CN100418679C - 用于修整硬质钢的复合涂层 - Google Patents
用于修整硬质钢的复合涂层 Download PDFInfo
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- CN100418679C CN100418679C CNB2006100940116A CN200610094011A CN100418679C CN 100418679 C CN100418679 C CN 100418679C CN B2006100940116 A CNB2006100940116 A CN B2006100940116A CN 200610094011 A CN200610094011 A CN 200610094011A CN 100418679 C CN100418679 C CN 100418679C
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- 229910052799 carbon Inorganic materials 0.000 claims abstract description 12
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- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 6
- 229910052735 hafnium Inorganic materials 0.000 claims abstract description 4
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Abstract
本发明提供一种切削刀具刀片、立式端铣刀或者钻头，包括基底和涂层。涂层由一层或多层耐高温化合物构成，其中，至少一层涂层包括立方(Me，Si)X相，其中Me是Ti、V、Cr、Zr、Nb、Mo、Hf、Ta和Al中的一种或多种，X是N、C、O或B中的一种或多种。c-MeSiX相的比例R＝(at-%X)/(at-%Me)在0.5和1.0之间，并且X含有小于30at-%的O+B。本发明对于切屑厚度小并且工件材料硬的金属加工应用特别有用，例如使用立式端铣刀、刀片铣削刀具进行的仿型铣削或者对硬质钢进行钻孔。
Description
技术领域
本发明涉及一种用于通过除去切屑进行机加工的切削刀具，它包括立方氮化硼基材料的基底和硬的耐磨耐高温涂层，该涂层的至少一层包括在沉积过程中形成的Me-Si-X相，沉积过程中该相或者作为单相沉积而成或者与其它相同时沉积而成，或者与具有不同化学成分的同一相同时沉积而成。根据本发明的刀具特别适用于金属切削应用，其中，切屑厚度小并且工件材料硬，例如硬质钢的修整。
背景技术
立方氮化硼(cBN)具有仅次于金刚石的硬度和导热性以及优良特性，例如比金刚石弱的与铁金属反应的性质。加工硬质钢、铸铁和镍基合金时，使用多晶立方氮化硼(PcBN)、例如含有cBN的烧结体的切削刀具替代了硬质合金或者金属陶瓷的刀具，以便提高加工效率。
用于切削刀具的PcBN烧结体包括cBN颗粒和粘结剂。它们通常分为下列两组：
-主要用于硬质钢且耐磨性和强度良好平衡的烧结体，包括通过粘结剂结合的30到80volume％(体积百分比)的cBN颗粒，粘结剂主要由Ti型陶瓷构成，例如TiN，TiC，Ti(C，N)等；
-主要用于铸铁且导热性和强度良好平衡的烧结体，包括直接结合的80到90volume％的cBN颗粒和余量的粘结剂，粘结剂主要由Al化合物或者Co化合物构成。
但是，cBN颗粒的缺点是它们与铁金属的亲和力比TiN，TiC，Ti(C，N)粘结剂的大。因此，采用cBN的切削刀具由于热磨损其服务寿命较短，因为热磨损最后引起刀具刀刃折断。为了进一步提高PcBN刀具的耐磨性和断裂强度，已经提出利用TiN、Ti(C，N)、(Ti，Al)N等的涂层涂覆PcBN刀具，例如US5853873和US6737178所述。
