CN1110581C - 用于加工铸铁的改进的硬质合金体 - Google Patents
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Abstract
本发明提供了一种经改进的、用于切削铸铁的、带涂层的硬质合金镶嵌件。该镶嵌件在基体和α-Al2O3涂层之间有多层TiCN层。最内部的TiCN层由大的柱状晶粒组成,而最外部的由小的等轴晶粒组成。
Description
在US 5137774中揭示了用α-Al2O3作为硬质合金镶嵌件上的涂层,在车削铸铁时与κ-Al2O3相比性能有所改进。此外,在US 5635247和5700569和US申请序号08/962683(代理人案卷号:024444-370)中,描述了多种涂覆氧化铝的硬质合金镶嵌件,其中氧化铝沉积在Ti(C,N)层或多层上。但是在本发明人所做的试验中,注意到当用镶嵌件车削铸铁时,α-Al2O3层与下面的TiCN层的粘附以及TiCN层与硬质合金基体的粘附经常不能令人满意。由于刃口碎屑导致磨损加速使涂层失败。
从这些试验中,本发明人已经确定出刃口碎屑的主要原因为基体-涂层间的粘附以及TiCN和α-Al2O3之间的粘附脆弱。
Vuorinen等人在“TiC/硬质合金界面的微观结构和结晶的TEM研究”(硬质材料科学,1983,433-447页)中,对有6μm厚CVD沉积的TiC层的TiC-硬质合金界面作了研究。用透射式电子显微镜(TEM)发现TiC层由两个区域组成。靠近基体、延伸厚度为1.5-2μm的是一层微细的等轴TiC晶粒层。其上是一层较大晶粒(典型地为2-4μm)的TiC层。
在“固体薄膜”,232(1993),73-82页登载的Vuorinen等人的另一项研究,题目为“硬质合金上化学蒸汽沉积的碳化钛的界面特征”中,TiC涂层在非渗碳条件下CVD-沉积在硬质合金基体上。在没有η-碳化物的情况下,发现TiC成核并在{0001}-和{1010}-WC面上外延生长。
由于用具有α-Al2O3外层的带涂层硬质合金镶嵌件进行铸铁的车削加工时性能提高,有关镶嵌件的可接受性的研究还在继续。
本发明的目的是避免或减轻现有技术的缺陷。
本发明进一步的目的是提供一种改进的带涂层硬质合金镶嵌件,它有氧化铝涂层,具有可接受的寿命,用于切削铸铁。
本发明的一个方面是一种带涂层的硬质合金体,包括硬质合金基体、多层Ti(C,N)中间层和Al2O3外层,其中Ti(C,N)中间层包括第一柱状晶粒Ti(C,N)内层和第二等轴晶粒Ti(C,N)外层。
本发明的另一方面是一种带涂层的硬质合金体,包括其上顺序排列有一系列涂层的硬质合金基体,所述涂层从基体开始顺序为:
(a)选自TiC、TiN和Ti(C,N)的、最厚为1μm的粘合层;
(b)多层TiCN层,包括第一柱状晶粒Ti(C,N)内层,晶粒的宽度(W)为涂层厚度的0.1-0.15倍,长度(L)为涂层厚度的0.5-0.8倍,和第二等轴晶粒外层,晶粒大小为0.2-1.0μm,Ti(C,N)层的总厚度在用于铣削加工时为3-5μm,在用于车削时为5-10μm;
(c)厚度为约0.5-3μm的(TiAl)(CO)层;
(d)厚度为约4-10μm的α-Al2O3层;和
(e)厚度为约1μm或更薄的TiN外层。
图1是本发明带涂层的硬质合金镶嵌件的一个角的截面示意图。
图2是本发明涂层的TEM显微图。
图3A和3B是现有技术和本发明的镶嵌件在车削试验后切削刃口的放大40倍的SEM显微图(二次电子成像)。
图4A和4B是现有技术和本发明的镶嵌件在铣削试验后切削刃口的放大29倍的SEM显微图。
硬质合金中主要的相是WC和富Co的粘合剂相。可以选择性地加入第三相—立方体过渡金属碳化物相(Ti,Ta,Nb,W,C),通常称之为γ相,以便改进直接WC-Co合金的耐磨性。在许多工业用硬质合金中WC是主要的成分。WC具有简单的六角晶体结构,每个单元两个原子:W在(0,0,0),C在(2/3,1/3,1/2)。
作为液相烧结的结果,WC的基本平衡形式为由三个{1010}和两个{1000}面限制的三角形晶粒。于是基体-涂层的界面由以下界面组成:
涂层-WC
涂层-Co
涂层-γ(当有的时候)
涂层-η(当形成的时候)
