JP2011152601A - Surface-coated cutting tool provided with hard coated layer demonstrating superior chipping resistance - Google Patents
Surface-coated cutting tool provided with hard coated layer demonstrating superior chipping resistance Download PDFInfo
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- 238000005520 cutting process Methods 0.000 title claims abstract description 49
- 239000013078 crystal Substances 0.000 claims abstract description 81
- 238000005259 measurement Methods 0.000 claims abstract description 19
- 238000010894 electron beam technology Methods 0.000 claims abstract description 7
- 239000010410 layer Substances 0.000 claims description 46
- 239000011247 coating layer Substances 0.000 claims description 20
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims description 3
- 238000005240 physical vapour deposition Methods 0.000 abstract description 3
- 239000010936 titanium Substances 0.000 description 52
- 239000007789 gas Substances 0.000 description 16
- 239000002184 metal Substances 0.000 description 12
- 229910052751 metal Inorganic materials 0.000 description 12
- 238000004544 sputter deposition Methods 0.000 description 8
- 238000000151 deposition Methods 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 230000008020 evaporation Effects 0.000 description 6
- 238000001704 evaporation Methods 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- 238000007733 ion plating Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000003801 milling Methods 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 229910001018 Cast iron Inorganic materials 0.000 description 3
- 229910004339 Ti-Si Inorganic materials 0.000 description 3
- 229910010978 Ti—Si Inorganic materials 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001887 electron backscatter diffraction Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 239000012495 reaction gas Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- 229910008482 TiSiN Inorganic materials 0.000 description 1
- 229910001315 Tool steel Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 235000000396 iron Nutrition 0.000 description 1
- QRXWMOHMRWLFEY-UHFFFAOYSA-N isoniazide Chemical compound NNC(=O)C1=CC=NC=C1 QRXWMOHMRWLFEY-UHFFFAOYSA-N 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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- Physical Vapour Deposition (AREA)
Abstract
Description
この発明は、硬質被覆層が微細な柱状晶として形成されるとともに、靭性にすぐれる二軸配向ドメインを備えることから、鋼や鋳鉄などの高速切削加工という厳しい切削条件下で用いられた場合にも、すぐれた耐熱性と耐欠損性を示し、切削工具の長寿命化が可能とな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 formed when the hard coating layer is formed as fine columnar crystals and has a biaxially oriented domain with excellent toughness, so that it is used under severe cutting conditions such as high-speed cutting of steel and cast iron. Further, the present invention relates to a surface-coated cutting tool (hereinafter referred to as a coated tool) that exhibits excellent heat resistance and fracture resistance and can extend the life of the cutting tool.
一般に、被覆工具には、各種の鋼や鋳鉄などの被削材の旋削加工にバイトの先端部に着脱自在に取り付けて用いられるインサートや、前記インサートを着脱自在に取り付けて、面削加工や溝加工、さらに肩加工などに用いられるソリッドタイプのエンドミルと同様に切削加工を行うインサート式エンドミルなどが知られている。 In general, for coated tools, inserts that are detachably attached to the tip of a cutting tool for turning of work materials such as various types of steel and cast iron, and the inserts are detachably attached to be used for chamfering and grooving. An insert type end mill that performs cutting processing in the same manner as a solid type end mill used for processing and shoulder processing is known.
また、被覆工具として、炭化タングステン（以下、ＷＣで示す）基超硬合金焼結体で構成された工具基体の表面に、Ｔｉ−Ｓｉの窒化物（以下、Ｔｉ1-ｘＳｉｘＮで示す）層からなる硬質被覆層を物理蒸着してなる被覆工具が広く知られており、各種の鋼や鋳鉄などの連続切削や断続切削加工に用いられている。
特にＴｉおよびＳｉなどの窒化物あるいは炭窒化物の結晶構造に着目した技術として、特許文献１および特許文献２に示される文献では、化学蒸着法によって蒸着された、チタンの炭窒化物が双晶構造を持つことにより、硬質被覆層を形成する粒同士の結合力を高める技術が提案されている。また、特許文献３に示される文献では、硬質被覆層を形成するＴｉＳｉＮの結晶粒が、工具基体の法線方向から０度〜１５度の方向に結晶方位＜１１１＞を有する結晶粒が全体の１５％を占め、隣り合う結晶粒同士のなす角を測定した場合に、小角粒界（０〜１５度）の割合が５０％であるような結晶配列を示すチタンの炭窒化物を構成することで、表面被覆切削工具の耐欠損性を向上させる技術が提案されている。
Further, a Ti—Si nitride (hereinafter referred to as Ti 1-x Si x N) is formed on the surface of a tool base composed of a tungsten carbide (hereinafter referred to as WC) based cemented carbide sintered body as a coated tool. A coating tool formed by physically vapor-depositing a hard coating layer is widely known, and is used for continuous cutting and intermittent cutting of various steels and cast iron.
In particular, as a technique paying attention to the crystal structure of nitride or carbonitride such as Ti and Si, in the documents shown in
近年の切削加工装置のＦＡ化はめざましく、加えて切削加工に対する省力化、省エネ化、低コスト化さらに効率化の要求も強く、これに伴い、高送り、高切り込みなどより高効率の重切削加工が要求される傾向にあるが、上記の従来被覆工具においては、各種の鋼や鋳鉄を通常条件下で切削加工した場合に特段の問題は生じないが、切刃に対して衝撃的かつ断続的な高負荷が作用する乾式の高速フライス加工などの断続高速切削に用いた場合には、硬質被覆層の内部にクラックが発達しやすいとともに、硬質被覆層の耐熱性が低いことから、硬質被覆層の欠損を生じやすく切刃部の欠損が生じ、これが原因で、比較的短時間で使用寿命に至るのが現状である。 In recent years, the FA of cutting devices has been remarkable, and in addition, there are strong demands for labor saving, energy saving, cost reduction and efficiency for cutting, and with this, high-efficiency heavy cutting such as high feed and high cutting However, in the above-mentioned conventional coated tools, there are no particular problems when various steels and cast irons are machined under normal conditions, but they are shocking and intermittent to the cutting edge. When it is used for intermittent high-speed cutting such as dry high-speed milling where high load is applied, cracks are likely to develop inside the hard coating layer and the heat resistance of the hard coating layer is low. The cutting edge portion is easily damaged, and this causes the service life to be reached in a relatively short time.