然而，涂层PcBN刀具面临的问题是经常发生不希望的涂层脱层。
JP-A-1-96083或JP-A-1-96084公开了对涂覆有这种涂层的PcBN刀具的粘结强度的改进，该涂层由钛的氮化物、碳化物或碳氮化物构成，通过金属Ti层形成，平均厚度为0.05-0.3μm。
US-A-5,583,873公开了具有高粘结强度并且作为cBN基底与(Ti，Al)N涂覆薄膜之间的中间层的TiN层，用于将(Ti，Al)N涂覆薄膜粘结到基底上。
US6,737,178公开了TiN、Ti(C，N)、(Ti，Al)N、Al2O3、ZrN、ZrC、CrN、VN、HfN、HfC和Hf(C，N)的涂层。
US6,620,491公开了一种表面涂覆氮化硼的刀具，其具有硬质涂层和从元素周期表的4a、5a和6a族选择的至少一种元素构成的中间层，中间层厚度最大为1μm。硬质涂层中含有的至少一层包括从4a、5a和6a族选择的至少一种元素，Al、B、Si和Y，以及从C、N和O构成的组中选择的至少一种元素，其厚度为0.5-10μm。中间层含有Cr、Zr和V中的至少一种。
US-B-6,811,580、US-B-6,382,951和US-B-6,382,951公开了涂覆有Al2O3的立方氮化硼刀片。
发明内容
本发明的目的是提供一种改进的切削刀具，其以包括高压相类型的氮化硼、例如cBN的烧结体为基，并且具有粘结强度优异的涂层，目的在于对硬质钢或铸铁进行除屑加工。
本发明的另一个目的是提供一种基于粘结强度优异的PcBN在切削刀具上沉积涂层的方法，目的在于对硬质钢或铸铁进行除屑加工。
本发明提供了一种制造涂层切削刀具刀片、立式端铣刀或钻头的方法，所述涂层切削刀具刀片、立式端铣刀或钻头包括多晶立方氮化硼(PcBN)基材料的基底和涂层，所述涂层由一层或多层耐高温化合物层构成，其中至少一层包括成分被描述为Me1-aSiaXb的Me1-aSiaXb相，其中，Me为元素Ti、V、Cr、Zr、Nb、Mo、Hf、Ta和Al中的一种或几种，a在0.05和0.4之间，X为元素N、C、O和B中的一种或几种，b在0.5和1.1之间，并且X含有小于30at-％的O+B，使用电弧蒸发技术进行涂覆，蒸发电流为50-200A，基底偏压为-10--150V，温度为400-700℃，总压力为0.5-9Pa，由此利用Ar离子蚀刻按照起始偏压Vs＜-500V到结束偏压Vs＞-150的两个或多个步骤的顺序，对要被涂覆的表面进行预处理，而获得cBN相的较小分数投影表面面积，与cBN的分数体积相比，比例L＜1.15，所述比例L定义为在进行涂层沉积之前，cBN的分数投影表面面积AcBN除以cBN的分数体积VcBN，L＝AcBN/VcBN。
已经发现，通过在PcBN基的切削刀具上施加性能和工艺优化的涂层可以显著地改进涂层刀具的摩擦性能。通过平衡生长期间的化学成分、热能的量和感应表面的激活程度，可以获得含有(Me，Si)X相的涂层，与现有技术相比，该涂层表现出对硬质钢进行金属切削的改进性能。由于优化的预处理和沉积条件，涂层的附着力非常好。涂层包括与其它相的晶粒同时存在的(Me，Si)X晶粒或者仅是(Me，Si)X晶粒。使用PVD技术、优选为电弧蒸发技术，沉积一层或多层涂层。
附图说明
图1为从根据本发明在PcBN基底上沉积Ti0.77Si0.23N涂层获得的θ-2θ几何内的CuKαX射线衍射图案，图中的指数表示涂层的NaCl型结构，即，(Ti，Si)N。
图2为根据本发明在PcBN基底上沉积的Ti0.77Si0.23N涂层的样品表面与主要光束之间，采用1°的恒定入射掠角所获得的CuKαX射线衍射图案，图中的指数表示涂层的NaCl型结构，即，(Ti，Si)N。
图3为示出涂覆之前常规离子蚀刻之后的PcBN材料结构的SEM显微图。
图4为示出涂覆之前根据本发明的离子蚀刻之后的PcBN材料结构的SEM显微图。
具体实施方式
