CN101209611A - 多层涂覆切削刀具 - Google Patents
多层涂覆切削刀具 Download PDFInfo
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- CN101209611A CN101209611A CNA2007101605961A CN200710160596A CN101209611A CN 101209611 A CN101209611 A CN 101209611A CN A2007101605961 A CNA2007101605961 A CN A2007101605961A CN 200710160596 A CN200710160596 A CN 200710160596A CN 101209611 A CN101209611 A CN 101209611A
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- 238000005520 cutting process Methods 0.000 title claims abstract description 36
- 238000000576 coating method Methods 0.000 claims abstract description 69
- 239000011248 coating agent Substances 0.000 claims abstract description 60
- 239000000203 mixture Substances 0.000 claims abstract description 31
- 239000000758 substrate Substances 0.000 claims abstract description 22
- 239000000126 substance Substances 0.000 claims abstract description 10
- 238000010276 construction Methods 0.000 claims description 49
- 239000010410 layer Substances 0.000 claims description 40
- 229910052719 titanium Inorganic materials 0.000 claims description 21
- 229910052782 aluminium Inorganic materials 0.000 claims description 18
- 229910052710 silicon Inorganic materials 0.000 claims description 16
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 12
- 150000004767 nitrides Chemical class 0.000 claims description 11
- 229910052804 chromium Inorganic materials 0.000 claims description 8
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- 229910052582 BN Inorganic materials 0.000 claims description 5
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 5
- 239000011195 cermet Substances 0.000 claims description 5
- 150000001247 metal acetylides Chemical class 0.000 claims description 4
- 230000009970 fire resistant effect Effects 0.000 claims description 2
