CN1112863A - 涂层刀具 - Google Patents

涂层刀具 Download PDF

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CN1112863A
CN1112863A CN95103073A CN95103073A CN1112863A CN 1112863 A CN1112863 A CN 1112863A CN 95103073 A CN95103073 A CN 95103073A CN 95103073 A CN95103073 A CN 95103073A CN 1112863 A CN1112863 A CN 1112863A
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安德斯·莱南德
莱夫·阿凯森
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Sandvik Intellectual Property AB
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Abstract

本发明涉及一种用于切屑形成机加工的CVD 工艺涂敷的硬质合金刀具，更特别地是，它涉及一种 具有中间涂层的涂层，该中间涂层起阻碍渗透的作 用，从而影响下一层涂膜的结构和粘附力。

Description

本发明涉及一种涂有非常耐磨溥表层的硬质合金刀体，更特别地是，它涉及这样的硬质合金刀体，其上的涂敷在碳化物层、氮化物层和（或）碳氮化物层之间的含氧溥层可改善涂层刀体的特性。
涂层刀片广泛使用于加工工业中，用它来加工铁和铁合金。借助碳化物、氮化物、碳氮化物或氧化物涂层，来延长刀具的寿命是一门完善的技术。刀具通常涂敷有由碳化物、氮化物、钛（Ti）或同类金属的碳氮化物组成的表层，许多情形中涂层包括一层或多层氧化铝，这种涂敷材料无法利用传统使用的化学气相沉积涂敷工艺（CVD）方便直接地涂覆于硬质合金基体上，所以，通常的作法是，先于三氧化二铝（Al2O3）的涂覆而覆盖一层碳化物、碳氮化物和（或）钛的氮化物。
当硬质合金基体在温度800-1200℃下借助CVD工艺涂覆一层碳化物、碳氮化物或氮化物耐磨涂层时，基体组元如钨、钴、碳将热渗透到不断增长的涂层中，从而影响晶体生长方向、显微结构和涂层结合力，同时涂层的物理、化学和机械特性也将由于基体渗出物的存在受到影响。
美国第5135801号专利揭示一种具有最深（离基体最近）含氧层的涂层硬质合金刀体。上述发明的目的是抑制碳渗进涂层，把上述含氧层如TiCO层直接使用于硬质合金基体上，使基体脱碳作用降至最低限度。
但是，本发明描述一种方法，在直接敷于基体的第一TiCxN1-x（0≤x≤1）层与敷于TiCO层上的另一TiCxN1-x（0≤x≤1）层之间，涂敷TiCO溥层作为中间层，用它来抑制物质由基体向涂膜的渗透。中间层同样可组成连续层。此外，在上述提及的碳氮化物、氮碳化合物组合层的上面，涂敷其它层，如Al2O3层，金属碳化物层和（或）金属氮化物层。
很意外地发现，上述TiCO或TiCON中间层可有效的抑制钴和钨由基体向涂层的扩散、大大地影响到显微结构和上述涂层的化学特性，从而引起涂层刀具抗磨性能显著提高。此外，钴渗透的抑制可借助减小涂层接合面处钴浓缩的有害作用来改善夹层涂层接合物中相邻涂层之间的粘附力。
图1所示为放大1600倍后的被研磨和腐蚀的涂层截面，按本发明，其中：
A：硬质合金
B：第一涂层（TiCN）
C：第二涂层（TiCO）
D：第三涂层（TiCN）
E：第四涂层（Al2O3）
图2所示为放大4000倍后的，与图1中名称相同的同一涂层的折断面。Met指的是钛（Ti）、锆（Zr）、铪（Hf）、钒（V）、铌（Nb）或钽（Ta）。
1.直接涂敷于硬质合金刀体上的第一MetCxN1-x（0≤x≤1）涂层。我们知道，第一层可由好几层MetCxN1-x（0≤x≤1）涂层组成，第一层最好由TiC组成。该层的厚度大于1但小于5μm，最好是在1.5-3μm之间。如果出现于硬质合金刀体上的表面粘结相在其沉积之前被清除，第一层的最小厚度可减小至0.5μm。粘合相可用喷沙法清除，但按WO 92/20841，最好用电解法来消除。
2.直接涂敷于第一MetCxN1-x（0≤x≤1）涂层上的第二MetCxOyNz涂层。本层厚0.1-5μm之间，最好在0.2-1μm之间，MetCxOyNz的组成结构是0.7≤x+y+z≤1.3，且0.2＜y＜0.8，最优值为0.4≤y≤0.6。最优地是，Met为Ti，且z=0。
3.直接涂敷于MetCxOyNz涂层上的第三Met CxN1-x（0≤x≤1）涂层。第三耐磨层的厚度为1-20μm，最优为5-12μm，本层由TiCxN1-x组成最佳，这里0.05＜x＜0.95，最优为0.3≤x≤0.7。与前～TiCN涂层比较，当其用于刀具时，本TiCN涂层显示出有所改善的耐磨性能，这主要是因为第三层具有较优晶向的缘故。按本发明，较佳地是，TiCN涂层在（220）方向上（由x光绕射（xRD）测量确定）具有较优的结晶生长方向。晶体结构系数TC，可确定为：
