリコンがポア等なく埋め込まれたような状態で充填されていることが確認された。 As for the above-described inventive tools 13 to 24, the crystal structure of the lower layer and the upper layer was analyzed using a transmission electron microscope. The lower layer was aluminum oxide having an α or κ type crystal structure, and the upper layer was an amorphous oxide. Similarly, when the interface between the lower layer and the upper layer in the vicinity of the concave portion was observed using a transmission electron microscope, the upper layer of amorphous silicon oxide was pored in the lower concave portion. It was confirmed that it was filled without being embedded.
次に、被覆工具の切削性能に及ぼす下層（結晶質酸化アルミニウム層）の平均層厚と凹部の形状・サイズの影響を調査するため、工具基体Ｅ〜Ｈを用いて、下地層及び下層の平均層厚を変更するとともに、表３に示す種々の条件で凹部形成処理を施すことにより、１２種類の比較材１３〜２４を作製した。
そして、その結果得られた比較材１３〜２４に形成された下層の凹部形状・サイズを測定し、その平均値を求めた。
表９に、下層の平均層厚、凹部形成処理条件、また、その結果得られた下層の凹部形状・サイズの測定平均値を示す。
Next, in order to investigate the influence of the average layer thickness of the lower layer (crystalline aluminum oxide layer) and the shape and size of the recesses on the cutting performance of the coated tool, the average of the lower layer and the lower layer was used using the tool bases E to H. Twelve types of comparative materials 13 to 24 were produced by changing the layer thickness and performing a recess formation process under various conditions shown in Table 3.
And the recessed part shape and size of the lower layer formed in the comparative materials 13-24 obtained as a result were measured, and the average value was calculated | required.
Table 9 shows the measured average values of the lower layer average layer thickness, the recess formation process conditions, and the lower layer recess shape and size obtained as a result.
ついで、上記比較材１３〜２４に対して、前記（イ）〜（ハ）と同様な工程で、シリカゾルの調製、保持を行い、下層表面に塗布、乾燥、焼成を行うことで、表９に示す比較例の被覆工具１３〜２４（比較例工具１３〜２４という）を作製した。 Then, for the comparative materials 13 to 24, the silica sol is prepared and held in the same steps as in the above (a) to (c), and applied to the lower layer surface, dried, and fired. Coated tools 13 to 24 (referred to as comparative example tools 13 to 24) of the comparative examples shown were produced.
上記比較例工具１３〜２４について、下層、上層の結晶構造を透過電子顕微鏡を用いた構造解析を行ったところ、下層はαまたはκ型の結晶構造を有する酸化アルミニウム、また、上層は非晶質酸化シリコンで構成されていることが確認されたが、凹部近傍の下層と上層との界面を観察したところ、一部の比較例工具では、下層の凹部に上層の非晶質酸化シリコンが十分に充填されていないことがわかった。 For the comparative tools 13 to 24, the lower and upper crystal structures were analyzed using a transmission electron microscope. The lower layer was an aluminum oxide having an α or κ crystal structure, and the upper layer was amorphous. It was confirmed that it was composed of silicon oxide, but when the interface between the lower layer and the upper layer near the recess was observed, in some comparative tools, the upper layer of amorphous silicon oxide was sufficiently in the lower recess It was found that it was not filled.
つぎに、上記本発明工具１３〜２４、比較例工具１３〜２４について、次の条件で乾式高速断続切削加工試験を行った。
被削材：ＪＩＳ・Ｓ５０Ｃの長さ方向等間隔４本縦溝入り丸棒、
切削速度： ３３０ ｍ／ｍｉｎ．、
切り込み： １．５ ｍｍ、
送り： ０．２４ ｍｍ／ｒｅｖ．、
切削時間： ５分、
（通常の切削速度は、２００ ｍ／ｍｉｎ）
切削加工試験後の、それぞれの工具の摩耗状態について観察を行い、逃げ面摩耗量の測定を行うとともに、硬質被覆層の損傷状況を観察した。
これらの結果を表１０に示す。
Next, a dry high-speed intermittent cutting test was performed on the above-described inventive tools 13 to 24 and comparative tools 13 to 24 under the following conditions.
Work material: JIS / S50C lengthwise equal 4 round grooved round bars,
Cutting speed: 330 m / min. ,
Cutting depth: 1.5 mm,
Feed: 0.24 mm / rev. ,
Cutting time: 5 minutes
(Normal cutting speed is 200 m / min)
After the cutting test, the wear state of each tool was observed, the flank wear amount was measured, and the damage state of the hard coating layer was observed.
These results are shown in Table 10.
表４〜６、８〜１０に示される結果から、本発明の被覆工具によれば、硬質被覆層の下層が、特定の凹部形状を有するαまたはκ型の結晶構造を有する酸化アルミニウム層で構成され、その上層として、ゾル−ゲル法により形成された非晶質酸化シリコン層が設けられていることから、硬質被覆層の潤滑性、平滑性が向上し、高い耐摩耗性を有するとともに、上層と下層の密着性が大で剥離が生じにくいことがわかる。 From the results shown in Tables 4 to 6 and 8 to 10, according to the coated tool of the present invention, the lower layer of the hard coating layer is composed of an aluminum oxide layer having an α or κ type crystal structure having a specific concave shape. Since the amorphous silicon oxide layer formed by the sol-gel method is provided as the upper layer, the lubricity and smoothness of the hard coating layer are improved, and the upper layer has high wear resistance. It can be seen that the adhesion between the lower layer and the lower layer is large and peeling does not easily occur.