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
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- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 3
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- 229910000831 Steel Inorganic materials 0.000 description 2
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 2
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- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
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- 238000010884 ion-beam technique Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- VSZWPYCFIRKVQL-UHFFFAOYSA-N selanylidenegallium;selenium Chemical compound [Se].[Se]=[Ga].[Se]=[Ga] VSZWPYCFIRKVQL-UHFFFAOYSA-N 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及一种涂覆切削刀具,其中基底涂覆有薄、粘附、硬且耐磨的涂层,该涂层包括薄片状多层结构,所述多层结构为金属氮化物、金属碳化物或金属碳氮化物的交替层。在所述涂层中,贯穿整个多层结构,单层厚度的次序没有重复周期,基本上是无周期的。所述涂层的平均化学组成为:AlaTibSicCrd(CeN1-e),其中0<a<0.5,优选0.05<a<0.4,其中0.1<b<0.9,优选0.3<b<0.9,其中0.01<c<0.17,优选0.02<c<0.1,其中0≤d<0.06,并且a+b+c+d=1,其中0≤e<1,优选0≤e<0.2。
Description
本发明涉及一种用于金属加工的切削刀具,包括:硬质合金、金属陶瓷、陶瓷、高速钢或立方硼氮化物的基底,以及在所述基底的表面上,通过物理气相沉积(PVD)沉积的坚硬且抗磨耐火涂层。该涂层粘着地结合到基底上,并且该涂层包括有薄片状多层结构,该多层结构为交替的作为单层的金属氮化物、金属碳化物或者金属碳氮化物,所述多层结构具有无周期结构并且平均Si含量为1-17at%。
将诸如氧化铝(Al2O3)、碳化钛(TiC)和/或氮化钛(TiN)的材料的薄耐火涂层(1-20μm)沉积到例如由硬质合金、金属陶瓷、陶瓷、高速钢或立方硼氮化物制成的切削刀具上的方法,是已确立的技术,并且当将刀片使用在金属加工时,这种涂覆切削刀具的使用寿命会显著地延长。在某些条件下,刀具所延长的使用寿命能提高几个百分点。现今的商用切削刀具的特征在于由双层或多层结构结合而成多层体。总涂层厚度在1-20微米(μm)之间变化,并且在现有技术中,多层结构的特征在于,其在纳米(nm)和/或微米(μm)范围内,即单层厚度在几微米和几百纳米之间变化。
存在多种能够在切削刀具上生成耐火薄层的PVD技术,并且最确立的方法是:离子镀、磁控溅射、电弧放电蒸发以及IBAD(离子束辅助沉积)。每种方法都具有自己的优点,并且所生成涂层的固有特性如微观结构/粒度、硬度、应力状态、对下基底的结合力和粘附力,会根据所选择的特定PVD方法而变化。通过优化一个或多个上述特性,能够提高PVD涂覆切削刀具的耐磨性和刀刃完整性,其中所述刀具被应用在特定的加工操作中。
对于纳米复合氮化物、碳化物或碳氮化物的硬质涂层材料,可以理解的是,在多层涂层中,每个单独的氮化物、碳化物或碳氮化物层的厚度在纳米范围内,通常在100nm之下。
近年来,刀具朝着更锋利切削刃的方向发展。这需要较薄的涂层,以保持锋利的切削刃。如果涂层太厚,刀刃就会容易形成较圆形状。如果沉积较薄的涂层,那么需要增加硬度以保持耐磨性。获得薄且硬的涂层的一种方法是使用多层纳米复合涂层。在现有技术中,这种纳米复合涂层通常被沉积到均质耐磨层上。
