CN113454047A - cBN烧结体及切削工具 - Google Patents

cBN烧结体及切削工具 Download PDF

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CN113454047A
CN113454047A CN202080015828.8A CN202080015828A CN113454047A CN 113454047 A CN113454047 A CN 113454047A CN 202080015828 A CN202080015828 A CN 202080015828A CN 113454047 A CN113454047 A CN 113454047A
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cbn
metal
sintered body
metal boride
boride
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CN113454047B (zh
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门马征史
小口史朗
武井亮太
油本宪志
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Mitsubishi Materials Corp
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Mitsubishi Materials Corp
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Abstract

本发明的cBN基超高压烧结体含有cBN粒子和结合相。所述结合相包含Al的氮化物或氧化物、或Ti的氮化物或碳化物或碳氮化物中的至少一种，且在所述结合相中，平均粒径为20～300nm的金属硼化物分散有0.1～5.0体积％。所述金属硼化物为金属成分包含Nb、Ta、Cr、Mo、W中的至少一种且不包含Ti的金属硼化物(B)和金属成分仅包含Ti的金属硼化物(A)。当将所述金属硼化物中金属硼化物(A)的比例(体积％)设为Va且将所述金属硼化物(B)的比例(体积％)设为Vb时，比Vb/Va为0.1～1.0。

Description

cBN烧结体及切削工具
技术领域
本发明涉及一种立方晶氮化硼(cBN)基超高压烧结体(以下，有时称为“cBN烧结体”)及将cBN烧结体作为工具基体的切削工具(以下，有时标记为“CBN工具”)。
本申请根据2019年2月27日在日本申请的专利申请2019-034794号主张优先权，并将其内容援用于此。
背景技术
一直以来，已知cBN烧结体的韧性优异，其被广泛用作钢、铸铁等铁系工件材料的切削工具材料，并且通过对结合相的结构进行改良来提高了韧性。
在专利文献1中记载有一种cBN烧结体，其在结合相中分散分布有平均粒径为50～500nm的微细的Ti硼化物相和平均粒径为50～500nm的微细的W硼化物相，并且通过结合相的分散强化作用来提高了韧性。
在专利文献2中记载有一种cBN烧结体，其通过在结合相中含有将V、Nb及Ta中的至少一种和Ti作为金属成分的复合氮化物及复合碳氮化物中的至少一种复合化合物、V、Nb及Ta中的至少一种的斜方晶硼化物及AlN来提高了热稳定性和韧性。
专利文献1：日本专利第6032409号公报
专利文献2：日本专利第4830571号公报
通过所述各技术，cBN烧结体的韧性得到了提高。但是，由于近年来进一步高速化的切削加工，对cBN烧结体要求进一步提高韧性。
本发明的目的在于提供一种更高韧性的cBN烧结体及将其作为工具基体的CBN工具。
