CN1456703A - 通过化学气相淀积产生的增强氧化铝层 - Google Patents

通过化学气相淀积产生的增强氧化铝层 Download PDF

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CN1456703A
CN1456703A CN03130958A CN03130958A CN1456703A CN 1456703 A CN1456703 A CN 1456703A CN 03130958 A CN03130958 A CN 03130958A CN 03130958 A CN03130958 A CN 03130958A CN 1456703 A CN1456703 A CN 1456703A
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萨卡里·鲁皮
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Abstract

本发明介绍了一种制作实质上比现有技术具有更好耐磨性和韧性的α－Al2O3层的新的改进方法。本发明的α－Al2O3层在(Ti，Al)(C，O，N)的粘结层上形成，所述的(Ti，Al)(C，O，N)粘结层的铝含量向着外表面增加。α－Al2O3的形核是通过由铝化和氧化步骤组成的形核步骤而得到的。根据本发明的α－Al2O3层厚度范围为1－20μm，由柱状颗粒构成。氧化铝颗粒的长/宽比为2－12，优选5－9。该层的特征在于通过XRD测定的强(012)生长织构，以及几乎完全不存在(104)、(110)、(113)和(116)衍射峰。

Description

通过化学气相淀积产生的增强氧化铝层
技术领域
本发明涉及用于金属加工的切削工具嵌入物，具有硬质合金、金属陶瓷或陶瓷衬底，上面淀积了硬耐磨被覆层。被覆层与衬底粘接并覆盖其所有零件。被覆层由一层或多层耐火材料层构成，其中至少一层为高度织构化的阿尔法-氧化铝(α-Al2O3)。
背景技术
淀积不同Al2O3多晶型物的关键步骤是形核步。κ-Al2O3可以受控的方式在具有fcc结构的TiN、Ti(C，N)或TiC的{111}面上生长。TEM确认了κ-Al2O3的密堆积(001)面在立体相的密堆积{111}面上的生长模式，存在以下外延取向关系：(001)κ//(111)Tix；[100]κ//[112]Tix。早先提出了亚稳κ-Al2O3的CVD(化学气相淀积)生长的解释和模型(Y.Yoursdshahyan，C.Ruberto，M.Halvarsson，V.Langer，S.Ruppi，U.Rolander和B.I.Lundqvist，一种复合材料的理论结构分析(TheoreticalStructure Determination of a Complex Material)：κ-Al2O3，J.Am.Ceram.Soc.82(6)(1999)1365-1380)。
当适当形核时，κ-Al2O3层可以生长到较大厚度(＞10μm)。通过在插入生长中的κ-Al2O3层的例如TiN的薄层上再形核，可以保证甚至更厚的κ-Al2O3层的生长。当确保形核时，通过使用相对低的淀积温度(＜1000℃)，可以避免淀积过程中的κ→α相变。在金属切削中，已确认有相变发生。除相稳定性外，在多数金属切削应用中应优选α-Al2O3层的原因还有几个。如早先所示，α-Al2O3在铸铁中表现出更好的耐磨性(US 5,137,774)。另外，以α-Al2O3形核的层不含任何相变裂缝和应力。因此，形核的α-Al2O3的延展性比完全或部分由于相变而形成的α-Al2O3的延展性强，甚至比κ-Al2O3的延展性强，κ-Al2O3的可塑性受到缺陷结构的限制。
但是，已发现稳定的α-Al2O3相比亚稳κ-Al2O3更难以形核，及更难以在适当的CVD温度下生长。如US 5,137,774所示，通过实验确认α-Al2O3可以在例如Ti2O3表面，(Ti，Al)(C，O)的粘结层上形核，或者如US 5,654,035所示，使用CO/CO2混合物，通过控制氧化电势可以使其形核。所有这些方法的要点是形核必须在TiC、TiN、Ti(C，N)或Ti(C，O，N)的111面上发生，否则会得到κ-Al2O3。
应该注意，在现有技术方法中，一般使用高淀积温度淀积α-Al2O3。当形核控制不完全时，就象许多现有技术产品的情形那样，生成的α-Al2O3层至少部分是由于κ-Al2O3→α-Al2O3相变而形成的。特别是考虑厚Al2O3层时。这些种类的α-Al2O3层由大颗粒构成，存在相变裂缝。这些覆层比由形核的α-Al2O3构成的α-Al2O3覆层具有更低的机械强度和延展性。
工业规模控制α-Al2O3多晶型物随二十世纪九十年代初基于美国专利5,137,774的商品的出现而得到实现。后来对该专利的改进用来淀积具有优选的被覆织构的α-Al2O3。在US 5,654,035中，公开了在(012)方向上织构的氧化铝层，在US 5,980,988中公开了在(110)方向上织构的氧化铝层。在US 5,863,640中，公开了沿(012)、或(104)或(110)的择优生长。US 6,333,103记载了控制α-Al2O3沿(10(10))方向形核和生长的改进方法。
发明内容
本发明的一个目的是提供新的改进的氧化铝层，其中α-Al2O3相由具有强的、充分控制的(112)生长织构的形核的α-Al2O3构成。
意外发现，具有强的、充分控制的(112)生长织构的α-Al2O3层优于现有技术的随机或其它织构如(011)。根据本发明的覆层基本上不存在相变应力，由位错密度低、切削能力提高的柱状α-Al2O3颗粒构成。