そこで、本発明者等は、上述のような観点から、被覆工具の耐欠損性を高め、使用寿命の延命化を図るべく、Ｔｉ1-ｘＳｉｘＮ層からなる硬質被覆層の結晶形態に着目し、鋭意研究を行った結果、次のような知見を得た。 In view of the above, the inventors of the present invention have adopted the crystalline form of the hard coating layer composed of the Ti 1-x Si x N layer in order to increase the fracture resistance of the coated tool and extend the service life. The following findings were obtained as a result of intensive research.
従来の被覆工具のＴｉ1-ｘＳｉｘＮ層からなる硬質被覆層は、例えば、図２に示される物理蒸着装置の１種であるスパッタリング（ＳＰ）装置に上記のＷＣ基超硬合金焼結体からなる工具基体を装着し、例えば、
装置内加熱温度：３００〜５００℃、
工具基体に印加する直流バイアス電圧：−５０〜−１００Ｖ、
カソード電極：Ｔｉ-Ｓｉ合金
スパッタリング電力：３〜６ｋＷ、
装置内ガス流量：窒素（Ｎ２）ガス＋アルゴン（Ａｒ）ガス、
装置内ガス圧力：０．３〜１．５Ｐａ、
の条件で、Ｔｉ1-ｘＳｉｘＮ層（以下、従来Ｔｉ1-ｘＳｉｘＮ層という）を形成することにより製造されている。
For example, a hard coating layer made of a Ti 1-x Si x N layer of a conventional coating tool can be obtained by sintering the above WC-based cemented carbide alloy in a sputtering (SP) apparatus, which is a kind of physical vapor deposition apparatus shown in FIG. Wearing a tool base consisting of a body, for example,
In-apparatus heating temperature: 300-500 ° C
DC bias voltage applied to the tool base: −50 to −100 V,
Cathode electrode: Ti-Si alloy Sputtering power: 3-6 kW,
Gas flow in the apparatus: nitrogen (N 2 ) gas + argon (Ar) gas,
In-apparatus gas pressure: 0.3 to 1.5 Pa,
Under these conditions, a Ti 1-x Si x N layer (hereinafter referred to as a conventional Ti 1-x Si x N layer) is formed.
しかし、本発明者等は、Ｔｉ1-ｘＳｉｘＮ層の形成を、例えば図１に概略説明図で示される物理蒸着装置の１種である圧力勾配型Ａｒプラズマガスを利用したイオンプレーティング装置を用いて、装置内に上記の工具基体を装着し、
工具基体温度：２４０〜４００ ℃、
蒸発源：金属Ｔｉ、金属Ｓｉ
プラズマガン放電電力 金属Ｔｉに対して：１０〜１２ ｋＷ、
プラズマガン放電電力 金属Ｓｉに対して：５〜８ ｋＷ、
反応ガス流量：窒素（Ｎ２）ガス ８０〜１２０ ｓｃｃｍ、
放電ガス：アルゴン（Ａｒ）ガス ３０〜５０ ｓｃｃｍ、
工具基体に印加する直流バイアス電圧： ０ Ｖ、
蒸着速度： ０．０４〜０．１１ ｎｍ／秒
という条件下で蒸着を行うと、このＴｉ1-ｘＳｉｘＮ層（以下、改質Ｔｉ1-ｘＳｉｘＮ層という）は、前記従来Ｔｉ1-ｘＳｉｘＮ層に比して、切刃に対して高負荷がかかる高送り、高切り込みの重切削加工において、すぐれた耐摩耗性と耐欠損性を示すことを見出したのである。
However, the present inventors have formed a Ti 1-x Si x N layer by ion plating using, for example, a pressure gradient type Ar plasma gas which is a kind of physical vapor deposition apparatus schematically shown in FIG. Using the device, install the tool base in the device,
Tool substrate temperature: 240-400 ° C.
Evaporation source: Metal Ti, Metal Si
Plasma gun discharge power For metal Ti: 10-12 kW,
Plasma gun discharge power For metal Si: 5 to 8 kW,
Reaction gas flow rate: nitrogen (N 2) gas 80 to 120 sccm,
Discharge gas: Argon (Ar) gas 30-50 sccm,
DC bias voltage applied to the tool base: 0 V,
Deposition rate: When Ti is deposited under the condition of 0.04 to 0.11 nm / second, this Ti 1-x Si x N layer (hereinafter referred to as a modified Ti 1-x Si x N layer) It has been found that it has excellent wear resistance and fracture resistance in heavy feed machining with high feed and high depth of cut, which requires a high load on the cutting edge, compared to the Ti 1-x Si x N layer. .