EP 1 690 959 A公开了一种耐磨涂层,其包括厚度为2-6μm的TiAlSiN的单相结构底层以及总厚度为0.5-1.5μm的Ti1-(A+B)AlASiBN/Ti1-(C+D)AlCSiDN的多层结构顶层。多层结构的组成为:A在0.01-0.06范围内,B在0.25-0.35范围内,C在0.30-0.45范围内,D在0.1-0.15范围内。
EP 1 702 997 A公开了一种用于切削刀具的硬质膜,其由以下组成:Ti1-a-b-c-dAlaCrbSicBd(C1-eNe),其中0.5<a<0.8,b>0.06,c为0-0.1,0<d<0.1并且0.5<e<1。硬质膜可以是多层结构的形式。
然而,仍然需要多层涂层的进一步发展,从而能提供具有改善的耐磨性同时仍具有锋利切削刃的涂层。
本发明的一个目的是提供具有耐磨涂层的切削刀具。
本发明的另一个目的是提供具有提高的硬度的涂层。
本发明的另一个目的是提供适用于锋利刀刃的涂层。
已经令人惊奇地发现,通过提供根据本发明的涂层,提高的硬度导致切削刃耐磨料磨损性增强,从而可以保持锋利的切削刃。还发现,即使没有现有技术描述的均质底层,也能获得硬且薄的涂层。所获得的结构为细晶结构,同时在晶粒边界处没有空隙或具有非常少量孔隙。高倍截面透射电子显微镜(TEM)显示了无周期的结构。
图1示出了根据本发明多层氮化物结构的TEM照片。贯穿整个多层结构,单层厚度的次序基本上是无周期的。
图2示出了基底1的示意性照片。所述基底1涂覆有薄片状多层氮化物涂层2,所述涂层2具有单个金属氮化物层X和Y,以及例式性的单层厚度3。
根据本发明,提供了一种切削刀具,其包括硬质合金、金属陶瓷、陶瓷、立方硼氮化物或高速钢的基底,在所述基底上沉积有耐磨的多层涂层。所述基底还预先涂覆有厚度为0.1-1μm的薄的单层或多层TiN、TiC、TiCN或者(Ti,Al)N,所述厚度优选为0.05-0.5μm。
粘着地结合到基底或者预涂覆基底上的所述多层涂层,包括薄片状多层结构,X+Y+X+Y+…(参见图1和2),其中交替层X和Y包括金属氮化物、金属碳化物或者金属碳氮化物,优选多晶氮化物,优选具有立方结构,同时所述金属元素选自钛(Ti)、铝(Al)、硅(Si)、铬(Cr)、铌(Nb)、铪(Hf)、钒(V)、钽(Ta)、钼(Mo)、锆(Zr)或钨(W)以及它们的混合物。层X的化学组成与层Y的化学组成不同。
由于多层结构中各单层的厚度很小,因此如果不借助相邻层的话,将无法测量各单层的组成。能够被测量的是整个多层结构的平均组成。然而,各单层的组成可通过所使用的靶的组成而被确定,但是这无法给出精确的组成。当较厚层被沉积后,并且厚到足以能够被分析,那么可以看到的是,沉积层的组成与靶材料的组成相差一些百分点。由此,本文所提到的根据本发明多层结构的单层的任意组成是通过沉积期间所使用的靶的组成来估计的。
在涂层的截面上使用EDS(能量色散谱仪)来测量多层结构中的平均化学组成。根据本发明的整个多层结构的平均组成优选为:AlaTibSicCrd(CeN1-e),其中0<a<0.5,优选0.05<a<0.4,其中0.1<b<0.9,优选0.3<b<0.9,其中0.01<c<0.17,优选0.02<c<0.1,其中0≤d<0.06,并且a+b+c+d=1,其中0≤e<1,优选0≤e<0.2。每个层的组成,即靶的组成,可以在上述界限之外,即便整个多层结构的平均组成在界限之内。
多层结构具有单独厚度的交替X和Y层的次序,所述次序在基本上贯穿整个多层结构中是无周期的。任意单层的厚度大于0.1nm,但小于100nm,优选大于1nm而小于50nm,最优选大于2nm而小于30nm。多层结构中任意十个连续层的总和小于300nm。
“无周期”可理解为:多层结构中,特定单层的厚度不取决于紧接其下面的单层的厚度,同时与其上面的单层也没有任何关系。因此,多层结构在单层厚度次序中不具有任何循环周期。多层结构的总厚度为0.5-20μm,优选1-10μm,最优选1-5μm。