发现了一种控制α-Al2O3的形核步骤从而可以得到强(012)织构的方法。本发明的特征在于，主要存在(012)织构(TC)，同时不存在现有技术的覆层中通常发现的其它常见织构。
这种Al2O3层特别地被拟用于要求韧性的钢应用，如间歇切削、用冷却剂的车削，特别是使用冷却剂的间歇车削。其它领域是铸铁，在此这种氧化铝层的边缘强度(edge strength)优于现有技术。
在通过常规的CVD或MTCVD，优选MTCVD可以得到的Ti(C，N)覆层上淀积α-Al2O3之前，需要几个步骤。首先，在Ti(C，N)层上淀积US 5,137,774中记载的改进粘结层(在该专利中称为κ-粘结层)，其特征在于存在Al浓度梯度。另外，淀积该粘结层时应用氮气。该层表面上的铝含量比根据5,137,774的粘结层显著高出约30％，并且粘结层明显含有氮。为进一步增加铝含量，使用AlCl3/H2气体混合物对该粘结层的表面进行其它处理。之后，使用CO2/H2气体混合物进行小心控制的氧化处理。氧化步骤时间短，继之可以使用AlCl3/H2混合物进行短期处理，然后再次进行短期氧化步骤。这种脉动(Al-处理/氧化)处理将为α-Al2O3产生理想的形核位。在改进的粘结层的表面上生长氧化铝层通过将按下面的顺序排序反应气来开始：CO、AlCl3、CO2。温度应优选为约1000℃。
本发明还涉及由衬底构成的切削工具嵌入物，所述的衬底至少部分被覆有总厚度为10-40μm、优选15-25μm的覆层，该覆层由一个或多个耐火材料层构成，其中至少一层为α-Al2O3层。该α-Al2O3层密集且无缺陷。它由具有强(012)织构的柱状颗粒组成。柱状颗粒的长/宽比为2-12，优选5-9，宽度为0.5-2.5μm，优选0.5-1.0(s＝2-5μm)或1.5-2.5(s＝5-15μm)。S＝氧化铝层的总厚度。
根据本发明层的α-Al2O3的织构系数(TC)由下式确定： TC ( hkl ) = I ( hkl ) I 0 ( hkl ) { 1 n Σ I ( hkl ) I 0 ( hkl ) } - 1 式中
I(hkl)＝(hkl)反射的强度
I0(hkl)＝根据JCPDS卡号46-1212的标准强度
n＝计算使用的反射数目
使用的(hkl)反射为：(012)、(104)、(110)、(113)、(024)、(116)。
氧化铝层的织构定义如下：
TC(012)＞1.8，TC(024)＞1.8，优选2.5-3.5，并同时TC(104)、TC(110)、TC(113)、TC(116)＜0.4，优选＜0.3。
注意面012和024的强度是相关的。
衬底含有硬质材料，如硬质合金、金属陶瓷、陶瓷、高速钢或超硬材料如立方氮化硼(CBN)或金刚石，优选硬质合金或CBN。这里的CBN是指含有至少40体积％CBN的切削工具材料。在一个优选实施方案中，衬底为具有富含粘结相的表面区的硬质合金。
覆层含有与CVD Ti(C，N)、CVD TiN、CVD TiC、MTCVD Ti(C，N)、MTCVD Zr(C，N)、MTCVD Ti(B，C，N)、CVD HfN或它们的组合、优选Ti(C，N)的主体相邻，厚度为1-20μm、优选1-10μm的第一层，以及与所述的第一层相邻，厚度为约1-40μm、优选1-20μm、最优选1-10μm的α-Al2O3层。优选在衬底与所述的第一层之间存在一个TiN中间层，厚度为＜3μm、优选0.5-2μm。
在一个实施方案中，α-Al2O3层是最上层。
在另一个实施方案中，在α-Al2O3层上面存在一个Ti、Zr和Hf中一种或多种的碳化物、氮化物、碳氮化物或羧基氮化物层，厚度为约0.5-3μm、优选0.5-1.5μm。或者该层的厚度为约1-20μm、优选2-8μm。
在再一个实施方案中，被覆层包括一个优选位于α-Al2O3上面的κ-Al2O3和/或γ-Al2O3层，厚度为0.5-10μm、优选1-5μm。
具体实施方式实施例1
用MTCVD Ti(C，N)层被覆含有5.9％Co、余量为WC的硬质合金切削嵌入物(硬度约1600HV)。MTCVD层的厚度为约8μm。a)根据下面限定的本发明，和b)根据现有技术，在该层上淀积8μm的α-Al2O3。使用XRD对嵌入物进行了研究，并求得了织构系数。表2列出了根据本发明的被覆层和现有技术被覆层的织构系数。可以看出，根据本发明得到了强(012)织构。
表1
    Hkl   发明(覆层a)   现有技术(覆层b)
    012     2.79       0.72
    104     0.05       0.64
    110     0.19       1.63
    113     0.07       0.87
    024     3.26       1.16
    116     0.15       0.97
“被覆层a”(发明)的淀积工艺规定如下：
步骤1：MTCVD被覆
      气体混合物        TiCl4         ＝4.0％
                        CH3CN         ＝1.0％
                        N2            ＝20％
                        余量：          H2
      持续时间          250分
      温度              850℃
      压力              100毫巴
步骤2：粘结层
      气体混合物        TiCl4         ＝2.8％
                        AlCl3         ＝0.8-4.2％