本发明提供一种切削刀具，用于通过切屑去除进行机加工，所述刀具包括多晶立方氮化硼(PcBN)基材料的基体，在基体上沉积耐磨涂层。该涂层由一层或多层耐高温化合物构成，包括由(Me，Si)X相的晶粒构成的至少一层，优选利用物理气相沉积(PVD)方法进行涂覆。其它层由元素周期表中的4-6族元素的氮化物和/或碳化物和/或氧化物构成。根据本发明的刀具对于修整硬质钢或者灰口铸铁的金属切削应用特别有效，硬质钢或者灰口铸铁的加工部件的表面粗糙度通常会限制刀具寿命。
一层或多层(Me，Si)X涂层包括Me1-aSiaXb相的晶粒，其中，Me为Ti、Zr、Hf、V、Nb、Ta、Cr和Al中的一种或多种，优选为Ti、Cr、Zr和All中的一种或多种，并且a在0.05和0.4之间，优选在0.1和0.3之间，X为N、C、O和B之间的一种或多种，并且b在0.5和1.1之间，优选在0.8和1.05之间。
通过X射线衍射(XRD)检测Me1-aSiaXb相晶体的存在，使用CuKα放射在θ-2θ和/或入射掠角几何内示出如下一个或多个特征：
●对于Ti1-xSixN在大约36°2θ，具有(Me，Si)X(111)波峰；
●对于Ti1-xSixN在大约42°2θ，具有(Me，Si)X(200)波峰；
●对于Ti1-xSixN在大约61°2θ，具有(Me，Si)X(220)波峰；
●当Me不是Ti或者Me和Si的相对含量不同时，波峰的位置会改变；
●(Me，Si)X的结构优选为NaCl型；
●将织构定义为，比例K为Me1-aSiaXb(111)的波峰面积(A(Me1-aSiaXb)111)与Me1-aSiaXb(200)的波峰面积(A(Me1-aSiaXb)200)之间的比例，即，K＝A(Me1-aSiaXb)111/A(Me1-aSiaXb)200，在X射线衍射图案中，在θ-2θ几何内，K值在0.0和1.0之间，优选在0.0和0.3之间，和/或对于Me1-aSiaXb(200)，波峰与背景的比例(波峰最大处的指数除以波峰附近的平均背景指数)大于2，优选大于4；
●该涂层的波峰宽度FWHM(半幅全宽)值主要是其小晶粒尺寸的影响(该设备的作用是大约2θ＝0.05°，并且因此在这些计算中不予考虑)：
○(Me，Si)X(111)波峰的FWHM在0.4和1.5°2θ之间，和/或
○(Me，Si)X(200)波峰的FWHM在0.4和1.5°2θ之间；
●X含有小于30at-％(原子百分比)的O和/或B，余量为N和/或C。碳氮化物和碳化物比氮化物更为优选。(Me，Si)X中的X应当小于15at％的C。添加1-10at-％的O会促进细小晶粒结构的生长并且提高抗氧化性，但是，这会提高出现非传导涂层空腔的危险并且因而导致产品问题；
●非结晶相被识别为宽波峰(FWHM＝4°-6°)并且定位在2θ＝36°-38°。非结晶相和结晶相的比例一般是0≤Aa/Ac＜0.20，Aa是测量的非结晶相波峰的折射强度，Ac是结晶相在(200)处波峰的强度。
与NaCl型Ti1-yAlyN结构的立方单相涂层相比，包括(Me，Si)X的涂层具有显著提高的硬度，请见实施例1，这已经为系统Ti1-xSixN和Ti1-yAlyN所证实。
如果根据本发明的含有(Me，Si)X的涂层与其它涂层结合，则总的涂层厚度为0.1到5μm，优选为0.1到3μm，不含有(Me，Si)X的涂层的厚度在0.1和3μm之间变化。对于修整的应用，涂层厚度小于2μm，优选小于1.2μm。
在一个实施例中，厚度为0.1到2μm的含有(Me，Si)X的涂层为0.5到5μm厚的多层涂层中的高达五种不同材料中的一种，该多层涂层由2-200个、优选5-50个单层构成。
在一个优选实施例中，Me＝Ti，其成分为(Ti0.9-0.7Si0.10-0.30)N，优选为(Ti0.85-0.75Si0.15-0.25)N。
在另一个优选实施例中，Me＝Ti和Al，其成分为(Ti0.6-0.35Al0.20-0.40Si0.15-0.30)N，优选为(Ti0.6-0.35Al0.25-0.35Si0.15-0.30)N。