TC(hkl)= (I(hkl))/(I0(hkl)) { 1/(n) Σ (I(hkl))/(I0(hkl)) }-1
其中：
I（hkl）=（hkl）反射测量强度；
I0（hkl）=ASTM标准粉状绕射数据的标准强度，
n=用于计算中的反射数目，所使用的（hkl）反射是（111）、（200）、（220）。
按本发明，晶面（220）的晶体结构系数TC应大于1.3，大于1.5更佳，大于1.8最佳。
在上述碳氮化物、氧化物和碳氮化物层结合体的上部，可涂覆更多的涂层，如Al2O3涂层多种金属碳化物涂层和（或）氮化物涂层。更好地是，按瑞典专利申请9203852-0号，这些涂层包括成分为微粒α氧化铝的最外涂层，紧随其后的是TiN溥层，它在用喷沙法把氧化铝层光滑平整之后进行涂敷。
按本发明，涂层可涂敷于以纯WC-Co和WC-立方碳化物-Co为基本结构的硬质合金刀体上，这里的立方相位由碳化物或Ti、Ta、Nb的碳氮化物组成。按瑞典专利申请9203851-2和9200530-5号，涂层还可用于通常所说的有浓度梯度硬质合金中，这种硬质合金具有浓缩粘结相的表面区。
本发明同时涉及一种制造刀体的方法，该刀体包括具有涂层的硬质合金基体，涂层由下列几个涂层组成。
1.第一涂层或相邻于基体的MetCxN1-x（0≤x≤1）涂层。此处Met从Ti、Zr、Hf、V、Ta、Nb中选取，基体与含有氢、氮、碳氢化物和一种或多种上述金属卤化物的气体相接触，在压力为5-1050毫巴、最佳为30-100毫巴下，该涂层形成碳化物、氮化物或碳氮化物。
2.直接涂敷于第一层上的第二涂层，在处理压力为5-1050毫巴，最佳为30-100毫巴下，在含有氢、氮、一氧化碳和一种或多种上述金属卤化物的气体中进行MetCxOyNz涂敷，它形成碳氧化物或碳氮氧化物。
3.直接涂敷于第二层上的第三涂层，在处理压力为5-1050毫巴、最佳为200-600毫巴下，在含有氢、氮、碳氢化物和一种或多种上述金属卤化物的气体中进行MetCxN1-x（0≤x≤1）涂敷，它形成碳氮化物。
在一优选实施例中，外部氧化铝层在含有氢、二氧化碳和卤化铝的气体中，用气相沉积方法进行涂覆。最优地是，该氧化铝层是一种α一氧化铝层，它在含有氢、二氧化碳和卤化铝的气体中用气相沉积的方法进行涂覆。
最佳地是，TiN最外层，在含有氢、氮和卤化钛的气体中，用气相沉积的方法涂覆在氧化铝涂层上面。
CVD涂敷过程的操作温度可在800-1200℃之间，最佳温度是900-1070℃，不同的操作步骤可在同一或不同的涂层设备上完成。在第二MetCxOyNz涂层CVD处理阶段，根据含有氧元素气体母体的不同，可在该涂层中出现除氮、碳外的其它原子夹杂物，如硫（S）、碲（Te）、硒（Se）、磷（P）、和（或）砷（As）。
第一和第二涂层可用物理气相沉积（PVD）方法交替地进行涂覆。如活性磁控管溅射、离子渡、阴极电弧放电涂层等。
实例1
先于中间层TiCO涂敷（气体成分：4%TiCl4，7%CO，3%HCl，其余H2，压力50毫巴、基体温度1000℃），对具有成分为5.5%CO、8.6%立方碳化物（TiC-TaC-NbC）、其余为WC的硬质合金刀片CNMG120408涂覆TiC1小时，紧随TiCO层的涂敷，是在400毫巴压力下涂覆TiCN耐磨层4小时，接着是涂覆微粒α-Al2O3涂层6小时（根据瑞典专利申请9303852-0号）。（实例A）
上述所论实例A中所用硬质合金在涂敷工序前进附加电解面清洗作业。（例B）
如上所述，使用于例A和B中的硬质合金刀片用相同的CVD工艺进行处理，但不包括第二TiCO涂层。（例C）
用150号氧化铝细粒湿喷例A、B、C、以便使涂敷表面光滑平整，之后涂覆TiN溥层。喷砂处理与最外TiN涂层相结合，使刀片具有从被使用刀刃处易于辨别的闪亮表面。
可依据以下因素来检验涂层刀片：η相涂层的存在及其厚度（μm）、涂层厚度（μm），反映TiCN耐磨涂层（220）生长方向的晶体结构系数（TC）和Al2O3涂层晶体平均粒度（μm）。其结果如下：
η相                                                A                                                B                                                        C（先有技术）
                                                        微量                                        没有                                                0.5
Tic                                            1.5                                            0.7                                                    1.6