                        CO             ＝5.8％
                        CO2           ＝2.2％
                        N2………            ＝5-6％
                        余量：          H2
      持续时间          60分
      温度              1000℃
      压力              100毫巴
步骤3：铝化步骤
      气体混合物        AlCl3          ＝0.8-4.2％
                        余量：           H2
      持续时间    15分钟或2分钟脉动
      温度              1000℃
      压力               50毫巴
步骤4：氧化步骤
        气体混合物     CO2          ＝0.1％
                       余量：         H2
        持续时间  2分钟或20秒脉动
        温度           1000℃
        压力           100毫巴
步骤5：形核步骤
        气体混合物     AlCl3       ＝3.2％
                       HCl          ＝2.0％
                       CO2         ＝1.9％
                       余量：        H2
        持续时间       60分
        温度           100℃
        压力           210毫巴
步骤6：淀积
        气体混合物     AlCl3       ＝4.2％
                       HCl          ＝1.0％
                       CO2         ＝2.1％
                       H2S         ＝0.2％
                       余量：        H2
        持续时间       420分
        温度           100℃
        压力           50毫巴实施例2
就纵向车削的边缘韧性对实施例1的被覆层a)和b)进行了试验。
工件：        圆柱条
材料：        SS0130
嵌入类型：    SNUN
切削速度：    400米/分
进料：        0.4mm/rev(一次旋转)
切削深度：    2.5mm
备注：        干车削
切削2分和4分钟后检查了嵌入物。从表2明显可以看出，当根据本发明制作被覆层时，现有技术产品的边缘韧性显著增强。
表2
2分钟后边缘线的剥落(％) 6分钟后边缘线的剥落(％)
被覆层a(发明)          0          ＜1
  被覆层b          38           62
实施例3
将根据本发明制作的被覆层与在此称为竞争者X(Competitor X)的市场主导品比较。该被覆层由MTCVD Ti(C，N)和α-Al2O3构成。用XRD求取这些竞争者被覆层的织构系数。为进行XRD，从竞争者X中随机选取两件嵌入物。表3列出了竞争者X的实测TC。竞争者X的被覆层显示(110)织构。表3
   Hkl     TC(hkl)
   012    0.64  0.59
   104    0.95  0.88
   110    1.75  2.00
   113    0.45  0.42
   024    1.15  1.10
   116    1.07  1.01
实施例4
来自竞争者X的嵌入物与根据本发明制作的具有相同的衬底组成、相同的被覆层结构的嵌入物作比较。试验前对根据本发明制作的两个嵌入物用X光检查。确认了强(012)织构。
将根据本发明制作的两个嵌入物与两个竞争者X嵌入物就滚珠轴承材料的面车削时的侧面耐磨性进行比较。
工件：        圆柱管(滚珠轴承)
材料：        SS2258
嵌入类型：    WNMG080416
切削速度：    500米/分
进料：        0.5mm/rev
切削深度：    1.0mm
备注：        干车削
工具寿命标准：  侧面磨损＞0.3mm，试验了各变体的三个边缘。
结果：        工具寿命(分)
被覆层1       22(发明)
被覆层2       23.5(发明)
竞争者1       15.5(现有技术)
竞争者2     13(现有技术)实施例5
根据本发明及根据实施例1中所述的现有技术被覆含有约90％多晶CBN(PCBN)的立方氮化硼(CBN)嵌入物。将被覆的CBN与未被覆的CBN嵌入物在切削含有铁氧体的钢时进行比较。已知B与铁氧化具有高亲合力，并且切削速度高时发生扩散磨损(diffusion wear)。
工件：        圆柱条
材料：        SS0130
嵌入类型：    SNUN
切削速度：    860米/分
进料：        0.4mm/rev
切削深度：    2.5mm
备注：        干车削结果
寿命时间(分)
被覆的CBN(发明)       22
根据现有技术被覆       14
未被覆的CBN       11