この発明は、上記の研究結果に基づいてなされたものであって、
「炭化タングステン基超硬合金焼結体からなる工具基体の表面に、０．２〜２μｍの平均層厚を有するＴｉ1-ｘＳｉｘＮ膜からなる硬質被覆層を物理蒸着した表面被覆切削工具において、ｘが ０．１≦ｘ≦０．３を満たし、さらに、
上記Ｔｉ1-ｘＳｉｘＮ層は上記平均層厚と等しい高さを有する柱状晶組織からなり、さらに、上記Ｔｉ1-ｘＳｉｘＮ層の水平断面における結晶粒組織を観察した場合、粒径が１０〜１００ｎｍの結晶粒が測定面積のうち９０％以上を占有し、かつ、電子線後方散乱回折装置で表面の結晶粒の結晶方位を測定した場合、隣り合う測定点との結晶方位の差が１５度以上となる結晶界面によって囲まれた直径０．２〜４μｍの区分が、測定された全体の面積のうち２０％以上を占有することを特徴とする表面被覆切削工具。」
に特徴を有するものである。
This invention was made based on the above research results,
“A surface-coated cutting tool obtained by physically vapor-depositing a hard coating layer made of a Ti 1-x Si x N film having an average layer thickness of 0.2 to 2 μm on the surface of a tool base made of a tungsten carbide-based cemented carbide sintered body X satisfies 0.1 ≦ x ≦ 0.3, and
The Ti 1-x Si x N layer has a columnar crystal structure having a height equal to the average layer thickness. Further, when the crystal grain structure in the horizontal section of the Ti 1-x Si x N layer is observed, When the crystal grains having a diameter of 10 to 100 nm occupy 90% or more of the measurement area and the crystal orientation of the crystal grains on the surface is measured with an electron beam backscattering diffractometer, the crystal orientation of the adjacent measurement point A surface-coated cutting tool characterized in that a section having a diameter of 0.2 to 4 μm surrounded by a crystal interface having a difference of 15 degrees or more occupies 20% or more of the total area measured. "
It has the characteristics.
この発明について、以下に詳細に説明する。 The present invention will be described in detail below.
既に述べたように、この発明は、例えば図１に概略説明図で示される圧力勾配型Ａｒプラズマガスを利用したイオンプレーティング装置を用いて、装置内にＷＣ基超硬合金焼結体からなる工具基体を装着し、
工具基体温度：２４０〜４００ ℃、
蒸発源：金属Ｔｉ、金属Ｓｉ
プラズマガン放電電力 金属Ｔｉに対して：１０〜１２ ｋＷ、
プラズマガン放電電力 金属Ｓｉに対して：５〜８ ｋＷ、
反応ガス流量：窒素（Ｎ２）ガス ８０〜１２０ ｓｃｃｍ、
放電ガス：アルゴン（Ａｒ）ガス ３０〜５０ ｓｃｃｍ、
工具基体に印加する直流バイアス電圧： ０ Ｖ、
蒸着速度： ０．０４〜０．１１ ｎｍ／秒、
という条件下で成膜を行うものである。従来Ｔｉ1-ｘＳｉｘＮ層の構成成分であるＴｉ成分が高温強度を向上させ、Ｓｉ成分が耐熱性を向上させ、また、Ｎが層の強度を向上させる作用があることはすでによく知られているが、これに加えて、この発明の改質Ｔｉ1-ｘＳｉｘＮ層は高速断続切削加工条件という厳しい使用条件下でも、すぐれた靭性と耐欠損性を発揮する。
そしてその理由は以下に述べるように、改質Ｔｉ1-ｘＳｉｘＮ層の特異な結晶粒形態と強い関連性を有する。
As already described, the present invention comprises, for example, a WC-based cemented carbide sintered body in an apparatus using an ion plating apparatus using a pressure gradient type Ar plasma gas shown schematically in FIG. Install the tool base,
Tool substrate temperature: 240-400 ° C.
Evaporation source: Metal Ti, Metal Si
Plasma gun discharge power For metal Ti: 10-12 kW,
Plasma gun discharge power For metal Si: 5 to 8 kW,
Reaction gas flow rate: nitrogen (N 2) gas 80 to 120 sccm,
Discharge gas: Argon (Ar) gas 30-50 sccm,
DC bias voltage applied to the tool base: 0 V,
Deposition rate: 0.04-0.11 nm / second,
The film is formed under the conditions. It is already well known that the Ti component, which is a conventional component of the Ti 1-x Si x N layer, improves the high-temperature strength, the Si component improves the heat resistance, and N has the effect of improving the layer strength. In addition to this, the modified Ti 1-x Si x N layer of the present invention exhibits excellent toughness and fracture resistance even under severe use conditions such as high-speed interrupted cutting conditions.
The reason for this is strongly related to the unique grain morphology of the modified Ti 1-x Si x N layer, as will be described below.
まず、上記蒸着で形成された改質Ｔｉ1-ｘＳｉｘＮ層について、表面を研磨面とした状態で、電子線後方散乱回折装置を用いて前記硬質被覆層のＴｉ1-ｘＳｉｘＮ層表面の水平断面の結晶方位を解析したところ、隣り合う測定点間での結晶方位の方位差が、特定軸周りでの回転角度（以下、回転角度という）で１５度以上となる結晶粒界によって囲まれたドメイン径０２〜４μｍのドメインの占有する面積が、測定された面積の２０％以上を占有することがわかった。
なお、前記方位差を記述する上での回転角度とは、向きの異なる２つの結晶の一方に対して、１回の回転操作で２つの結晶が完全に同じ向きとなる場合の回転角度を指し、
また、ここでいうドメイン径とは、そのドメイン領域と同じ面積をもつ真円の直径を指す。
First, with respect to the modified Ti 1-x Si x N layer formed by the above vapor deposition, the hard coating layer Ti 1-x Si x N is formed using an electron beam backscattering diffractometer in a state where the surface is a polished surface. When the crystal orientation of the horizontal cross section of the layer surface is analyzed, the crystal grain boundary where the orientation difference in crystal orientation between adjacent measurement points is 15 degrees or more around a specific axis (hereinafter referred to as the rotation angle). It was found that the area occupied by the domain having a domain diameter of 02 to 4 μm surrounded by occupies 20% or more of the measured area.