在本发明的一个实施方式中,涂层包括至少两个、优选至少五个多层结构,所述多层结构反复地与均质层交替。该多层结构中关于单层厚度与化学组成与上面描述的相同。均质层优选包括TixAlySiz(CwN1-w),其中0<x<0.7,优选0.05<x<0.6,其中0.1<y<0.9,优选0.3<y<0.9,其中0.01<z<0.17,优选0.02<z<0.1,并且x+y+z=1,其中0≤w<1,优选0≤w<0.2。均质层的厚度优选为25-150nm,更优选为50-75nm。整个涂层的平均组成为AlaTibSicCrd(CeN1-e),其中0<a<0.5,优选0.05<a<0.4,其中0.1<b<0.9,优选0.3<b<0.9,其中0.01<c<0.17,优选0.02<c<0.1,其中0≤d<0.06,并且a+b+c+d=1,其中0≤e<1,优选0≤e<0.2。涂层的总厚度优选为0.5-20μm,更优选0.5-10μm,最优选1-5μm,所述涂层中多层结构反复地与均质层交替。
所有涂层呈现出具有明显的(200)织构的立方NaCl结构,所述明显的(200)织构的立方NaCl结构通过使用Bragg-Brentano X射线衍射而被确定。相比均质涂层,所有多层涂层都呈现出更强的XRD峰。相比均质层与多层结构交替的涂层,多层涂层呈现出更明显的(200)织构。
沉积有多层涂层的切削刀具可以是例如端铣刀、钻头以及刀具刀片,其中所述端铣刀、钻头以及刀具刀片由硬质合金、金属陶瓷、陶瓷、立方硼氮化物或高速钢制成。
包括多层结构的涂层可通过不同的PVD技术沉积到基底上并且交替地形成单层。单层厚度的无周期次序可以通过随机地开关单层源的闸门或者通过随机地切换所述源的开和关而形成。另外一种想得到的方法是在所述源前面随机地旋转或移动待涂覆基底。优选将基底放置在3次旋转基底工作台上来完成上述方法,所述工作台被布置成用于获得无周期的结构。能够在顺时针或逆时针方向上,调整3次旋转的旋转速度和旋转方向。
电子束蒸发、磁控溅射或阴极电弧沉积或者它们的组合,都是沉积涂层的优选PVD方法。
电弧源可包括金属的不同组合,并且单个源的组成可与整个多层结构的平均组成有所不同,并且仍然形成了在本发明范围之内的涂层。源的数目至少2个。
在本发明的一个实施方式中,包括(Ti,Al,Si)N+(Ti,Si)N、(Ti,Si)N+(Ti,Al)N、(Al,Cr)N+(Ti,Si)N或者(Al,Ti,Si)N+(Al,Cr)N的多层涂层被沉积到基底上,所述基底为高速钢,优选钻头或端铣刀。
在本发明的另一个实施方式中,包括(Ti,Al,Si)N+(Ti,Si)N、(Ti,Si)N+(Ti,Al)N、(Al,Cr)N+(Ti,Si)N或者(Al,Ti,Si)N+(Al,Cr)N的多层涂层被沉积到硬质合金基底上。
除上述涂层之外,根据本发明的涂层还包括一个或多个顶层,例如提高耐热性的层以及便于鉴定磨损的层。
根据本发明的多层结构特别适用于具有锋利切削刃的刀具几何形状。根据本发明的涂覆切削刀具在加工钢铁或不锈钢的时候,相对于现有技术中的刀具表现出改善的耐磨性。
实施例1
无周期通过反应PVD电弧放电蒸发将无周期多层结构沉积到由Co(10wt%)和其余为WC组成的硬质合金车削刀片上,从而制成涂覆刀片。多层结构从两种电弧源沉积到刀片上,所述刀片被安装到3次旋转基底工作台上,该工作台被布置成用于获得无周期的结构。电弧蒸发是在氩气与氮气的气氛中进行。得到的总涂层厚度约为2μm。沉积了三种不同的无周期多层结构。两种电弧源的组成以及无周期多层结构的平均化学组成如表1所示。多层结构具有无周期的单层次序,即非重复的厚度。截面透射电子显微镜研究显示了单个氮化层厚度在2到30nm范围内,并且层的总数超过100。
表1
涂层编号 | 源1 | 源2 | 平均化学组成 |
1 | Ti0.90Si0.10 | Al0.60Ti0.30Si0.10 | Al0.19Ti0.73Si0.08N |
2 | Ti0.90Si0.10 | Al0.55Ti0.40Si0.05 | Al0.16Ti0.78Si0.06N |
3 | Ti0.90Si0.10 | Al0.16Ti0.84 | Al0.06Ti0.88Si0.06N |
实施例2