TiCO                                        0.4                                            0.4                                                    --
TiCN                                        7.0                                            7.0                                                    7.2
Al2O35.5 5.3 5.7
TiN                                            0.1                                            0.1                                                    0.1
晶体结构系数TiCN    2.0                                1.9                                                    1.2
粒度
Al2O3-层 1.9 1.7 1.7
实例2
先于含氧、氮中间层TiCON的涂敷（气体成分：4%TiCl4、7%CO，3%HCl，25%N2，其余为H2，压力为50毫巴，基体温度1000℃），具有成分为5.5%CO，8.6%立方碳化物（TiC-TaC-NbC），其余为WC的硬质合金刀片CNMG120408涂覆TiC1.5小时，紧随TiCON涂层的涂敷，是在600毫巴压力下，涂覆TiCN耐磨涂层4小时，接着再涂覆TiN涂层2小时。（例D）。
使用于变种D中的硬质合金刀片，用相同的CVD工艺进行处理，但不包括TiCON中间层。（例E）
依据η相涂层的存在及其厚度（μm）涂膜厚度（μm）、反映TiCN耐磨层（220）生长方向的晶体结构系数（TC）来检验涂层刀片，其结果如下：
η相                                                                D                                                        E（先有技术）
                                                                                    1.1                                                    1.7
Tic                                                                        1.9                                                    2.1
TiCON                                                                0.5                                                    --
TiCN                                                                    8.2                                                    8.5
TiN                                                                        1.6                                                    1.4
晶体结构系数TiCN                    1.8                                                    1.1
实例3
先于TiCO中间层的涂敷（生产气体成分：3%TiCl4、4%CO、4%HCl、其余为Hz，压力为100毫巴、基体温度1000℃），具有成分为6.5%CO，8.7%立方碳化物（TiC-TaC-NbC），其余为WC，且具有25μm厚的粘结相状浓缩表面区的硬质合金刀片CN-MG120408，涂覆TiC0.5小时，紧接着涂覆TiCN0.25小时。紧随中间涂层的涂敷，是在200毫巴压力下涂覆TiCN耐磨层4小时，接着是微粒αAl2O3涂层的涂敷（按瑞典专利申请9203852-0号），它需涂覆1小时。最上层TiN涂层涂覆1小时。（例F）
在涂敷工序之前对例F中的硬质合金刀片，进行附加电解面清理作业。（例G）