Note that the rotation angle in describing the difference in orientation refers to the rotation angle when two crystals have the same orientation in one rotation operation with respect to one of two crystals having different orientations. ,
The domain diameter here refers to the diameter of a perfect circle having the same area as the domain region.
さらに、膜の表面から０．１μｍの深さの水平断面の結晶組織を、透過型電子顕微鏡を用いて観察し個々の結晶粒径を測定したところ、直径１０〜１００ｎｍの結晶粒が全測定面積のうち面積割合で９０％以上を占めることがわかった。
なお、ここでいう直径とは、その結晶粒と同じ面積をもつ真円の直径を指す。
Furthermore, when the crystal structure of a horizontal cross section having a depth of 0.1 μm from the surface of the film was observed using a transmission electron microscope and the individual crystal grain sizes were measured, the crystal grains having a diameter of 10 to 100 nm were found to have a total measurement area. It was found that the area ratio accounted for 90% or more.
Here, the diameter refers to the diameter of a perfect circle having the same area as the crystal grain.
この特性について、以下に詳細に説明する。 This characteristic will be described in detail below.
上記、面積割合で９０％以上の直径１０〜１００ｎｍの結晶粒によって構成されており、かつ、ドメイン内部で隣り合う結晶方位の角度差が１５度未満となるようなドメイン径０．２〜４μｍのドメインが面積割合で２０％以上存在する前記改質Ｔｉ1-ｘＳｉｘＮ層においては、前記ドメインの内部を構成する結晶粒は少なくとも面積割合で５０％以上の直径１０〜１００ｎｍの結晶粒によって構成されている。
したがって、面積割合で前記ドメイン内に存在する少なくとも５０％以上の結晶粒は近傍に存在する結晶粒、特に同一のドメイン内に存在する結晶粒と、結晶方位の差が回転角度で１５度未満となるような二軸配向性を示していることから、前記ドメイン内に存在する結晶粒同士の界面整合性が高く、あたかも単結晶のような優れた靭性を具備するとともに、さらに、直径１０〜１００ｎｍという微細組織をもち優れた耐欠損性を維持できることから、皮膜中に亀裂や欠損が生じやすい断続重切削加工においても、工具の長寿命化がはかられるものである。
The domain diameter is 0.2 to 4 μm, which is composed of crystal grains having a diameter of 10 to 100 nm with an area ratio of 90% or more, and an angle difference between adjacent crystal orientations within the domain is less than 15 degrees. In the modified Ti 1-x Si x N layer in which the domain is present in an area ratio of 20% or more, the crystal grains constituting the inside of the domain are at least 50% or more of the crystal grains having a diameter of 10 to 100 nm in the area ratio. It is configured.
Accordingly, at least 50% or more of the crystal grains existing in the domain in terms of area ratio are close to the crystal grains, particularly the crystal grains existing in the same domain, and the difference in crystal orientation is less than 15 degrees in rotation angle. Since it exhibits such biaxial orientation, the interfacial consistency between the crystal grains existing in the domain is high, and it has excellent toughness like a single crystal, and further has a diameter of 10 to 100 nm. Since it has a fine structure and can maintain excellent fracture resistance, the tool life can be extended even in intermittent heavy cutting, in which cracks and fractures tend to occur in the coating.
上記の改質Ｔｉ1-ｘＳｉｘＮ層について、ｘの値が０．０５未満であるとＳｉの割合が相対的に少なくなり、Ｓｉが持つ耐熱特性効果が十分に得られず、０．３を超えるとＴｉの割合が相対的に少なくなり過ぎ、所望の高温強度が得られないため、ｘの値を０．０５≦ｘ≦０．３と定めた。
また、結晶粒の大きさが１０ｎｍ未満であると、結晶粒自体の強度が得られず所望の強度を得られなくなり、また１００ｎｍを超えると結晶粒が粗大になりチッピングの原因となることから、面積割合で皮膜の９０％以上を占める結晶粒の大きさを１０ｎｍ〜１００ｎｍと定めた。
また、Ｔｉ1-ｘＳｉｘＮ層を構成する、結晶方位が１５度以上の界面で囲まれるドメインの面積割合が２０％未満では、所望の靭性を得ることが出来ないため、該ドメインの面積割合を２０％以上と定めた。
In the above modified Ti 1-x Si x N layer, when the value of x is less than 0.05, the proportion of Si is relatively reduced, and the heat resistance characteristic effect of Si cannot be sufficiently obtained. If it exceeds 3, the ratio of Ti becomes relatively small, and the desired high-temperature strength cannot be obtained. Therefore, the value of x was set to 0.05 ≦ x ≦ 0.3.
Also, if the size of the crystal grains is less than 10 nm, the strength of the crystal grains themselves cannot be obtained and the desired strength cannot be obtained, and if it exceeds 100 nm, the crystal grains become coarse and cause chipping. The size of crystal grains occupying 90% or more of the film in terms of area ratio was determined as 10 nm to 100 nm.
Further, if the area ratio of the domain constituting the Ti 1-x Si x N layer and surrounded by the interface having a crystal orientation of 15 degrees or more is less than 20%, the desired toughness cannot be obtained. The ratio was set to 20% or more.