本发明人对cBN粒子与结合相的结合状态进行了深入研究，其结果得到了如下的新见解：若将金属硼化物粒子分散于结合相中，则促进烧结体中的cBN粒子与结合相的反应而使结合变得牢固，从而cBN烧结体的韧性得到提高。
发明内容
本发明基于所述见解，其包括下述方式。
(1)本发明的一方式的cBN基超高压烧结体含有cBN粒子和结合相，所述结合相包含Al的氮化物或氧化物、或Ti的氮化物或碳化物或碳氮化物中的至少一种，且在所述结合相中分散有0.1～5.0体积％的平均粒径为20～300nm的金属硼化物，更优选分散有0.1～4.0体积％，进一步优选分散有0.1～3.0体积％。所述金属硼化物含有金属成分包含Nb、Ta、Cr、Mo及W中的至少一种且不包含Ti的金属硼化物(B)和仅包含Ti的金属硼化物(A)。当将所述金属硼化物中所述仅包含Ti作为金属成分的金属硼化物(A)的比例(体积％)设为Va、且将所述包含Nb、Ta、Cr、Mo、W中的至少一种作为金属成分且不包含Ti的金属硼化物(B)的比例(体积％)设为Vb时，比Vb/Va满足0.1～1.0。比Vb/Va更优选为0.2～0.8，进一步优选为0.3～0.7。
(2)另一方式为所述(1)中所记载的cBN基超高压烧结体，其中，当将所述包含Nb、Ta、Cr、Mo及W中的至少一种作为金属成分且不包含Ti的金属硼化物(B)中六方晶结构的金属硼化物的{001}面的X射线衍射峰的最大强度设为Ihex、且将所述cBN粒子的{111}面的X射线衍射峰强度设为IcBN时，0.04≤Ihex/IcBN≤0.20。Ihex/IcBN更优选为0.06～0.17，进一步优选为0.08～0.15。
(3)另一方式为所述(1)或(2)中所记载的cBN基超高压烧结体，其中，所述cBN粒子的含有比例为40～80体积％。并且，当将所有的所述cBN粒子的含有比例设为100体积％时，平均粒径小于2μm的cBN粒子为5～40体积％，平均粒径为2μm以上且小于8μm的cBN粒子为60～95体积％。
(4)另一方式为一种切削工具，其具备所述(1)至(3)中任一项中所记载的cBN基超高压烧结体。所述切削工具可以具有由所述cBN基超高压烧结体构成的工具主体和形成于该工具主体的切削刃。所述切削工具也可以为具有由所述cBN基超高压烧结体构成的刀片(insert)主体和形成于该刀片主体的切削刃的切削刀片。
本发明的cBN基超高压烧结体的韧性得到更进一步提高，具备该cBN基超高压烧结体的切削工具发挥优异的耐缺损性、耐崩刀性。
附图说明
图1是表示本发明的cBN基超高压烧结体的烧结组织的示意图。各组织的形状或尺寸并不是描绘了实际烧结组织。
具体实施方式
以下，对本发明的cBN烧结体及将其作为工具基体的切削工具(CBN工具)进行更详细的说明。在本说明书及权利要求书中，当使用“～”表示数值范围时，该范围包括上限及下限的数值。
1.结合相
结合相优选包含Al的氮化物或氧化物、或Ti的氮化物或碳化物或碳氮化物中的至少一种。这些Al的氮化物或氧化物、或Ti的氮化物或碳化物或碳氮化物能够使用以往公知的化合物。
2.分散于结合相中的金属硼化物粒子
在结合相中以规定比例分散有规定大小的金属硼化物(也可以为复合硼化物)粒子。金属硼化物包含以往公知的所有原子比，并且该原子比并不一定仅限于化学计量范围内的原子比。
(1)金属硼化物粒子的平均粒径
关于分散于结合相中的金属硼化物粒子的大小，优选平均粒径为20～300nm的金属硼化物粒子相对于cBN烧结体整体优选以0.1～5.0体积％、更优选以0.1～4.0体积％、进一步优选以0.1～3.0体积％分散。当金属硼化物粒子的平均粒径小于20nm时，无法充分得到cBN粒子与结合相的反应促进效果，当超过300nm时，金属硼化物变得粗大，成为切削中的缺损的主要原因。并且，当金属硼化物粒子的含有比例小于0.1体积％时，金属硼化物量不充分，无法充分得到cBN粒子与结合相的反应促进效果，当超过5.0体积％时，作为cBN烧结体的硬度和韧性下降，成为切削中的缺损的主要原因。即使在金属硼化物粒子的含有比例为3.0～5.0体积％的情况下，若金属硼化物以微粒形式分散于结合相中且cBN烧结体的烧结充分进行，则通过硬质粒子的分散而显现韧性提高，硬度和韧性的下降被抑制为较小，成为切削中的缺损的主要原因的情况较少。