使用于例F和G中的硬质合金刀片，用同一CVD工艺进行处理，但不包括TiCO中间涂层。（例H）
依据η相层的存在及其厚度（μm）、涂层厚度（μm）、反映TiCN耐磨涂层（220）生长方向的晶体结构系数（TC）来检验涂层刀片。
η相                                                                    F                                                G                                            H（先有技术）
                                                                                0.7                                        微量                                1.0
TiC                                                                    1.2                                        0.3                                    1.4
TiCN                                                                0.3                                        0.2                                    0.4
TiCO                                                                0.4                                        0.4                                    －－
TiCN                                                                3.6                                        3.7                                    3.9
Al2O32.1 1.9 2.2
TiN                                                                    0.2                                        0.2                                    0.2
晶体结构系数TiCN                1.7                                        1.6                                    1.1
实例4
依据刀刃变形引起的涂层剥落，来测试例A-H涂层刀片，条件为：合金钢（AISI4340）沿纵向车削，进刀量为0.7mm/r，切削深度为2.0mm，同时改变切削速度，以便引起切削刃不同程度的塑性变形。依据测量刀刃凹陷的塑性变形，来检验刀刃，并用下述结果来估计随之产生的涂层剥落。
按本发明，在刀刃至少凹陷80μm时，刀片A、B、D、F、G没有发现任何剥落。
刀片C在刀刃下降了40μm时，后刀面上出现涂层连续损伤。
刀片E在刀刃下降了35μm时，后刀面上出现涂层连续损伤。
刀片H在刀刃下降了45μm时，后刀面上出现涂层连续损伤。
实例5
依据灰铸铁（AISI    No.35B）端面车削时前刀面的剥落、来测试实例1中的涂层刀片。被加工工件的形状应满足每转1周切削中断2次的要求。
切削数据：
速度=500m/min
走刀量=0.5mm/r
切削深度=3.0mm
依照位于刀片前刀面上氧化铝涂层的剥落，来检验刀片，其结果表示为：剥落的前刀面区域与切屑接触区域面积之比。
结果
表面剥落
刀片A（本发明）        0%
刀片B（本发明）        0%
刀片C（先前技术）        19%
实例6：
依据灰铸铁（AISI    No.35B）表面加工时前刀面的剥落，来检测涂层刀片。被加工工件的形状应满足每转1周切削中断2次的要求。
切削数据：
速度=400m/min
走刀量=0.3mm/r
切削深度=3.0mm
依据切削刀片前刀面上氧化铝层的剥落，来检验刀法，其结果可表示为：剥落的前刀面区域与前刀面上切屑接触区域面积之比。
结果：
表面剥落
刀片F（本发明）        0%
刀片G（本发明）        0%
刀片H（先前技术）        26%

Claims (15)