この発明の被覆工具は、Ｔｉ1-ｘＳｉｘＮ層からなる硬質被覆層を構成するＴｉ1-ｘＳｉｘＮ結晶粒のうち、粒径が１０〜１００ｎｍの結晶粒が面積割合で全体の９０％以上を占有し、かつ、電子線後方散乱回折装置で表面の結晶粒の結晶方位を測定した場合、隣り合う測定点との結晶方位の差が１５度以上となる結晶界面によって囲まれた直径０．２〜４μｍの区分が、測定された全体の面積のうち２０％以上を占有するため、切刃に対して高い負荷がかかる乾式断続高速切削加工においても、優れた高温強度、耐熱性に加えて、優れた耐欠損性と靭性を示し、すぐれた工具特性を発揮し、工具寿命の延命化に寄与するものである。 Coated tool of the present invention, among the Ti 1-x Si x N crystal grains constituting the hard coating layer comprising Ti 1-x Si x N layer, a particle size of 10~100nm crystal grains in total area ratio When the crystal orientation of the crystal grains on the surface occupies 90% or more and is measured with an electron beam backscattering diffractometer, the difference between crystal orientations between adjacent measurement points is 15 degrees or more. The section with a diameter of 0.2 to 4 μm occupies 20% or more of the total area measured, and therefore excellent high-temperature strength and heat resistance even in dry intermittent high-speed cutting that places a high load on the cutting edge. In addition, it exhibits excellent fracture resistance and toughness, exhibits excellent tool characteristics, and contributes to prolonging the tool life.
つぎに、この発明の被覆工具を実施例により具体的に説明する。
なお、ここでは被覆インサートを中心にして説明するが、被覆インサートに限らず、被覆エンドミルや被覆ドリル等の各種の被覆工具に適用できるものである。
Next, the coated tool of the present invention will be specifically described with reference to examples.
In addition, although demonstrated centering on a covering insert here, it is applicable not only to a covering insert but to various covering tools, such as a covering end mill and a covering drill.
原料粉末として、いずれも０．８〜４μｍの平均粒径を有するＷＣ粉末、ＴｉＣ粉末、ＶＣ粉末、ＮｂＣ粉末、Ｃｒ3 Ｃ2 粉末、およびＣｏ粉末を用意し、これら原料粉末を、表１に示される配合組成に配合し、ボールミルで７２時間湿式混合し、乾燥した後、１００ＭＰａ の圧力で圧粉体にプレス成形し、この圧粉体を６Ｐａの真空中、温度：１４００℃に１時間保持の条件で焼結し、焼結後、表面を研磨し、ＩＳＯ規格・ＳＥＥＮ１２０３のインサート形状をもったＷＣ基超硬合金製のフライス加工用工具基体Ａ１〜Ａ１０を形成した。 As raw material powders, WC powder, TiC powder, VC powder, NbC powder, Cr 3 C 2 powder, and Co powder all having an average particle diameter of 0.8 to 4 μm are prepared. Blended into the composition shown, wet mixed with a ball mill for 72 hours, dried, and then pressed into a green compact at a pressure of 100 MPa. The green compact was held at a temperature of 1400 ° C. for 1 hour in a vacuum of 6 Pa. After sintering, the surface was polished, and tool bases A1 to A10 for milling made of WC-base cemented carbide having an ISO standard / SEEN1203 insert shape were formed.
ついで、上記の工具基体Ａ１〜Ａ１０およびＢ１〜Ｂ１０を、アセトン中で超音波洗浄し、乾燥した状態で、図１に示される圧力勾配型Ａｒプラズマガンを利用したイオンプレーティング装置に装着し、蒸発源として、金属Ｔｉを装着し、まず、装置内を排気して１．０×１０−３Ｐａ以下の真空に保持しながらヒーターで装置内を２４０〜４２０℃に加熱した後、Ａｒガスを導入して２．３×１０−２Ｐａとしたのち、圧力勾配型プラズマガンの放電電力を２ｋＷとし、装置内にＡｒイオンを発生させ、工具基体に−２００Ｖのバイアス電圧を印加することによって、前記工具基体を１０分間Ａｒボンバード処理し、ついで、装置内を一旦１×１０−３Ｐａ程度の真空にした後、
表２に示す条件で、圧力勾配型Ａｒプラズマガンの放電電力を１２ｋＷとし、Ａｒガスを６０ｓｃｃｍ，窒素ガスを１００ｓｃｃｍ流しながら、炉内の圧力を３×１０−２〜６×１０−２Ｐａに保ち、金属Ｔｉ蒸発源および金属Ｓｉ蒸発源にプラズマビームを入射し金属Ｔｉおよび金属Ｓｉの蒸気を発生させるとともにプラズマビームでイオン化し、かつ、チャンバー内での改質Ｔｉ1-ｘＳｉｘＮ層の成長速度を、水晶発振式膜厚コントローラを用いて測定しながら、前記成長速度が目的の速度（０．０４〜０．１１ｎｍ／ｓｅｃ）から±０．０１ｎｍ／ｓｅｃの範囲となるようプラズマガンの出力を調整しながら、工具基体表面に、表４に示される所定目標層厚の改質Ｔｉ1-ｘＳｉｘＮ層を蒸着形成させ、本発明被覆工具としての本発明被覆インサート（以下、本発明インサートという）１〜１４を製造した。
なお、表２に、本発明インサート１〜１４の改質Ｔｉ1-ｘＳｉｘＮ層の形成条件である圧力勾配型Ａｒプラズマガンを利用したイオンプレーティングの各種条件を示す。
Next, the tool bases A1 to A10 and B1 to B10 are ultrasonically cleaned in acetone and dried, and attached to an ion plating apparatus using a pressure gradient type Ar plasma gun shown in FIG. As the evaporation source, metal Ti was attached. First, the inside of the apparatus was evacuated and the inside of the apparatus was heated to 240 to 420 ° C. with a heater while maintaining a vacuum of 1.0 × 10 −3 Pa or less. After being introduced to 2.3 × 10 −2 Pa, the discharge power of the pressure gradient plasma gun is set to 2 kW, Ar ions are generated in the apparatus, and a bias voltage of −200 V is applied to the tool base, The tool base was treated with Ar bombardment for 10 minutes, and then the inside of the apparatus was once evacuated to about 1 × 10 −3 Pa,
Under the conditions shown in Table 2, the discharge power of the pressure gradient type Ar plasma gun is 12 kW, the pressure in the furnace is 3 × 10 −2 to 6 × 10 −2 Pa while flowing Ar gas at 60 sccm and nitrogen gas at 100 sccm. A plasma beam is incident on the metal Ti evaporation source and the metal Si evaporation source to generate vapors of metal Ti and metal Si, ionize with the plasma beam, and the modified Ti 1-x Si x N layer in the chamber The plasma gun is measured so that the growth rate is within a range of ± 0.01 nm / sec from the target rate (0.04 to 0.11 nm / sec) while measuring the growth rate using a crystal oscillation type film thickness controller. The modified Ti 1-x Si x N layer having a predetermined target layer thickness shown in Table 4 is vapor-deposited on the surface of the tool base while adjusting the output of the tool. Light coated inserts (hereinafter referred to as the present invention inserts) 1 to 14 were produced.