为了求出金属硼化物的平均粒径，使用俄歇电子能谱(Auger ElectronSpectroscopy：以下，称为AES)装置，对cBN烧结体的截面组织得到金属元素及硼元素的映射图像，通过图像处理提取金属元素及硼元素重叠的部位，将该部位确定为金属硼化物粒子。接着，对所确定的各粒子进行图像分析来求出平均粒径。具体而言，为了明确地判断结合相中的金属硼化物粒子，在使用AES得到的同一视场中的金属元素及硼元素的各映射图像中，将对象元素不存在的部位设为白色，将对象元素存在的部位设为黑色，以黑色为0、白色为255的256灰度的单色获取，并以在各个单色图像中各元素存在的位置成为黑色的方式进行二值化处理。在进行二值化处理而得到的同一视场内的金属元素及硼元素的映射图像中，比较金属元素及硼元素存在的、即金属元素及硼元素的各映射图像，将均成为黑色的部位确定为金属硼化物粒子。
也可以进行将认为金属硼化物粒子彼此接触的部分切离的处理，例如使用作为图像处理法之一的分水岭算法(Watershed)将认为相互接触的金属硼化物粒子彼此分离的处理。例如，可以比较金属元素及硼元素的各映射图像，对提取了均为黑色的部分之后的图像进行所述分离处理。
首先，对二值化处理后得到的图像内的相当于金属硼化物粒子的部分(黑色部分)进行粒子分析，将求出的最大长度作为各粒子的直径。作为求出最大长度的粒子分析，例如从通过对一个金属硼化物粒子计算出费雷特径而得到的两个长度中，将较大的长度的值作为最大长度，并将该值作为各粒子的直径。将假定为具有该直径的理想球体而通过计算求出的体积作为各粒子的体积来求出累计体积，基于该累计体积，将纵轴作为体积百分比[％]、横轴作为直径[μm]而描绘出图表。接着，将体积百分比为50％时的直径作为金属硼化物粒子的平均粒径，对3个观察区域进行该处理，将其平均值作为金属硼化物的平均粒径[μm]。在进行粒子分析时，使用利用SEM(扫描型电子显微镜)可预先得知的标度(scale)值，设定好每个像素的长度(μm)。作为图像处理中使用的观察区域，作为一例优选8.0μm×8.0μm的视场区域。
(2)金属硼化物粒子的金属成分
金属硼化物粒子优选具有金属成分包含Nb、Ta、Cr、Mo及W中的至少一种且不包含Ti的金属硼化物(B)(也可以为复合硼化物)和仅包含Ti的金属硼化物(A)。在该情况下，促进cBN粒子与结合相的反应而使结合变得牢固，从而cBN烧结体的韧性得到提高。
(3)不包含Ti的金属硼化物粒子
当将金属硼化物中仅包含Ti作为金属成分的金属硼化物(A)的比例(体积％)设为Va且将包含Nb、Ta、Cr、Mo及W中的至少一种作为金属成分且不包含Ti的金属硼化物(B)的比例(体积％)设为Vb时，优选它们的比Vb/Va满足0.1～1.0。当比Vb/Va小于0.1时，不包含Ti的金属硼化物(B)的量不足，无法充分得到cBN粒子与结合相的反应促进效果。另一方面，若比Vb/Va超过1.0，则与得到反应促进效果所需要的量相比，不包含Ti的金属硼化物(B)会过剩地存在，无法得到作为cBN烧结体的硬度和韧性。
金属硼化物的含有比例能够以如下方式求出。首先，使用AES得到金属元素及硼元素的映射图像，通过图像处理提取金属元素及硼元素重叠的部位，将该部位确定为金属硼化物粒子。接着，通过图像分析计算出金属硼化物粒子所占的面积来求出金属硼化物粒子的面积比例。对至少3个图像进行该处理，求出所计算出的各金属硼化物粒子的面积比例的平均值来作为在cBN烧结体中所占的金属硼化物的含有比例。作为图像处理中使用的观察区域，例如优选8.0μm×8.0μm的视场区域。
