CN103974922A - 陶瓷烧结体 - Google Patents
陶瓷烧结体 Download PDFInfo
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Abstract
本发明涉及一种陶瓷烧结体,其包含碳化钨、氧化锆和氧化铝。所述碳化钨的含量为20~50体积%,且所述氧化锆的含量为5~25体积%。所述氧化锆的晶相为正方晶或者正方晶与单斜晶的混晶。所述陶瓷烧结体实质上不含Ti化合物。所述碳化钨的平均粒径、所述氧化锆的平均粒径和所述氧化铝的平均粒径都为1μm以下。
Description
相关申请的交叉参考
本国际申请要求2012年6月28日在日本专利局提交的日本专利申请2012-145676号的权益,并通过参考将日本专利申请2012-145676号的完整内容并入本文中。
技术领域
本发明涉及能够用于例如切削工具等的陶瓷烧结体。
背景技术
耐热合金(heat resistant super alloys)具有优异的耐热性,而其非常难以加工。因此,要求用于切削耐热合金的工具具有高的物理性质和耐热性。包含碳化硅晶须(下文中称作SiC晶须)的氧化铝基材料具有高的硬度、韧度和耐热性,由这种材料制成的工具在切削耐热合金时显示比其他工具更优异的性能。然而,存在的问题是SiC晶须昂贵。
因此,已经考虑了SiC晶须之外的材料。专利文献1和2公开了其中向氧化铝添加碳化物、氮化物和/或碳氮化物所得的材料(所谓的黑陶瓷)。黑陶瓷由于其中通过将碳化物等分散在氧化铝中从而对烧结体进行增强的分散增强,因而具有比氧化铝更高的强度。其中,使用极硬的碳化钨的黑陶瓷是具有高硬度和优异耐磨性的材料。
专利文献3和4公开了其中将氧化锆分散在氧化铝中的材料(所谓的白陶瓷)。白陶瓷由于分散了氧化锆而具有提高的强度。尽管白陶瓷与黑陶瓷相比具有较低的硬度,但是白陶瓷由于使用部分稳定化的氧化锆所赋予的相变增韧而具有提高的韧度。
现有技术文献
专利文献
专利文献1:日本特许第3145470号公报
专利文献2:日本特许第4177493号公报
专利文献3:日本特许第2511700号公报
专利文献4:日本特开2000-128626号公报
发明内容
发明要解决的问题
然而,专利文献1~4中公开的材料对于例如在高负载和高温条件下实施的切削耐热合金中的应用具有不足的耐破损性和耐磨性。在本发明的一方面中,期望提供一种具有优异耐破损性和耐磨性的陶瓷烧结体。
解决问题的手段
根据本发明一方面的陶瓷烧结体的特征在于:所述陶瓷烧结体包含碳化钨、氧化锆和氧化铝;所述碳化钨的含量为20~50体积%;所述氧化锆的含量为5~25体积%;所述氧化锆的晶相为正方晶或者为正方晶与单斜晶的混晶;所述陶瓷烧结体实质上不含Ti化合物;且所述碳化钨的平均粒径、所述氧化锆的平均粒径和所述氧化铝的平均粒径都为1μm以下。
根据本发明一方面的陶瓷烧结体即使在高负载和高温条件下仍具有优异的耐破损性和耐磨性。
在根据本发明一方面的陶瓷烧结体中,所述碳化钨的平均粒径优选为0.7μm以下。在这种情况中,耐破损性和耐磨性还进一步提高。
在根据本发明一方面的陶瓷烧结体中,锆元素优选分布在所述氧化铝与所述碳化钨之间的晶界处。在这种情况中,耐破损性和耐磨性还进一步提高。
根据本发明一方面的接合体可以是由上述陶瓷烧结体制成的第一构件和由超硬合金或金属陶瓷制成的第二构件接合在一起的所得物。这种接合体即使在高负载和高温条件下仍具有优异的耐破损性和耐磨性。