1、一种涂层硬质合金刀体，其特征在于，所述涂层包括第一涂层或相邻于基体的MetCxN1-x(0≤x≤1)金属涂层组，紧随第一层的是由MetCxOyNz组成的第二涂层(此处：0.7≤x+y+z≤1.3、且0.2＜y＜0.8，最佳值为0.04≤y≤0.6)，紧随第二层的是MetCxN1-x(0≤x≤1)耐磨涂层，此处金属Met选取于金属族Ti、Zr、Hf、V、Nb和Ta中，且第一涂层或涂层组MetCxN1-x(0≤x≤1)的厚度大于1μm，但小于5μm，或当基体不含表面钴(Co)时在0.5-5μm之间。
2、按权利要求1，涂层刀体的特征在于，第三MetCxN1-x（0≤x≤1）涂层厚度大于第一和第二涂层的总厚度。
3、按权利要求1或2，涂层刀体的特征在于，第二涂层厚度在0.1-0.5μm之间，最优厚度在0.2-1.0μm之间。
4、按上述任何权利要求，涂层刀体的特征在于，相邻于基体的第一MetCxN1-x（0≤x≤1）涂层或涂层组的厚度在1.3-3μm之间，或当基质不含表面钴时在0.5-2μm之间。
5、按权利要求3或4，涂层刀体的特征在于，第三MetCxN1-x（0≤x≤1）耐磨层的厚度小于20μm，最佳值在5-12μm之间。
6、按上述任何权利要求，涂层刀体的特征在于，第三MetCxN1-x（0≤x≤1）耐磨涂层由TiCxN1-x组成，此处，0.05≤x≤0.95，最优值为0.3≤x≤0.7。
7、按权利要求6，涂层刀体的特征在于，第三耐磨涂层最好在（220）方向上结晶生长，其晶体结构系数TC大于1.3，大于1.5更佳、大于1.8最佳。TC确定为：
TC(hkl)= (I(hkl))/(I0(hkl)) { 1/(n) Σ (I(hkl))/(I0(hkl)) }-1
这里：I（hkl）=hkl被测反射强度，
I0（hkl）=ASTM标准粉状绕射数据的标准强度，
n=用于计算中的反射数目，所使用的（hkl）反射是（111）、（200）、（220）。
8、按上述任何权利要求，涂层刀体的特征在于，所述涂层刀体包括一外部氧化铝涂层。
9、按权利要求8，涂层刀体的特征在于，氧化铝涂层由粒度为S的单相α氧化铝组成，其中0.5＜S＜3μm。
10、按权利要求8和9，涂层刀体的特征在于，所述刀体包括一最外TiN涂层。
11、按权利要求10，涂层刀体的特征在于，最外TiN涂层厚在0.01-1μm之间。
12、一种制造由硬质合金基体组成、具有涂层刀体的方法，其特征在于，它包括：
①第一涂层组或相邻于基体的MetCxN1-x（0≤x≤1）涂层组，这里Met从Ti、Zr、Hf、V、Ta、Nb中选取，基体与含有氢、氮、碳氢化物和一种或多种上述金属卤化物的气体相接触，在温度范围为800°-1200℃、最佳为900°-1070℃，且处理压力为5-1050毫巴、最优为30-100毫巴情况下，形成一种氮化物；
②第二涂层，它在含有氢、氮、一氧化碳和一种或多种上述金属卤化物的气体中直接涂敷MetCxOyNz于第一涂层上。这里0.7≤x+y+z≤1.3，且0.2＜y＜0.8，y的最佳值为0.4＜y＜0.6，它在温度范围为800-1200℃、最佳为900°-1070℃、处理压力为5-1050毫巴、最佳为30-100毫巴的条件下，形成一种碳氧化物或碳氮氧化物；
③第三涂层，它在含有氢、氮、氢碳化物和一种或多种上述金属卤化物气体中直接涂敷MetCxN1-x（0≤x≤1）于第二涂层上。在温度范围为800-1200℃，最佳为900-1070℃、处理压力为5-1050毫巴，最佳为200-600毫巴条件下，它形成一种碳氮化物。
13、按权利要求12，制造涂层刀体的方法，其特征在于，外部氧化铝涂层在含有氢、二氧化碳和卤化铝的气体中，用气相沉积的方法进行涂覆。
14、按权利要求12，制造涂层刀体的方法，其特征在于，一种外部α氧化铝涂层在含有氢、二氧化碳和卤化铝的气体中，用气相沉积的方法进行涂覆。
15、按权利要求13和14，制造涂层刀体的方法，其特征在于，一种最外层TiN涂层，在含有氢、氮和卤化钛的气体中用气相沉积的方法，涂覆于氧化铝涂层之上。
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US4399168A (en) * 1980-01-21 1983-08-16 Santrade Ltd. Method of preparing coated cemented carbide product
DE3114351A1 (de) * 1981-04-09 1982-11-04 Hoechst Ag, 6000 Frankfurt "oxindol-derivate, verfahren zu ihrer herstellung und sie enthaltende arzneimittel mit neuroanaboler wirkung"
IL63802A (en) * 1981-09-11 1984-10-31 Iscar Ltd Sintered hard metal products having a multi-layer wear-resistant coating