当将包含所述Nb、Ta、Cr、Mo及W中的至少一种且不包含Ti的金属硼化物(B)中六方晶结构的金属硼化物的{001}面的X射线衍射峰的最大强度设为Ihex、且将cBN粒子的{111}面的X射线衍射峰强度设为IcBN时，优选为0.04≤Ihex/IcBN≤0.20。X射线衍射峰强度使用Cu-Kα射线来进行测定。
若将不包含Ti但包含所述金属元素的金属硼化物(B)中尤其具有六方晶结构的金属硼化物分散于结合相中，则促进cBN粒子与结合相的反应。另一方面，当Ihex/IcBN小于0.04时，不包含Ti但包含所述金属元素的金属硼化物(B)不足，无法充分得到cBN粒子与结合相的反应促进效果。当Ihex/IcBN超过0.20时，cBN与结合相过度反应而进行cBN的分解，因此金属硼化物相对于cBN过剩地存在，从而无法得到作为cBN烧结体的强度、韧性。
3.cBN粒子的含有比例
在本发明中，在cBN烧结体中所占的cBN粒子的含有比例并不受特别限定，但优选为cBN烧结体整体的40～80体积％。当cBN粒子的含有比例小于40体积％时，在烧结体中硬质物质少，当用作工具时，有时耐缺损性会下降。另一方面，若cBN粒子的含有比例超过80体积％，则在烧结体中生成作为裂纹起点的空隙，有时耐缺损性会下降。因此，为了更进一步可靠地发挥本发明所起到的效果，在cBN烧结体中所占的cBN粒子的含有比例优选设在40～80体积％的范围内。
当将所有的cBN粒子的含有比例设为100体积％时，优选平均粒径小于2μm的cBN粒子为5～40体积％，平均粒径为2μm以上且小于8μm的cBN粒子为60～95体积％。
将平均粒径小于2μm的cBN粒子设在所述范围内的原因是因为，当小于5体积％时，基于微粒cBN的分散的耐裂纹扩展性不充分，耐缺损性下降，若超过40体积％，则粗粒cBN不足，耐磨性下降。并且，将平均粒径为2μm以上且小于8μm的cBN粒子设在所述范围内的原因是因为，当小于60体积％时，粗粒cBN不足，耐磨性下降，若超过95体积％，则微粒cBN的分散作用不充分，耐缺损性下降。
cBN粒子的平均粒径和含有比例能够以如下方式求出。
(1)平均粒径
利用扫描型电子显微镜(Scanning Electron Microscope：以下称为SEM)观察cBN烧结体的截面组织，得到二次电子像。通过图像处理提取所得到的图像内的cBN粒子的部分，基于通过图像分析求出的各粒子的最大长度计算出平均粒径。
每次通过图像处理提取图像内的cBN粒子的部分时，为了明确地判断cBN粒子和结合相，以0为黑色、255为白色的256灰度的单色显示图像，使用cBN粒子部分的像素值与结合相部分的像素值之比成为2以上的像素值的图像，以cBN粒子成为黑色的方式进行二值化处理。
作为用于求出cBN粒子部分或结合相部分的像素值的区域，作为一例设为0.5μm×0.5μm的区域，优选将至少从同一图像内的不同的3个部位求出的平均值作为各自的对比度。
二值化处理后，进行将认为cBN粒子彼此接触的部分切离的处理，例如使用分水岭算法将认为接触的cBN粒子彼此分离。
对二值化处理后得到的图像内的相当于cBN粒子的部分(黑色部分)进行粒子分析，将求出的最大长度作为各粒子的直径。作为求出最大长度的粒子分析，例如从通过对一个cBN粒子计算出费雷特径而得到的两个长度中，将较大的长度的值作为最大长度，并将该值作为各粒子的直径。将假定为具有该直径的理想球体而通过计算求出的体积作为各粒子的体积来求出累计体积，基于该累计体积，将纵轴作为体积百分比[％]、横轴作为直径[μm]而描绘出图表，将体积百分比为50％时的直径作为cBN粒子的平均粒径，对3个观察区域进行该处理，将其平均值作为cBN的平均粒径[μm]。在进行粒子分析时，使用利用SEM可预先得知的标度值，设定好每个像素的长度(μm)。
(2)含有比例
关于在cBN烧结体中所占的cBN粒子的含有比例，利用SEM观察cBN烧结体的截面组织，通过图像处理提取所得到的二次电子像内的cBN粒子的部分，通过图像分析计算出cBN粒子所占的面积，求出一个图像内的cBN粒子所占的比例及粒度分布，对至少3个图像进行处理，将所求出的值的平均值作为cBN粒子的含有比例而求出。关于提取图像内的cBN粒子的部分的图像处理，以与得到cBN粒子的平均粒径的二值化处理后的图像的步骤相同的方式进行。