在另一个优选实施例中，在最外面涂覆TiN和/或CrN和/或ZrN的顶层。
PcBN具有的立方氮化硼(cBN)其含量在30和80vol-％之间，用于加工硬质钢，具有80和90vol-％之间含量的立方氮化硼用于加工铸铁，在用于加工硬质钢的NaCl型粘结相Ti(C，N)中，优选含量在35和60vol-％之间并且具有0.5-2μm的晶粒尺寸的cBN。
优选地，根据本发明的涂层成分是这样，其晶胞参数在NaCl型结构粘结相的晶胞参数的+/-2％内，最优选为在其+/-1％内，以便获得增加的外延生长量和最大的粘结强度。采用X射线衍射在抛光的样品截面上测量NaCl型结构粘结相的晶胞参数。采用X射线衍射在涂层样品上测量涂层的晶胞参数。优选该涂层与基底直接接触。这种晶胞匹配成分的例子是(Ti0.85-0.75Si0.15-0.25)N和(Ti0.37Al0.25Zr0.18Si0.20)N。或者，可以具有位于基底与该涂层之间且厚度＜0.3μm的中间层(一层或多层)，而不是匹配的晶胞。
本发明也涉及一种在PcBN基底上生长包括(Me，Si)X相的涂层的方法。
首先，优选通过施加温和的Ar离子蚀刻获得优化的表面状态，该蚀刻能够获得cBN晶粒以及粘结相的良好刻蚀和清洁，而不会利用优选的溅射降低粘结相的表面成分。在Ar气氛或者Ar和H2的混和气氛下进行Ar离子蚀刻，在后一情形下可以实现物理溅射和化学蚀刻的综合效果，按照两个或多个步骤的顺序进行，其中碰撞离子的平均能量从基底偏压Vs＜-500V开始到最后Vs＞-150V逐渐减小。如果需要，中间步骤采用-500V＜Vs＜-150V。最优选地，向采用的基底偏压利用双极电压施加频率＞5kHz的脉冲并被施加。负脉冲优选大于随后的正放电脉冲的80％。
图3为示出具有NaCl型结构粘结相的PcBN材料在涂覆之前进行传统的离子蚀刻后结构的SEM显微图，图4是在涂覆之前进行根据本发明的蚀刻之后结构的SEM显微图。如图所示，比较图3和图4，传统蚀刻除去太多的粘结相因此露出cBN晶粒。比例L被定义为，进行涂层沉积之前，露出的cBN分数投影表面面积AcBN除以cBN的分数体积VcBN(L＝AcBN/VcBN)，L＜1.15，优选＜1.0。与50％的大块的体积分数相比，cBN的表面含量在图3中为59％(L＝1.18)，在图4中为49％(L＝0.98)。
通过化学处理和/或机械处理，例如在沉积之前进行轻微的喷丸处理，和/或与沉积系统中的原地处理相结合，也可以获得适宜的表面。
为了获得根据本发明的涂层的优选结构，需要精密调节数个沉积参数。影响沉积的因素为与碰撞离子的能量有关的温度、阴极与基底的距离和N2的分压，PN2，碰撞离子的能量可被基底偏压改变。
用于生长包括本发明的(Me，Si)X相的涂层的方法，在这里该涂层可被示例为Ti1-xSixN系统，其建立在合金或复合阴极在下述条件下的电弧蒸发的基础上：
Ti+Si阴极的成分是60到90at-％的Ti，优选为70到90at-％的Ti和余量的Si；
根据阴极大小和阴极材料，蒸发电流在50A和200A之间。当使用直径为63mm的阴极时，蒸发电流优选在60A和120A之间；
基底偏压优选在-10V和-150V之间，优选在-40V和-70V之间；
沉积温度在400℃和700℃之间，优选在500℃和700℃之间。
当生长含有(Me，Si)X的一层或多层涂层时，其中，X为N，采用Ar+N2气氛，其中含有0-50vol-％、优选为0-20vol-％的Ar，总压力为0.5Pa到9.0Pa，优选为1.5Pa到5.0Pa。
为了生长(Me，Si)X，其中X包括C和O，需要向N2和/或Ar+N2气氛(例如C2H2，CH4，CO，CO2，O2)中加入含有C和/或O的气体。如果X也包括B，可以或者通过利用B对标靶进行合金化或者通过向气氛中添加含有B的气体来实现。
准确的工艺参数取决于采用的涂覆设备的设计和条件。本领域技术人员应当能够确定是否已经获得必需的结构和根据说明书内容对沉积条件进行修改。