US4447263A (en) * 1981-12-22 1984-05-08 Mitsubishi Kinzoku Kabushiki Kaisha Blade member of cermet having surface reaction layer and process for producing same
JPS60238481A (ja) * 1984-05-14 1985-11-27 Sumitomo Electric Ind Ltd 多重層被覆超硬合金
JPS61223181A (ja) * 1985-03-29 1986-10-03 Mitsubishi Metal Corp 表面被覆炭化タングステン基超硬合金製切削工具
JPH0732961B2 (ja) * 1986-10-03 1995-04-12 三菱マテリアル株式会社 表面被覆炭化タングステン基超硬合金製切削工具
US5135801A (en) * 1988-06-13 1992-08-04 Sandvik Ab Diffusion barrier coating material
JPH0349834A (ja) * 1989-07-14 1991-03-04 Sumitomo Electric Ind Ltd 金を接合材とする工具及びその製造方法
JP3099834B2 (ja) * 1991-03-18 2000-10-16 三菱マテリアル株式会社 すぐれた靭性を有する表面被覆炭窒化チタン基サーメット製切削工具
SE9101469D0 (sv) * 1991-05-15 1991-05-15 Sandvik Ab Etsmetod
JP2867803B2 (ja) * 1992-06-25 1999-03-10 三菱マテリアル株式会社 耐チッピング性にすぐれた表面被覆炭化タングステン基超硬合金製切削工具
SE514737C2 (sv) * 1994-03-22 2001-04-09 Sandvik Ab Belagt skärverktyg av hårdmetall

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1829599B (zh) * 2003-02-27 2012-03-21 钴碳化钨硬质合金公司 涂覆碳化物丝锥
CN1997766B (zh) * 2004-05-19 2010-06-16 Tdy工业公司 具有扩散粘结增强层的三氧化二铝陶瓷工具
CN103476527A (zh) * 2011-04-22 2013-12-25 京瓷株式会社 切削工具
CN103476527B (zh) * 2011-04-22 2016-02-10 京瓷株式会社 切削工具
CN103826781A (zh) * 2011-09-22 2014-05-28 株式会社图格莱 被覆切削工具
CN104507859A (zh) * 2012-07-27 2015-04-08 韩化石油化学株式会社 多孔碳及其制备方法
US9428390B2 (en) 2012-07-27 2016-08-30 Hanwha Chemical Corporation Porous carbon and method of preparing the same
CN104703734A (zh) * 2012-10-01 2015-06-10 日立工具股份有限公司 硬质皮膜被覆工具及其制造方法
CN104703734B (zh) * 2012-10-01 2016-08-24 日立工具股份有限公司 硬质皮膜被覆工具及其制造方法
CN105828992A (zh) * 2013-12-26 2016-08-03 京瓷株式会社 切削工具

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RU2131328C1 (ru) 1999-06-10
US5800868A (en) 1998-09-01
RU95105176A (ru) 1996-12-27
KR950032707A (ko) 1995-12-22
SE514737C2 (sv) 2001-04-09
SE9400951L (sv) 1995-09-23
BR9501144A (pt) 1996-05-14
EP0678594A1 (en) 1995-10-25
JPH0847999A (ja) 1996-02-20
DE69509820T2 (de) 1999-09-23
ATE180518T1 (de) 1999-06-15
IL113067A0 (en) 1995-06-29
EP0678594B1 (en) 1999-05-26
DE69509820D1 (de) 1999-07-01
US5705263A (en) 1998-01-06
CN1060983C (zh) 2001-01-24
KR100348543B1 (ko) 2002-11-30
SE9400951D0 (sv) 1994-03-22

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