由反复交替均质层和无周期多层结构组成的涂层通过反应PVD电弧放电蒸发沉积到由Co(10wt%)和其余为WC组成的车削刀片上。多层结构从两种电弧源沉积到刀片上,所述刀片被安装到3次旋转基底工作台上,该工作台被布置成用于获得无周期的结构。蒸发在氩气与氮气的混合物中进行。得到的总涂层厚度约为2μm。多层结构具有无周期的单层次序,即非重复的厚度。截面透射电子显微镜研究显示了单个氮化层厚度在2到30nm范围内。均质层厚度在25到150nm范围内。电弧源的组成以及整个涂层的平均化学组成如表2所示。均质层由表2中的电弧源2形成。
表2
涂层编号 | 源1 | 源2 | 平均化学组成 |
4 | Ti0.90Si0.10 | Al0.60Ti0.30Si0.10 | Al0.37Ti0.55Si0.08N |
5 | Ti0.90Si0.10 | Al0.55Ti0.40Si0.05 | Al0.34Ti0.60Si0.06N |
实施例3
在车削操作中对侧面磨损进行测试,切削条件如下:
工件材料: SS0737,具有厚壁的环
操作: 连续的端面车削
切削速度m/min 200
进给速度mm/r 0.10
切削深度mm 2
备注: 干工况
操作一直进行到整个外部直径都接受到车削操作。此后,刀片被直观地进行分析并且被分成“差”、“一般”和“好”。
多层结构与均质Ti0.9Si0.1N、均质Al0.51Ti0.45Si0.05N、均质Al0.56Ti0.34Si0.10N以及包括Al0.50Ti0.50N底层和Ti0.9Si0.1N顶层的涂层进行比较。所有涂层均具有与多层相同的总厚度。结果如表3所示:
表3
涂层类型 | 抗后面磨损能力 |
多层1号 | 好 |
多层2号 | 好 |
多层3号 | 好 |
多层4号 | 一般 |
多层5号 | 一般 |
均质Ti0.9Si0.1N | 差 |
均质Al0.51Ti0.45Si0.05N | 差 |
均质Al0.56Ti0.34Si0.10N | 差 |
两层Al0.50Ti0.50N(底层)Ti0.9Si0.1N(顶层) | 差 |
实施例4
在不锈钢车削操作中测试根据本发明的多层涂层1号、2号以及3号的抗剥落性,切削条件如下:
工件材料: 304L,Sanmac
操作: 端面车削,改变切削深度
切削速度m/min 100/140
进给速度mm/r 0.35
切削深度mm 4-0-4
备注: 湿工况
通过在SEM(扫描电子显微镜)中的研究来测量剥落。
多层结构与均质Ti0.9Si0.1N、均质Al0.51Ti0.45Si0.05N、均质Al0.56Ti0.34Si0.10N以及包括Al0.50Ti0.50N底层和Ti0.9Si0.1N顶层的涂层进行比较。所有涂层均具有与多层相同的总厚度。结果如表4所示:
表4
涂层类型 | 抗后面磨损能力 |
多层1号 | 好 |
多层2号 | 好 |
多层3号 | 好 |
均质Ti0.9Si0.1N | 差 |
均质Al0.51Ti0.45Si0.05N | 差 |
均质Al0.56Ti0.34Si0.10N | 差 |
两层Al0.50Ti0.50N(底层)Ti0.9Si0.1N(顶层) | 差 |
实施例5
在钢铁的车削操作中对刀具寿命进行测试,所述刀具涂覆有根据本发明的多层结构1-5号,切削条件如下:
工件材料: Ovako 825B
操作: 纵向车削
切削速度m/min 160
进给速度mm/r 0.35
切削深度mm 2
备注: 湿工况
刀具寿命在车削操作仪表中的距离上测量。刀具寿命的标准是刀具破裂。
多层结构与均质Ti0.9Si0.1N、均质Al0.51Ti0.45Si0.05N和均质Al0.56Ti0.34Si0.10N涂层进行比较。所有涂层均具有与多层相同的总厚度。结果如表5所示:
表5
涂层类型 | 刀具寿命(m) |
多层1-3号 | 20 |
多层4和5号 | 22 |
均质Ti0.9Si0.1N | 16 |
均质Al0.51Ti0.45Si0.05N | 5.5 |
均质Al0.56Ti0.34Si0.10N | 5.5 |
Claims (7)