内部TEM观察显示出TiCN和TiN涂层在WC晶粒界面上外延生长,正如也可以使用的TiC一样。如此形成的外延生长的涂层-WC之间的界面成为主要的,对第一涂层与硬质合金基体的良好粘附起作用。当涂覆操作之前对基体进行了化学清洗时尤其是这样。但由于η相反应可逆,如下所述,这一情形较为复杂。
相对于合金的C含量来说,WC-Co硬质合金的两相区(或WC-Co-γ的三相区)非常窄,C-含量的微小变化会导致形成三相区合金(或WC-Co-γ四相区合金),C含量降低时形成η-碳化物。参见,例如,上述“固体薄膜”文献第74页图1。当用常规CVD技术施加Ti(C和/或N)涂层时,形成TiC和/或TiCN或TiN(低压下)的碳部分得自于基体,从而使基体脱碳。于是基体的外部转变成η-相的M12C型。至少是在带涂层镶嵌件的刃口经常形成此η-相(即使是非常薄的)(在脱碳程度最高时表面-体积比最高)。
要强调的是此η-相反应是可逆的,特别在比较薄和涂覆在碳含量较高的基体上的时候。在退火过程中,此η-相将转变回富Co合金和WC。由上可知,这一情况在切削的刃口非常显著。
对于铸铁来说,4-6μm的较厚的α-Al2O3层是优选使用的。氧化铝层施加在TiCN层上面。在氧化铝层沉积的过程中,基体-TiCN界面经受长达6小时的热处理。在氧化铝层沉积的过程中,在基体-涂层界面上将发生可逆的η-碳化物反应,使TiCN层和硬质合金基体之间形成一层富Co层。当η-相的形成被限于靠近基体表面的区域时尤其是这样,如同采用现代CVD法的情况。结果,外延的TiCN-WC界面将被涂层-Co界面代替,使得粘附程度下降。
为了避免这一情况,第一TiCN层必须在基体不脱碳的情况下沉积。这一涂层是用CH3CN和CH4气作为前体沉积的。结果形成具有柱状晶粒结构的涂层。柱状晶粒的宽度为涂层厚度的0.1-0.5倍(就是说,一般宽度为0.3-1.5μm),长度接近涂层的厚度,优选为涂层厚度的0.5-0.8倍(就是说,一般长度为1.5-8.0μm)。为了使外延界面量最佳并确保在界面处有良好的粘附,操作应开始于不用CH3CN沉积第一层TiCN、TiC或TiN层,过程要非常短,形成厚度最大为1μm,优选最厚约0.5μm的层。钨将扩散到此界面层。这一内部扩散降低了涂层-WC界面的不适合,对良好粘附来说是重要的。
但即使在加粘合层的情况下,所得的柱状TiCN层与氧化铝层的粘附也不理想。为了改进粘附状况,在柱状TiCN晶粒涂层的上面加上一层由等轴晶粒组成的CVD TiCN层。等轴晶粒的粒径为0.2-1.0μm,优选0.3-0.5μm。在此等轴晶粒层上面可以成功地加上一层粘合层使粘结情况明显改进。整个TiCN层由柱状和等轴晶粒的TiCN层组成,如图2的TEM显微图清楚示意。
粘合层是含有Al的Ti(CO)立方体层。重要的是控制该粘合层使粘合层-氧化铝界面处获得晶须状的形态。此层的正确化学和微观构造是通过调节前体的TiCl4和AlCl3的量来控制的。在正确的比例下,晶须生长,粘合层中可发现多达10%的Al。
硬质合金镶嵌件上的整个涂层包括下面各层(图1):
1、由直接沉积在化学清洗过的、突出的WC晶粒占优势的基体上的TiC、TiCN或TiN组成的CVD粘合层1。此种基体也可以根据已知的技术通过改性烧结法获得。该层的特征是W在该层中发生扩散,并且具有外延涂层-WC界面。外延的方向关系如下:
在{0001}WC面:
(111)TiCN//(0001)WC;[110]TiCN//[1120]WC
在{1010}WC面:
(001)TiCN//(1010)WC;[110]TiCN//[0001]WC
外延界面决定了基体-涂层界面间的良好粘附,这在车削/铣削铸铁时特别重要。
此粘合层的厚度应不大于1μm,优选不大于约0.5μm。
2、CVD沉积的柱状晶体TiCN涂层2。这一层用CH3CN和CH4作为前体在MTCVD(中间温度CVD)条件下沉积。沉积温度为约800℃-900℃,优选约840℃-860℃。基体的脱碳被避免了,没有η-碳化物形成,并且排除了可逆η-碳化物反应的可能性。保护了步骤1中产生的外延界面。应当指出此层2还能够直接加在有外延的硬质合金基体上,并且粘附良好。但没有CH3CN的粘合(在更高温下)可以得到更好的粘附状况,在WC晶粒上有更显著的外延生长。
3、在TiCN之间可以选择性地加TiN层3。
4、由等轴结晶组成的CVD TiCN层4,沉积在由柱状结晶组成的MTCVD层上面。