Table 2 shows various conditions for ion plating using a pressure gradient type Ar plasma gun, which are conditions for forming the modified Ti 1-x Si x N layers of the
比較の目的で、上記の工具基体Ａ１〜Ａ１０を、アセトン中で超音波洗浄し、乾燥した状態で、図２に示されるスパッタリング（ＳＰ）装置に装着し、カソード電極（蒸発源）として金属ＣｒおよびＴｉ-Ｓｉ合金を装着し、まず、装置内を排気して０．０１Ｐａ以下の真空に保持しながらヒーターで装置内を４００℃に加熱した後、Ａｒガスを２００ｓｃｃｍ導入し、金属Ｃｒと前記工具基体との間に−８００Ｖの直流バイアス電圧を印加し、前記工具基体表面を５分間Ｃｒボンバード処理し、ついで、表３に示す条件で、装置内に雰囲気ガスとして窒素ガスおよびＡｒガスを導入して０．５Ｐａの雰囲気とするとともに、前記金属Ｔｉと前記工具基体との間にバイアス電圧として−５０Ｖの直流バイアス電圧を印加し、もって前記工具基体の表面に、表６に示される目標層厚の従来Ｔｉ1-ｘＳｉｘＮ層を硬質被覆層として蒸着形成することにより、従来被覆工具としての従来表面被覆インサート（以下、従来インサートという）１〜１４を製造した。
なお、表３には、従来インサート１〜１４の従来Ｔｉ1-ｘＳｉｘＮ層の形成されるスパッタリング条件を示す。
For the purpose of comparison, the above tool bases A1 to A10 are ultrasonically cleaned in acetone and dried, and then mounted on the sputtering (SP) apparatus shown in FIG. 2, and metal Cr is used as a cathode electrode (evaporation source). And the Ti—Si alloy, first, the inside of the apparatus is evacuated and the inside of the apparatus is heated to 400 ° C. with a heater while maintaining a vacuum of 0.01 Pa or less, Ar gas is introduced at 200 sccm, and the metal Cr and the aforementioned A DC bias voltage of −800 V is applied between the tool substrate and the surface of the tool substrate is subjected to Cr bombardment for 5 minutes, and then nitrogen gas and Ar gas are introduced into the apparatus as atmospheric gases under the conditions shown in Table 3. And an atmosphere of 0.5 Pa, and a DC bias voltage of −50 V is applied as a bias voltage between the metal Ti and the tool base, thereby the tool base. A conventional surface-coated insert (hereinafter referred to as a conventional insert) 1 as a conventional coated tool is formed by vapor-depositing a conventional Ti 1-x Si x N layer having a target layer thickness shown in Table 6 as a hard coating layer on the surface of ~ 14 were produced.