Claims (11)

1.一种切削工具嵌入物，由至少部分被总厚10-40μm、优选15-25μm的被覆层被覆的衬底构成，所述的被覆层由一个或多个耐火材料层构成，其中至少一层为氧化铝层，所述的切削工具嵌入物的特征在于，所述的氧化铝层由柱状α-Al2O3颗粒构成，所述的柱状α-Al2O3颗粒具有下面的织构系数：
a)TC(012)和TC(024)均大于1.8，优选为2.5-3.5，以及
b)TC(104)、TC(110)、TC(113)、TC(116)均小于0.4，优选小于0.3，
织构系数TC(hkl)的定义如下： TC ( hkl ) = I ( hkl ) I 0 ( hkl ) { 1 n Σ I ( hkl ) I 0 ( hkl ) } - 1 式中
I(hkl)＝(hkl)反射的实测强度，
I0(hkl)＝根据JCPDS卡号46-1212的标准强度
n＝计算使用的反射数目
使用的(hkl)反射为：(012)、(104)、(110)、(113)、(024)、(116)。
2.如权利要求1所述的切削工具嵌入物，其特征在于，所述的氧化铝层由长/宽比为2-12、优选5-9的柱状颗粒构成。
3.如前述任一项权利要求所述的切削工具嵌入物，其特征在于，所述的衬底含有硬质合金、CBN或烧结的CBN合金。
4.如前述任一项权利要求所述的切削工具嵌入物，其特征在于，被覆层包括与CVD Ti(C，N)、CVD TiN、CVD TiC、MTCVD Ti(C，N)、MTCVD Zr(C，N)、MTCVD Ti(B，C，N)、CVD HfN或它们的组合、优选Ti(C，N)的主体相邻，厚度为1-20μm、优选1-10μm的第一层，以及与所述的第一层相邻，厚度为约1-40μm、优选1-20μm、最优选1-10μm的所述α-Al2O3层。
5.如前述任一项权利要求所述的切削工具嵌入物，其特征在于，α-Al2O3层为最上层。
6.如前述任一项权利要求所述的切削工具嵌入物，其特征在于，在α-Al2O3层上面存在一个Ti、Zr和Hf中一种或多种的碳化物、氮化物、碳氮化物或羧基氮化物层，厚度为约0.5-3μm、优选0.5-1.5μm。
7.如权利要求1-6的任一项所述的切削工具嵌入物，其特征在于，在α-Al2O3层上面存在一个Ti、Zr和Hf中一种或多种的碳化物、氮化物、碳氮化物或羧基氮化物层，厚度为约1-20μm、优选2-8μm。
8.如前述任一项权利要求所述的切削工具嵌入物，其特征在于，在α-Al2O3上面存在一个κ-Al2O3或γ-Al2O3层，厚度为0.5-10μm、优选1-5μm。
9.如前述任一项权利要求所述的切削工具嵌入物，其特征在于，在衬底与所述的第一层之间存在一个TiN层，厚度为＜3μm、优选0.5-2μm。
10.如前述任一项权利要求所述的切削工具嵌入物，其特征在于，所述的衬底包括具有富含粘结相的表面区的硬质合金。
11.制作如权利要求1所述的α-Al2O3层的方法，其特征在于，所述的α-Al2O3的形核是通过用铝化和氧化步骤改进形核表面而得到的，并且所述的形核表面是(Ti，Al)(C，O，N)的一个粘结层，其铝含量向着形核表面增加。
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US7396581B2 (en) 2008-07-08
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US7163735B2 (en) 2007-01-16
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