当生长含有(Me，Si)X相的涂层时，存在着压缩残余应力变得很大的危险，在使用尖锐的切削刃时和/或对良好附着力的需求是非常重要的情形下时，这会负面影响加工应用中的性能。通过在Ar和/或N2气氛下，在600℃和1100℃温度之间回火20到600分钟，而能够减小残余应力。
另外，通过增加改进切削刃表面粗糙度的后处理可以获得改善。这可以通过湿喷实现。并且，可以使用嵌有研磨颗粒的尼龙刷。另一方法是通过研磨方式，例如抛光或拖压精加工(dragfinishing)，移动涂覆的PcBN刀具。
已经参照使用电弧蒸发沉积的含有(Me，Si)X相的涂层描述了本发明。很明显，也可以采用其它PVD技术，例如磁控管溅射，来制造含有(Me，Si)X相的涂层。
实施例1
在超声波浴中使用苛性碱溶液和酒精清洗RCGN0803M0S类型的多晶立方氮化硼(PcBN)刀片，其具有50％的体积分数、平均晶粒尺寸为1μm的cBN并含有Ti(C，N)的粘结相，然后使用三折旋转(three foldrotation)的固定件将刀片定位在PVD系统中。阴极到基底的最短距离是160mm。将系统排气到小于2.0×10-3Pa的压力，然后利用Ar离子对刀片进行溅射清洁。使用双极脉冲工艺，其中，基底偏压在-Vs(80％)和+50V(20％)之间变化一个周期，该周期的频率为20kHz。Vs是工艺的起始偏压-550V，然后递进变化到最后的-120V。图4示出PcBN表面在采用这种工艺蚀刻后的表面。
使用Ti0.75Si0.25阴极、其直径为63mm的电弧蒸发对样品A进行涂层生长，而样品B使用Ti0.80Si0.20阴极。在纯度为99.995％的N2气氛下进行沉积，总压力为4.0Pa，使用基底偏压-110V，进行60分钟。沉积温度大约530℃。沉积后，立即用干燥的N2排空沉积室。参考现有技术的涂覆工艺，使用Ti0.34Al0.66N和没有涂层的样品
图1和图2中示出沉积Ti1-xSixN涂层和TiN涂层的X射线衍射图案。除了与PcBN基底相应的波峰外，显示出来的唯一波峰是那些与立方NaCl型Ti1-xSixN相和立方NaCl型TiN相对应的波峰，从(111)、(200)、(220)、(311)、(222)、(400)、(331)、(420)、(422)，和(511)波峰的标记可以看出。由(Me，Si)X(111)波峰和(Me，Si)X(200)波峰的面积之间的比例(K)所定义的织构，对于本样品是0.28。(Me，Si)X(111)波峰的FWHM是1.30°2θ，而(Me，Si)X(200)波峰的FWHM是1.44°2θ。
利用X射线衍射使用主要光束和样品表面之间恒定的1°入射掠角，制造在沉积状态下的Ti1-xSixN的相标记，并且扫描检测器，以便放大来自涂层的波峰，参见图2。通过NaCl型结构内的衍射图案的指数来确定Ti1-xSixN的存在。
对于Ti1-xSixN(200)波峰，波峰与背景的比例是24。
在横截面上使用扫描电子显微镜(SEM)，确定切削刃上Ti1-xSixN涂层的厚度是1.0μm。
(Ti0.77Si0.23)N的晶胞参数是4.29
含有Ti(C，N)相的PcBN粘结相的晶胞参数是4.30
Ti0.34Al0.66N的晶胞参数是4.14
采用Nano IndenterTM II设备，在抛光的锥形横截面上使用导致大约200nm的最大穿透深度的25mN的最大载荷，利用纳米压痕方法，测量涂层的维氏硬度。表1中给出硬度。从表1中可以看出，与Ti1-yAlyN样品相比，当涂层中出现Si时，硬度急剧增加。
表1
实施例2
实施例1的涂层切削刀具刀片包括RCGN0803M0S型号的多晶立方氮化硼(PcBN)，在硬质齿轮的修整操作中对其进行测试。使用的切削数据如下：
●材料：SAE 5120(20MnCr5)，59-61HRC
●vf＝190m/min
●ap＝0.10mm
●fn＝0.07mm/rev.