Table 3 shows sputtering conditions for forming the conventional Ti 1-x Si x N layers of the
本発明インサート１〜１０の改質Ｔｉ1-ｘＳｉｘＮ層および従来インサート１〜１０の従来Ｔｉ1-ｘＳｉｘＮ層について、その表面を研磨面とした状態で、電子線後方散乱回折装置（ＥＢＳＤ）を用いて硬質被覆層表面の結晶方位を解析した。すなわち、１０μｍ×１０μｍの領域を０．０３μｍ/ｓｔｅｐの間隔で、前記改質Ｔｉ1-ｘＳｉｘＮ層がもつ結晶方位を測定し、測定ノイズを除去したのち、隣り合う測定点間の結晶方位の差が回転角度で１５度以上となる界面を図３（ｂ）に例示されるように測定領域のマップ上に表示し、それらの界面によって区分される領域（以下、ドメインという）のうち、０．２〜４μｍのドメイン径を有する全測定面積に対する面積割合を求め、この値を、ドメイン径の平均値とともに表４および表５に示した。
さらに、前記硬質被覆層を基板側から約１ｍｍの厚さまで機械研磨したのち、Ａｒイオン研磨装置を用いて厚さ１００ｎｍとなるまで研磨し薄片とした状態で、透過型電子顕微鏡を用いて層の表面から１００ｎｍの深さ近傍におけるＴｉ1-ｘＳｉｘＮ層の結晶粒径を観察し、図３（ａ）に例示されるように改質Ｔｉ1-ｘＳｉｘＮ層の工具基体表面のうち、幅１０〜１００ｎｍの微細粒が占有する面積割合αを求め、ドメインの全測定面積に対する面積割合とともに表４および表５に示した。
表４から、本発明インサート１〜１４の改質Ｔｉ1-ｘＳｉｘＮ層は、直径１０〜１００ｎｍのＴｉ1-ｘＳｉｘＮ結晶粒が面積割合で９０％を占め、かつ、電子線後方散乱回折装置で結晶方位を解析したときに、回転角度で１５度以上の結晶方位の差をもつ界面によって囲まれるドメイン径０．２〜４μｍのドメインの面積割合が、全測定面積の２０％以上となっており、二軸配向性を有する１０〜１００ｎｍの微細結晶によって構成されているドメインが面積割合で２０％以上存在ことが分かる。
一方、表５から、従来インサート１〜１４の従来Ｔｉ1-ｘＳｉｘＮ層は、回転角度で１５度以上の結晶方位の差をもつ界面によって区分されるドメイン径０．２〜４μｍのドメインの面積割合が全測定面積の２０％以上となるものの、１０〜１００ｎｍの微細結晶の存在割合は面積割合で９０％以下となっており、表面組織は直径１００ｎｍ以上の粗大粒によって構成されている。すなわち、二軸配向性を有する１０〜１００ｎｍの微細結晶によって構成されるドメインは全く存在せず、１００ｎｍ以上の粗大な単結晶によってのみ構成されていることが分かる。
A conventional Ti 1-x Si x N layer of the reforming Ti 1-x Si x N layer and a conventional insert 10 of the present invention the insert 10, while the surface and the polishing surface, electron backscatter diffraction The crystal orientation of the hard coating layer surface was analyzed using an apparatus (EBSD). That is, the crystal orientation of the modified Ti 1-x Si x N layer is measured in a 10 μm × 10 μm region at an interval of 0.03 μm / step, measurement noise is removed, and then the crystal between adjacent measurement points is measured. An interface whose azimuth difference is 15 degrees or more in the rotation angle is displayed on the measurement area map as illustrated in FIG. 3B, and among the areas (hereinafter referred to as domains) divided by these interfaces. The area ratio with respect to the total measurement area having a domain diameter of 0.2 to 4 μm was obtained, and this value is shown in Table 4 and Table 5 together with the average value of the domain diameter.
Further, after mechanically polishing the hard coating layer from the substrate side to a thickness of about 1 mm, using an Ar ion polishing apparatus, the hard coating layer was polished to a thickness of 100 nm to form a thin piece, and then the layer was formed using a transmission electron microscope. The crystal grain size of the Ti 1-x Si x N layer in the vicinity of a depth of 100 nm from the surface is observed, and the surface of the tool base surface of the modified Ti 1-x Si x N layer is exemplified as shown in FIG. Among these, the area ratio α occupied by fine grains having a width of 10 to 100 nm was obtained and shown in Tables 4 and 5 together with the area ratio with respect to the total measurement area of the domain.
From Table 4, the modified Ti 1-x Si x N layers of the
On the other hand, from Table 5, the conventional Ti 1-x Si x N layers of the
つぎに、上記本発明インサート１〜１０及び従来インサート１〜１０について、これを工具鋼製バイトの先端部に固定治具にてネジ止めした状態で、
被削材：平面寸法 １００ｍｍ×２５０ｍｍ 厚さ５０ｍｍの ＪＩＳ規格・ＳＵＳ３１６の板材
切削速度： ２００ ｍ／ｍｉｎ．、
切り込み： ３ ｍｍ、
１刃あたりのテーブル送り： ０．３ ｍｍ／刃、
切削時間： ２ 分、
の条件（切削条件１という）でのステンレス鋼の乾式高速フライス加工試験（通常の切削速度及びテーブル送りは、それぞれ、１５０ｍ／ｍｉｎ、０．２ｍｍ／ｒｅｖ．）、
被削材：平面寸法 １００ｍｍ×２５０ｍｍ 厚さ５０ｍｍの ＪＩＳ・ＳＣＭ４４０の板材
切削速度： ２５０ ｍ／ｍｉｎ．、
切り込み： ３ ｍｍ、
１刃あたりのテーブル送り： ０．３ ｍｍ／刃、
切削時間： ２ 分、
の条件（切削条件２という）での合金鋼の乾式高速フライス加工試験（通常の切削速度及びテーブル送りは、それぞれ、１６０ｍ／ｍｉｎ、０．２ｍｍ／ｒｅｖ．）、
を行い、いずれの切削加工試験でも切刃の逃げ面摩耗幅を測定した。
この測定結果を表６に示した。
Next, for the above-mentioned
Work material: Plane dimension 100 mm x 250 mm Thickness 50 mm JIS standard / SUS316 plate material Cutting speed: 200 m / min. ,
Cutting depth: 3 mm,
Table feed per blade: 0.3 mm / tooth,
Cutting time: 2 minutes,
Stainless steel dry high-speed milling test under the following conditions (referred to as cutting condition 1) (normal cutting speed and table feed are 150 m / min and 0.2 mm / rev., Respectively),
Work material: Plane size 100 mm × 250 mm JIS / SCM440 plate material with a thickness of 50 mm Cutting speed: 250 m / min. ,
Cutting depth: 3 mm,
Table feed per blade: 0.3 mm / tooth,
Cutting time: 2 minutes,
Dry high-speed milling test of alloy steel under the following conditions (referred to as cutting condition 2) (normal cutting speed and table feed are 160 m / min and 0.2 mm / rev., Respectively),
In each cutting test, the flank wear width of the cutting edge was measured.