层2和4的总厚度为5-10μm,优选6-8μm。柱状TiCN层的厚度为2μm到TiCN层(层2和4)总厚度的90%,根据基体的碳含量而定。
5、由立方体(TiAl)(CO)组成的粘合层5。此层的厚度为0.5-3.0μm,优选约1.5μm。由于此层中的铝含量高,具有晶须状的生长。
6、α-Al2O3涂层6,其厚度对于车削来说为4-10μm,优选约6μm,对于铣削来说为1-4μm,优选约2μm。
7、厚度≤1μm的TiN顶层。
下面结合实施例进一步描述本发明。但应理解实施例仅是例子,本发明并不限于实施例的具体细节。
实施例1
按现有技术制备两个试样:
(1)-TiCN CVD层,厚6μm
-粘合层
-α+κ氧化铝层,厚6μm
(2)-TiCN MTCVD层,厚6μm
-根据现有技术的粘合层
-κ氧化铝层,厚6μm
和两个根据本发明的涂层:
(3)-有外延的CVD粘合层
-4μm厚的柱状晶粒TiCN MTCVD层,用CH3CN和
CH4沉积,晶粒宽约0.5μm、长2.5μm,
-2μm厚的等轴晶粒TiCN CVD层,粒径约0.5μm
-粘合层
-6μm厚的α-Al2O3层
(4)-有外延的CVD粘合层
-4μm厚的柱状晶粒TiCN MTCVD层,用CH3CN和
CH4沉积,晶粒宽约0.5μm、长2.5μm
-选择性的TiN层
-2μm厚的等轴晶粒TiCN CVD层,粒径约0.5μm
-粘合层
-6μm厚的α-Al2O3层
所有的涂层有相同的TiCN和氧化铝层厚度(6μm+6μm)。在刮痕粘附试验仪中将镶嵌件进行比较。用带有声音发射检验仪(acoustic emission detertor)(AE)的刮痕粘附试验仪(Revetest,LSRH提供)进行刮痕粘附试验。用AE信号记录临界负载并进一步用SEM证实。使用一个新的钻石唱针,在每次试验后检查它的状况。结果概括在表1。
表1
试样 | 氧化铝相 | 刮痕粘附 |
1 | κ | ≤60 |
2 | κ(+α) | ≤60 |
3(根据本发明) | α | ≥90 |
4(根据本发明) | α | ≥90 |
本发明试样的粘附性能明显增强,涂层由100%α-Al2O3组成。
实施例2
将实施例1的试样1-4在铸铁中进行切削试验。切削参数如下:
操作: 车削
材料: 铸铁,SS0130
切削速度:450m/min
切削深度:3.0mm
进料速度:0.3mm/转
镶嵌件几何形状:SNUN 120408
未使用冷却剂
镶嵌件的刃口碎屑和寿命列于表2。本发明制备的镶嵌件比现有技术的优异。
表2
实施例3
试样 | 2分钟后的刃口碎屑% | 5分钟后的刃口碎屑% | 寿命(分钟) |
1 | 60 | >90 | 5 |
2 | 60 | >90 | 7 |
3 | 0 | <10 | 15 |
4 | 0 | <10 | 17 |
将实施例1和2讨论的镶嵌件1和4在铸铁中按实施例1给出的数据进行车削试验,除了切削速度要高一些,为550m/min。
从图3A和3B分别示意的镶嵌件1和4在车削5分钟后的SEM显微图可以看出,本发明的镶嵌件碎屑的倾向明显降低。
实施例4
用透射式电子显微镜(TEM)研究本发明制备的涂层——实施例1中的涂层4。涂层截面的微观结构如图2所示。TiCN层明显地由本发明的两个不同的层组成。可以看到沉积在较厚(最大1μm)粘合层上的α-Al2O3层。在基体—涂层界面上还可看到一些WC晶粒。用TEM证实了WC-TiCN界面的外延关系。
实施例5
将按本发明沉积的涂层用于铣削。除了涂层厚度之外,沉积的过程与实施例1中的涂层4相同。
-有外延和从基体扩散的W的TiCN粘合层
-4μm厚的柱状晶粒TiCN层,用CH3CN和CH4沉积,晶粒宽
约0.5μm、长2.5μm
-TiN层(选择性的)
-2μm厚的等轴晶粒TiCN CVD层,粒径约0.5μm
-TiCO粘合层+氧化铝
-2μm厚的α-Al2O3层
将该涂层与如下的按现有技术制备的相同厚度的涂层进行对比。
-厚度4μm的等轴晶粒CVD TiCN层,粒径0.7μm
-现有技术的粘合层
-α+κ氧化铝,2μm
铣削数据:
操作: 表面铣削
切削速度:300m/min
每齿进料:0.15mm/齿
切削深度:2.5mm
切削宽度:70mm
镶嵌件几何形状:SEKN 1203AFTN
未使用冷却剂