工具寿命标准是对于加工部件的给定75％最小浮力水平(buoyancy level)加工出的齿轮数目。表2中给出结果。
表2
测试表明，样品A和B(本发明)能够加工最大数目的部件，样品C加工的部件数目在它们之后。
实施例3
刮擦器类型的切削刀具刀片以类似实施例1的方式进行涂覆，由CNGA120408S-L1-WZ型号的多晶立方氮化硼(PcBN)刀片构成，在硬质齿轮轴的情况下进行修整操作。使用下列切削数据：
●材料：SAE 5115(16MnCrS5)，58HRC
●vf＝190m/min
●ap＝0.15/0.35mm
●fn＝0.3mm/rev.
工具寿命标准是加工出给定最大表面粗糙度的齿轮轴的数目。结果示于表3中。
表3
测试表明，样品A(本发明)能够加工出最大数目的部件。
实施例4
以类似实施例1的方式涂覆切削刀具刀片，其由CNGA120408S-L0-B型号的多晶立方氮化硼(PcBN)刀片构成，刀片插在硬质插座内。使用的切削数据如下：
●材料：SAE 52100(100Cr6)，63HRC
●vf＝220m/min
●ap＝0.11/0.15mm
●fn＝0.3mm/rev.
工具寿命标准是加工出给定最大表面粗糙度的插座的数目。结果示于表4中。
表4
该测试表明，样品B(本发明)能够加工出最大数目的部件。
Claims (4)
1. 一种制造涂层切削刀具刀片、立式端铣刀或钻头的方法，所述涂层切削刀具刀片、立式端铣刀或钻头包括多晶立方氮化硼(PcBN)基材料的基底和涂层，所述涂层由一层或多层耐高温化合物层构成，其中至少一层包括成分被描述为Me1-aSiaXb的Me1-aSiaXb相，其中，Me为元素Ti、V、Cr、Zr、Nb、Mo、Hf、Ta和Al中的一种或几种，a在0.05和0.4之间，X为元素N、C、O和B中的一种或几种，b在0.5和1.1之间，并且X含有小于30at-％的O+B，使用电弧蒸发技术进行涂覆，蒸发电流为50-200A，基底偏压为-10--150V，温度为400-700℃，总压力为0.5-9Pa，其特征在于，由此利用Ar离子蚀刻按照起始偏压Vs＜-500V到结束偏压Vs＞-150的两个或多个步骤的顺序，对要被涂覆的表面进行预处理，而获得cBN相的较小分数投影表面面积，与cBN的分数体积相比，比例L＜1.15，所述比例L定义为在进行涂层沉积之前，cBN的分数投影表面面积AcBN除以cBN的分数体积VcBN，L＝AcBN/VcBN。
2. 根据权利要求1所述的方法，其特征在于a在0.1和0.3之间。
3. 根据权利要求1所述的方法，其特征在于b在0.8和1.05之间。
4. 根据权利要求1所述的方法，其特征在于L＜1.0。
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Also Published As
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| US20060292399A1 (en) | 2006-12-28 |
| ATE418626T1 (de) | 2009-01-15 |
| EP1736565A1 (en) | 2006-12-27 |
| CN1883855A (zh) | 2006-12-27 |
| BRPI0602327A (pt) | 2007-02-21 |
| SE0501487L (sv) | 2006-12-23 |
| SE529161C2 (sv) | 2007-05-22 |
| EP1736565B1 (en) | 2008-12-24 |
| US20110123829A1 (en) | 2011-05-26 |
| JP2007001007A (ja) | 2007-01-11 |
| CZ2006400A3 (cs) | 2007-01-31 |
| DE602006004400D1 (de) | 2009-02-05 |
| KR20060134859A (ko) | 2006-12-28 |
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