The measurement results are shown in Table 6.
表４、表６から、本発明インサート１〜１４は、粒径が１０〜１００ｎｍの結晶粒が測定面積のうち９０％以上を占有し、かつ、電子線後方散乱回折装置で表面の結晶粒の結晶方位を測定した場合、隣り合う測定点との結晶方位の差が１５度以上の回転角度となる結晶界面によって囲まれた直径０．２〜４μｍのドメインが、測定された全体の面積のうち２０％以上を占めており、すなわち、強く配向した１０〜１００ｎｍの結晶粒によって構成される０．２〜４μｍのドメインが多く存在することにより、すぐれた耐欠損性と靭性を発揮し、乾式断続高速切削加工条件においても優れた工具寿命を実現していることが分かる。
これに対して、表５、表６から、従来インサート１〜１４においては、従来Ｔｉ1-ｘＳｉｘＮ層は、１０〜１００ｎｍの結晶粒の占める面積割合が小さく、粗大な単結晶粒子のみが存在することから、耐欠損性と靭性に劣り、乾式断続高速切削加工条件ではチッピングや欠損等により、比較的短時間で使用寿命に至ることが明らかである。
From Tables 4 and 6, according to the
On the other hand, from Tables 5 and 6, in the
上述のように、この発明の被覆工具は、硬質被覆層（改質Ｔｉ1-ｘＳｉｘＮ層）がすぐれた耐欠損性、靭性を有することから、被覆インサートばかりでなく、被覆エンドミル、被覆ドリル等の各種被覆工具として用いることができ、そして、これによって、靭性不足、強度不足等に起因する工具欠損の発生を防止し、長期の使用に亘って優れた切削性能を発揮するものであるから、低コスト化に十分満足に対応できるとともに、工具寿命の延命化を図ることができるものである。 As described above, the coated tool according to the present invention has a hard coating layer (modified Ti 1-x Si x N layer) having excellent fracture resistance and toughness. It can be used as various types of coated tools such as drills, and thereby prevents the occurrence of tool defects due to insufficient toughness, insufficient strength, etc., and exhibits excellent cutting performance over a long period of use. Therefore, it is possible to sufficiently satisfy the cost reduction and prolong the tool life.
Claims (1)
上記Ｔｉ1-ｘＳｉｘＮ層は上記平均層厚と等しい高さを有する柱状晶組織からなり、さらに、電子線後方散乱回折装置で表面の結晶粒の結晶方位を測定した場合、隣り合う測定点との結晶方位の差が１５度以上となる結晶界面によって囲まれた直径０．２〜４μｍの区分が、測定された全体の面積のうち２０％以上を占有し、かつ、上記Ｔｉ1-ｘＳｉｘＮ層の表面から１００ｎｍの深さの水平断面における結晶粒組織を観察した場合、粒径が１０〜１００ｎｍの結晶粒が測定面積のうち９０％以上を占有することを特徴とする表面被覆切削工具。 In a surface-coated cutting tool in which a hard coating layer made of a Ti 1-x Si x N film having an average layer thickness of 0.2 to 2 μm is physically vapor-deposited on the surface of a tool base made of a tungsten carbide-based cemented carbide sintered body , X satisfies 0.05 ≦ x ≦ 0.3, and
The Ti 1-x Si x N layer has a columnar crystal structure having a height equal to the average layer thickness, and when the crystal orientation of the surface crystal grains is measured with an electron beam backscattering diffractometer, adjacent measurements are performed. A section having a diameter of 0.2 to 4 μm surrounded by a crystal interface where the difference in crystal orientation with respect to a point is 15 degrees or more occupies 20% or more of the total area measured, and the Ti 1− A surface characterized in that when a crystal grain structure in a horizontal cross section having a depth of 100 nm is observed from the surface of the x Si x N layer, crystal grains having a grain size of 10 to 100 nm occupy 90% or more of the measurement area Coated cutting tool.
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| JPH11256336A (en) * | 1998-03-10 | 1999-09-21 | Hitachi Metals Ltd | Titanium carbonitride-coated tool |
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| WO2005089990A1 (en) * | 2004-03-18 | 2005-09-29 | Sumitomo Electric Hardmetal Corp. | Surface-coated cutting tool |
| JP2009214196A (en) * | 2008-03-07 | 2009-09-24 | Mitsubishi Materials Corp | Surface-coated cutting tool having hard coating layer exhibiting excellent resistance to defect |
| JP2009220239A (en) * | 2008-03-18 | 2009-10-01 | Mitsubishi Materials Corp | Surface coated cutting tool having hard coating layer exerting superior chipping resistance |
| JP2011121145A (en) * | 2009-12-11 | 2011-06-23 | Mitsubishi Materials Corp | Surface-coated cutting tool having hard coating layer exhibiting superior chipping resistance |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11256336A (en) * | 1998-03-10 | 1999-09-21 | Hitachi Metals Ltd | Titanium carbonitride-coated tool |
| JP2003117706A (en) * | 2001-10-04 | 2003-04-23 | Hitachi Tool Engineering Ltd | Covered tool |
| JP2005212047A (en) * | 2004-01-29 | 2005-08-11 | Kyocera Corp | Surface-coated member and cutting tool |
| WO2005089990A1 (en) * | 2004-03-18 | 2005-09-29 | Sumitomo Electric Hardmetal Corp. | Surface-coated cutting tool |
| JP2009214196A (en) * | 2008-03-07 | 2009-09-24 | Mitsubishi Materials Corp | Surface-coated cutting tool having hard coating layer exhibiting excellent resistance to defect |
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