附图说明
图1A是显示第一构件1和第二构件3的构造的透视图,且图1B是显示接合体5的构造的透视图。
图2A是显示第一构件1和第二构件3的构造的透视图,且图2B是显示接合体5的构造的透视图。
附图标记
1:第一构件;3:第二构件;3A、3B:顶点;5:接合体
具体实施方式
下文中将对本发明的实施方式进行说明。
根据本发明一个实施方式的陶瓷烧结体包含氧化铝。在根据本发明的陶瓷烧结体中,碳化钨和氧化锆之外的剩余物可以为例如氧化铝。通过包含氧化铝,陶瓷烧结体变得化学稳定,由此具有还进一步提高的耐磨性。碳化钨、氧化锆和氧化铝的平均粒径优选为1μm以下。在这种情况中,陶瓷烧结体具有更高的硬度和强度,且还具有更高的耐破损性。在本发明中平均粒径是指通过截距法测得的值,所述截距法是基于通过利用SEM对经过蚀刻处理的镜面研磨的烧结体进行观察而得到的图像实施的。
根据本发明的陶瓷烧结体可以通过包含20~50体积%的碳化钨而产生如下效果。碳化钨的含量是在将全部陶瓷烧结体定义为100体积%时的含量。
·碳化钨的均匀分散效果能够抑制晶粒生长。结果,陶瓷烧结体具有提高的强度和硬度。
·实现了陶瓷烧结体的高韧度、低热膨胀和高热导率。
·陶瓷烧结体通过包含50体积%以下的碳化钨而具有高烧结性和耐氧化性。
·碳化钨的平均粒径尤其优选为0.7μm以下。通过包含具有更小平均粒径的碳化钨还进一步提高上述分散效果。
根据本发明的陶瓷烧结体实质上不含Ti化合物(例如Ti的碳化物、碳氮化物或氮化物)。这导致陶瓷烧结体的强度、热特性和耐破损性提高。“实质上不含”是指陶瓷烧结体可以完全不包含、或者可以包含不会影响根据本发明的陶瓷烧结体的功能和效果的非常少的量(例如对应于不可避免的杂质的量)。该不会影响功能和效果的非常少的量是例如在将全部陶瓷烧结体定义为100重量%时为0.1重量%以下的量。
如果包含Ti化合物,则会产生如下效果。Ti化合物和碳化钨会在对根据本发明的陶瓷烧结体进行烧结的温度范围内形成固溶体(WX-Ti1-X-C)。固溶体化的碳化钨(WX-Ti1-X-C)会具有下降的硬度和热导率,由此具有下降的切削性能。由于Ti化合物具有比碳化钨更高的热膨胀,所以陶瓷烧结体整体还会具有更高的热膨胀,由此具有下降的耐热冲击性。此外,与氧化铝或氧化锆的热膨胀系数之差会下降,从而导致残余应力的增强效果下降。
根据本发明的陶瓷烧结体可能由于制造原因而不可避免地被Fe、Ni、Co和Cr污染。在这种情况中,Fe、Ni、Co和Cr的含量优选为不会影响根据本发明的陶瓷烧结体的功能和效果的非常少的量。
具体地,当将全体陶瓷烧结体定义为100重量%时,Fe的含量优选为0.04重量%以下,更优选0.03重量%以下。此外,Ni的含量优选为0.02重量%以下,更优选0.015重量%以下。Co的含量优选为0.03重量%以下,更优选0.02重量%以下。Cr的含量优选为0.03重量%以下,更优选0.02重量%以下。
通过以等于或低于上述上限值的含量包含Fe、Ni、Co和Cr,陶瓷烧结体中的晶界结合强度提高,由此提高陶瓷烧结体的高温强度和硬度。
根据本发明的陶瓷烧结体具有高断裂韧性,因为其中包含5~25体积%的氧化锆能够有效产生应力诱发相变。此外,通过使得耐磨性和耐热冲击性通常差的氧化锆的含量为25体积%以下,能够使得耐磨性和耐热冲击性在用于切削等时不会造成问题。氧化锆的含量是在将全体陶瓷烧结体定义为100体积%时的含量。