在铣削2400mm深后检查镶嵌件。从SEM显微图图4A和4B可以看出,本发明制备的镶嵌件的刃口碎屑明显降低。此镶嵌件的寿命比现有技术长约35%。
使用的所有基体均是可商购的硬质合金,WC-6%(重量)Co,硬度约HV 1600。
作为原则,前文说明书已经描述了本发明的优选实施方案和模式。但本发明在这里试图被保护的并不限于所公开的具体形式,因为这些应被看作是举例说明而不是限制。在不偏离本发明精神的情况下本领域技术人员可以进行改变。
Claims (15)
1、一种带涂层的硬质合金体,包括硬质合金基体,多层的Ti(C,N)中间层和Al2O3外层,其特征在于,所述的Ti(C,N)中间层包括第一柱状晶粒Ti(C,N)内层和第二等轴晶粒Ti(C,N)外层,并且在第一和第二Ti(C,N)层之间有一TiN层。
2、权利要求1的带涂层的硬质合金体,其中在基体和第一柱状晶粒Ti(C,N)内层之间有一层选自TiC、TiN和Ti(C,N)的粘合层。
3、权利要求1的带涂层的硬质合金体,其中Ti(C,N)中间层的总厚度为5-10μm。
4、权利要求3的带涂层的硬质合金体,其中柱状层的厚度为2μm到Ti(C,N)中间层总厚度的90%。
5、权利要求1的带涂层的硬质合金体,其中在Ti(C,N)层和Al2O3层之间有一(TiAl)(CO)层。
6、权利要求5的带涂层的硬质合金体,其中(TiA1)(CO)层的厚度为约0.5-3μm。
7、权利要求1的带涂层的硬质合金体,其中的Al2O3层厚度为约4-10μm。
8、权利要求7的带涂层的硬质合金体,其中的Al2O3是α-Al2O3。
9、权利要求1的带涂层的硬质合金体,其中在Al2O3层上有一TiN层。
10、权利要求9的带涂层的硬质合金体,其中TiN层厚度为约1μm或更薄。
11、权利要求1的带涂层的硬质合金体,其中所述的柱状晶粒Ti(C,N)的宽度为涂层厚度的0.1-0.5倍,长度为涂层厚度的0.5-0.8倍。
12、权利要求1的带涂层的硬质合金体,其中所述的等轴晶粒Ti(C,N)的粒径为0.2-1.0μm。
13、一种带涂层的硬质合金体,包括一硬质合金基体,其特征在于,在所述的基体上顺序排列有一系列涂层,所述涂层的顺序从基体开始为:
(a)选自TiC、TiN和Ti(C,N)的、厚度不大于1μm的粘合层;
(b)多层TiCN层,包括第一柱状晶粒Ti(C,N)内层,晶粒的宽度(W)为涂层厚度的0.1-0.5倍,长度(L)为涂层厚度的0.5-0.8倍,和第二等轴晶粒外层,晶粒大小为0.2-1.0μm,Ti(C,N)层的总厚度在用于铣削时为3-5μm,用于车削时为5-10μm;
(c)厚度为0.5-3μm的(TiAl)(CO)层;
(d)厚度为4-10μm的α-Al2O3层;和
(e)厚度为1μm或更薄的TiN外层。
14、权利要求13的带涂层的硬质合金体,其中等轴晶粒的粒径为0.3-0.5μm。
15、用带涂层的硬质合金镶嵌件切削铸铁的方法,其改进之处包括使用如权利要求1所述的硬质合金体作为镶嵌件。
Applications Claiming Priority (2)
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US09/207,688 | 1998-12-09 | ||
US09/207,688 US6251508B1 (en) | 1998-12-09 | 1998-12-09 | Grade for cast iron |
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CN1256183A CN1256183A (zh) | 2000-06-14 |
CN1110581C true CN1110581C (zh) | 2003-06-04 |
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US (1) | US6251508B1 (zh) |
EP (1) | EP1008673B1 (zh) |
JP (1) | JP2000234172A (zh) |
CN (1) | CN1110581C (zh) |
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