4.制造方法
以下示出本发明的制造方法的一例。
(1)构成结合相的成分的原料粉末的准备
作为构成结合相的原料粉末，准备Nb硼化物、Ta硼化物、Cr硼化物、Mo硼化物、W硼化物中的至少一种和Ti硼化物(以下，统称为金属硼化物)各自的粉末和成为结合相的主体的原料的粉末。为了制成粉碎成所期望的粒径的金属硼化物的原料粉末，例如与硬质合金制球和丙酮共同填充于用硬质合金作内衬的容器内，盖上盖之后，利用球磨机进行粉碎之后，使用离心分离装置进行分级，由此得到将纵轴作为体积百分比、横轴作为粒径时的中值粒径D50作为粉碎的金属硼化物的原料粉末的平均粒径时其值为20～300nm的金属硼化物的原料粉末。并且，作为成为结合相的主体的原料粉末，准备以往已知的结合相的形成原料粉末(例如，TiN粉末、TiC粉末、TiCN粉末、TiAl3粉末)。
(2)粉碎/混合
将这些原料粉末例如与硬质合金制球和丙酮共同填充于用硬质合金作内衬的容器内，盖上盖之后，利用球磨机进行粉碎及混合。
然后，将作为硬质相发挥作用的平均粒径0.2～8.0μm的cBN粉末以烧结后的cBN粒子的含有比例成为规定的体积％的方式进行添加，进而，进行球磨机混合。
(3)成型、烧结
将所得到的烧结体原料粉末以规定压力进行成型而制作成型体，将其在真空下、在1000℃预烧结，然后装入超高压烧结装置中，例如在压力：4～6GPa、温度：1200～1600℃的范围内的规定温度下进行烧结，由此制作本发明的cBN烧结体。
5.CBN工具
具备将如此制作的本发明的韧性优异的cBN烧结体作为工具基体的cBN基超高压烧结体的切削工具，其耐崩刀性、耐缺损性优异，在长期使用中发挥优异的耐磨性。
实施例
在本实施例的cBN烧结体的制造中，作为用于构成结合相的原料粉末，准备Ta硼化物、Cr硼化物、Nb硼化物、Mo硼化物、W硼化物中的至少一种和Ti硼化物的粉末，为了控制粒径，利用球磨机实施粉碎处理之后，使用离心分离法进行分级，由此准备了所期望的粒径范围的各金属硼化物的原料粉末。
即，将所述各金属硼化物的原料粉末与硬质合金制球和丙酮共同填充于用硬质合金作内衬的容器内，盖上盖之后，使用球磨机实施粉碎之后，使混合的浆料干燥之后，使用离心分离装置进行分级，由此得到了平均粒径为20～300nm的各金属硼化物的原料粉末。
准备了如上所述那样事先准备的各金属硼化物的原料粉末和平均粒径为0.02μm～0.5μm的TiN粉末、TiC粉末、TiCN粉末、TiAl3粉末。配合从这些原料粉末中选择的几种结合相构成用原料粉末和作为硬质相用原料的cBN粉末，并进行了湿式混合及干燥。在表1中示出各原料粉末配合组成的体积％，在表2中示出将该配合中的哪一个用作了本发明烧结体和比较例烧结体的硼化物原料以外的结合相原料。
接着，将所得到的烧结体原料粉末以成型压力1MPa冲压成型为直径：50mm×厚度：1.5mm的尺寸。接着，将该成型体在压力：1Pa以下的真空气氛中保持在1000℃的规定温度并进行预烧结，然后装入超高压烧结装置中，在压力：5GPa、表3所示的温度：1200～1600℃的温度下进行烧结，由此制作出表4所示的本发明的cBN烧结体1～9(称为本发明烧结体1～9)。
为了比较在本发明中规定的范围以外的Vb/Va比、Ihex/IcBN的情况，使用表2所示的硼化物原料以外的结合相原料，在表3所示的温度下进行了烧结。改变各金属硼化物的添加量、超高压烧结温度而制作出表4所示的比较例的cBN烧结体(以下，称为比较例烧结体)1’～6’。
[表1]
Figure BDA0003221957430000081
(注)“-”表示不包含。
[表2]
Figure BDA0003221957430000082
[表3]
Figure BDA0003221957430000091
[表4]