これに対して、硬質被覆層の下層が、特定の凹部形状を有する結晶質酸化アルミニウム層で構成されていない比較例の被覆工具では、硬質被覆層の潤滑性、平滑性が劣り、また、耐摩耗性も劣り、さらに、剥離も生じるため、短時間で使用寿命に至ることは明らかである。 On the other hand, in the comparative coated tool in which the lower layer of the hard coating layer is not composed of a crystalline aluminum oxide layer having a specific concave shape, the lubricity and smoothness of the hard coating layer are inferior, It is obvious that the wear life is inferior, and further, peeling occurs, so that the service life is reached in a short time.
この発明の耐チッピング性、耐剥離性、耐摩耗性にすぐれた表面被覆切削工具によれば、高熱発生を伴うと共に、断続的・衝撃的負荷が作用する高速断続切削に用いた場合に、長期の使用に亘ってすぐれた耐摩耗性を発揮するものであるから、工具寿命の長寿命化を図れるばかりか、製造工程上の省資源、省エネにも寄与し得るものであって、実用上の効果が大である。
According to the surface-coated cutting tool having excellent chipping resistance, peel resistance, and wear resistance according to the present invention, when used for high-speed intermittent cutting with high heat generation and intermittent / impact loads, Because it exhibits excellent wear resistance over the use of the tool, not only can the tool life be extended, but it can also contribute to resource saving and energy saving in the manufacturing process. The effect is great.
Claims (2)
（ａ）該下地層は、１．０〜１５．０μｍの平均層厚を有する周期律表の４ａ、５ａ、６ａ族、ＡｌおよびＳｉから選ばれる少なくとも一種以上の元素の炭化物、窒化物、炭窒化物、炭酸化物および炭窒酸化物層であって、
（ｂ）下層は、０．８〜１０．０μｍの平均層厚を有する結晶質酸化アルミニウム層、
（ｃ）上層は、０．２〜４．０μｍの平均層厚を有する非晶質酸化シリコン層であって、
（ｄ）下層の結晶質酸化アルミニウム層の表面には、凹部が形成されており、上層の非晶質酸化シリコン層は、下層の上記凹部を埋め込むように充填成膜されており、
（ｅ）下層に形成された凹部の平均深さは、０．５〜１０．０μｍの範囲（但し、下層の平均層厚以下）であり、
（ｆ）下層に形成された凹部の平均アスペクト比は、１．０〜４０の範囲であり、
（ｇ）下層に形成された凹部相互の平均水平間隔は、０．５〜１５μｍの範囲であることを特徴とする表面被覆切削工具。 Underlayer was made form the surface of the tungsten carbide based cemented carbide or tool substrate made of titanium carbonitride based cermet, and on the lower strata, the hard composed of a top layer consisting of a lower layer and a silicon oxide consisting of aluminum oxide In a surface-coated cutting tool with a coating layer formed ,
(A) The underlayer is composed of carbide, nitride, charcoal of at least one element selected from Group 4a, 5a, 6a, Al and Si in the periodic table having an average layer thickness of 1.0 to 15.0 μm. A nitride, carbonate and carbonitride layer,
(B) The lower layer is 0 . A crystalline aluminum oxide layer having an average layer thickness of 8 to 10.0 μm;
(C) The upper layer is an amorphous silicon oxide layer having an average layer thickness of 0.2 to 4.0 μm,
(D) A concave portion is formed on the surface of the lower crystalline aluminum oxide layer, and the upper amorphous silicon oxide layer is filled to fill the lower concave portion,
(E) The average depth of the recesses formed in the lower layer is in the range of 0.5 to 10.0 μm (however, below the average layer thickness of the lower layer),
(F) The average aspect ratio of the recesses formed in the lower layer is in the range of 1.0 to 40,
(G) The surface-coated cutting tool, wherein the average horizontal interval between the recesses formed in the lower layer is in the range of 0.5 to 15 μm.
The surface-coated cutting tool according to claim 1, wherein the lower layer aluminum oxide has a κ-type crystal structure.
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|---|---|---|---|---|
| JPH0892741A (en) * | 1994-09-20 | 1996-04-09 | New Japan Radio Co Ltd | Surface treatment of sintered hard alloy for deposition with diamond |
| US5571616A (en) * | 1995-05-16 | 1996-11-05 | Crystallume | Ultrasmooth adherent diamond film coated article and method for making same |
| JP3236910B2 (en) * | 1996-03-13 | 2001-12-10 | 三菱マテリアル株式会社 | Surface-coated tungsten carbide based cemented carbide cutting tool with excellent fracture resistance with hard coating layer |
| JPH11229144A (en) * | 1998-02-12 | 1999-08-24 | Hitachi Tool Eng Ltd | Coated tool |
| WO2007049785A1 (en) * | 2005-10-28 | 2007-05-03 | Kyocera Corporation | Surface-coated member, method for manufacture thereof, and cutting tool |
| JP2007130741A (en) * | 2005-11-14 | 2007-05-31 | Mitsubishi Materials Corp | Surface coated cemented carbide cutting tool having hard coating layer exhibiting superior chipping resistance in heavy cutting for material hard to cut |
| JP5321356B2 (en) * | 2009-08-28 | 2013-10-23 | 三菱マテリアル株式会社 | Surface coated cutting tool |
| JP5876724B2 (en) * | 2011-12-27 | 2016-03-02 | 三菱マテリアル株式会社 | Surface coated cutting tool with excellent chipping resistance, peel resistance and wear resistance |
-
2012
- 2012-03-15 JP JP2012058156A patent/JP5850405B2/en active Active
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2013
- 2013-01-09 CN CN 201310007912 patent/CN103302324A/en active Pending
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| Publication number | Publication date |
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| CN103302324A (en) | 2013-09-18 |
| JP2013188852A (en) | 2013-09-26 |
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