1.一种切削刀具,包括基底,所述基底为烧结的硬质合金或金属陶瓷、陶瓷、立方硼氮化物或高速钢,所述切削刀具包括薄、粘附、硬且耐磨的涂层,所述涂层包括薄片状多层结构,所述多层结构为以非重复形式X+Y+X+Y+X…的耐火化合物交替层,其中所述交替层X和Y由金属氮化物、金属碳化物或者金属碳氮化物组成,其中在所述涂层中,贯穿整个多层结构,单层厚度的次序没有重复周期,而基本上是无周期的,其特征在于,所述单个X或Y层的厚度大于0.1nm但小于100nm,优选小于50nm,最优选在2-30nm之间,基本上随机地变化,并且所述多层涂层的总厚度为0.5μm-20μm,优选1-10μm,并且最优选1-5μm,所述多层结构的平均化学组成为:AlaTibSicCrd(CeN1-e),其中0<a<0.5,优选0.05<a<0.4,其中0.1<b<0.9,优选0.3<b<0.9,其中0.01<c<0.17,优选0.02<c<0.1,其中0≤d<0.06,并且a+b+c+d=1,其中0≤e<1,优选0≤e<0.2。
2.根据权利要求1所述的切削刀具,其特征在于,层X和Y为金属元素的氮化物,所述金属元素选自Ti、Cr,、Al和Si以及它们的混合物。
3.根据前述权利要求中任一项所述的切削刀具,其特征在于,所述多层结构X+Y+X+Y+X…是下列组合中的任一种:(Al,Ti,Si)N+(Ti,Si)N、(Ti,Si)N+(Al,Ti)N、(Al,Cr)N+(Ti,Si)N以及(Al,Ti,Si)N+(Al,Cr)N。
4.根据前述权利要求中任一项所述的切削刀具,其特征在于,所述涂层包括均质层,所述均质层反复地与多层结构交替,并且其中所述均质层包括金属氮化物、金属碳化物或金属碳氮化物或者它们的混合物,并且其中所述涂层的平均化学组成为:AlaTibSicCrd(CeN1-e),其中0<a<0.5,优选0.05<a<0.4,其中0.1<b<0.9,优选0.3<b<0.9,其中0.01<c<0.17,优选0.02<c<0.1,其中0≤d<0.06,并且a+b+c+d=1,其中0≤e<1,优选0≤e<0.2。
5.根据权利要求4所述的切削刀具,其特征在于,所述均质层的化学组成为:TixAlySiz(CwN1-w),其中0<x<0.7,优选0.05<x<0.6,其中0.1<y<0.9,优选0.3<y<0.9,其中0.01<z<0.17,优选0.02<z<0.1,并且x+y+z=1,其中0≤w<1,优选0≤w<0.2。
6.根据权利要求4或5中的任一项所述的切削刀具,其特征在于,所述均质层的平均厚度为25-150nm,优选50-75nm。
7.根据权利要求4、5或6中的任一项所述的切削刀具,其特征在于,反复地与所述多层结构交替的所述均质层的总厚度为0.5μm-20μm,优选1-10μm,并且最优选为1-5μm。
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KR101520962B1 (ko) | 2015-05-15 |
JP4874947B2 (ja) | 2012-02-15 |
US20080166583A1 (en) | 2008-07-10 |
SE0602814L (sv) | 2008-06-28 |
US20080166588A1 (en) | 2008-07-10 |
WO2008079088A3 (en) | 2008-08-14 |
US8119262B2 (en) | 2012-02-21 |
EP1939327B1 (en) | 2018-06-27 |
EP1939327A1 (en) | 2008-07-02 |
JP2010514578A (ja) | 2010-05-06 |
WO2008079088A2 (en) | 2008-07-03 |
CN101578396A (zh) | 2009-11-11 |
KR20090094108A (ko) | 2009-09-03 |
EP1939328B1 (en) | 2018-02-21 |
CN101209611B (zh) | 2012-12-05 |
EP1939328A1 (en) | 2008-07-02 |
JP5406041B2 (ja) | 2014-02-05 |
JP2008162009A (ja) | 2008-07-17 |
CN101578396B (zh) | 2012-05-09 |
KR20080061323A (ko) | 2008-07-02 |
KR101465278B1 (ko) | 2014-11-26 |
US8227098B2 (en) | 2012-07-24 |
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