Figure BDA0003221957430000092
(注1)“-”表示不包含。
(注2)cBN粒子的大小为平均粒径。
在表4中，作为Ti以外的金属硼化物的金属成分而记载有多个金属元素的表示存在具有所记载的金属元素的复合硼化物。
接着，用线割电火花加工机将本发明烧结体1～9、比较例烧结体1’～6’切割为规定尺寸而得到了试验片。另一方面，准备了组成为Co：5质量％、TaC：5质量％、剩余：WC且具有ISO标准CNGA120408的刀片形状的WC基硬质合金制刀片主体。使用钎料将所述试验片钎焊于该WC基硬质合金制刀片主体的钎焊部(角部)。作为钎料，使用了具有由Cu：26质量％、Ti：5质量％、剩余：Ag构成的组成的Ag合金的钎料。通过对所得到的刀片实施上下表面及外周的研磨、珩磨处理来制造出具有ISO标准的CNGA120408的刀片形状的本发明的cBN基超高压烧结体切削工具(称为本发明工具)1～9及比较例的cBN基超高压烧结体切削工具(称为比较例工具)1’～6’。
接着，对本发明工具1～9和比较例工具1’～6’在以下的切削条件下实施切削加工而测定了发生缺损为止的工具寿命(断续次数)。
＜干式切削条件＞
工件材料：渗碳淬火钢(JIS·SCR420，硬度：HRC58～62)的沿长度方向形成有等间隔的纵槽的圆棒
切削速度：250m/min、
切深量：0.15mm、
进给速度：0.1mm/rev。
将各工具的刀尖发生崩刀或缺损为止的断续次数作为工具寿命，断续次数每2000次时观察刀尖，确认了有无刀尖的缺损或崩刀。在表5中示出所述切削加工试验的结果。
[表5]
Figure BDA0003221957430000101
根据表5所示的结果可知，本发明工具1～9没有发生突发性的刀尖的缺损、崩刀，工具寿命明显地延长化，且韧性得到了提高。另一方面，具备不满足一个以上的本发明的必要特征的cBN基超高压烧结体的比较例工具1’～6’的工具寿命较短。
产业上的可利用性
本发明的韧性优异的cBN烧结体的韧性高，若用作CBN工具的工具基体，则不会发生缺损、破损，在长期使用中发挥优异的耐缺损性，从而能够实现工具寿命的延长化。因此，本发明能够充分满足对应切削加工装置的高性能化、以及切削加工的省力化及节能化、低成本化，因此能够在产业上利用。

Claims (4)

1.一种cBN基超高压烧结体，其含有cBN粒子和结合相，其中，
所述结合相包含Al的氮化物或氧化物、或Ti的氮化物或碳化物或碳氮化物中的至少一种，且分散有0.1～5.0体积％的平均粒径为20～300nm的金属硼化物，
所述金属硼化物含有：金属硼化物B，金属成分包含Nb、Ta、Cr、Mo及W中的至少一种且不包含Ti；和金属硼化物A，金属成分仅包含Ti，
在所述金属硼化物中，当将仅包含Ti作为金属成分的所述金属硼化物A的比例设为Va、且将包含Nb、Ta、Cr、Mo及W中的至少一种作为金属成分且不包含Ti的所述金属硼化物B的比例设为Vb时，比Vb/Va为0.1～1.0，
其中，所述比例为体积％。
2.根据权利要求1所述的cBN基超高压烧结体，其中，
当将包含Nb、Ta、Cr、Mo及W中的至少一种作为金属成分且不包含Ti的所述金属硼化物中六方晶结构的金属硼化物的{001}面的X射线衍射峰的最大强度设为Ihex、且将所述cBN粒子的{111}面的X射线衍射峰强度设为IcBN时，0.04≤Ihex/IcBN≤0.20。
3.根据权利要求1或2所述的cBN基超高压烧结体，其中，
所述cBN基超高压烧结体中的所述cBN粒子的含有比例为40～80体积％，当将所有的所述cBN粒子的含有比例设为100体积％时，平均粒径小于2μm的cBN粒子的含有比例为5～40体积％，平均粒径为2μm以上且小于8μm的cBN粒子的含有比例为60～95体积％。
4.一种切削工具，其具备权利要求1至3中任一项所述的cBN基超高压烧结体。
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