根据本发明的陶瓷烧结体,尤其是在包含30~40体积%的碳化钨的情况中,优选以5~25体积%的范围包含氧化锆,由此具有优异的耐破损性和耐磨性。在包含20~30体积%的碳化钨的情况中,从耐破损性考虑,更优选包含5~15体积%的氧化锆。在包含40~50体积%的碳化钨的情况中,从耐磨性考虑,更优选包含5~15体积%的氧化锆。
根据本发明的陶瓷烧结体主要包含WC作为碳化钨,但是在诸如在制造陶瓷烧结体时不对碳含量进行调节的情况中可以包含非常少量的W2C。即使在这种情况中,陶瓷烧结体的性能也不易受到损害,因为W2C的含量通常非常少。
在根据本发明的陶瓷烧结体中,氧化锆的晶相为正方晶或者为正方晶与单斜晶的混晶。这使得可以引起应力诱发相变,由此提高陶瓷烧结体的强度和韧度。通过例如X射线衍射分析仪或拉曼光谱装置能够鉴定氧化锆的晶相。可以使用稳定剂如氧化钇、二氧化铈、氧化镁和氧化钙而使得氧化锆的晶相为正方晶或者为正方晶与单斜晶的混晶。在根据本发明的陶瓷烧结体中,氧化锆的平均粒径为1μm以下。这使得可以将氧化锆的晶相容易地保持在正方晶、或者正方晶与单斜晶的混晶的状态下。
在根据本发明的陶瓷烧结体中,锆元素优选分布在氧化铝与碳化钨之间的晶界处。在这种情况中,烧结性提高,且晶界结合强度提高。推断这是因为锆元素提高了晶界结合强度。更具体地,作为氧化物且化学稳定的氧化铝和作为碳化物的碳化钨难以相互反应,因此,在所述两者之间通常不能获得足够的结合强度。然而,推断通过在晶界处包含锆元素,在氧化铝与碳化钨之间的晶界处的结合强度增大,因为锆元素形成与氧化铝具有良好反应性的氧化锆并且与同样是过渡金属的钨具有良好的反应性。作为提高的晶界结合强度的结果,由根据本发明的陶瓷烧结体制成的工具的耐崩刃性(chipping resistance)提高,从而导致工具的寿命更长。
为了将锆元素分布在上述晶界处,应在制造陶瓷烧结体时通过砂磨机研磨等技术对各成分进行充分分散。使用细氧化锆粉末或锆盐的溶液作为氧化锆的原料时,能够将锆元素有效分布在晶界处。另外,其中仅提前对氧化锆原料进行研磨的分散混合、及使用氧化锆制的研磨介质也是有效的。
此外,对烧结时的升温速率和保持时间进行优化能够促进锆元素的移动(扩散)。
例如能够在不使用晶须原料的条件下制备根据本发明的陶瓷烧结体。在这种情况中,在更低成本下制造陶瓷烧结体。
根据本发明的陶瓷烧结体能够为例如用于工具(用于难切削材料如耐热合金的切削工具)的材料。在这种情况中,能够制造提供优异切削性能的切削工具。
实施例1
1.陶瓷烧结体的制造方法
各自以预定量称量如下三种原料粉末,将其与乙醇一起放入由树脂制成的磨中,并使用氧化铝球研磨48小时,由此得到浆料。
平均粒径为0.4μm的氧化铝粉末
平均粒径为0.1~1.5μm的碳化钨粉末
平均粒径为0.6μm的氧化锆粉末(包含0~8摩尔%的氧化钇作为稳定剂)
使得到的浆料在热水中升温以除去乙醇并过筛以得到混合粉末。将混合粉末放入碳模具中并热压烧结以得到陶瓷烧结体。用于热压烧结的条件如下:
烧结温度:1650℃
烧结时间:2小时
压力:30MPa
气氛:Ar气
在上述制造方法中,各种改变原料粉末的配比、碳化钨粉末的平均粒径和氧化钇在氧化锆粉末中的含量以制造S1~S20和S30~S36的陶瓷烧结体,所述陶瓷烧结体满足表1中所示的组成。然而,仅有S35在快速升温(30℃/分钟以上)下而不是在上述热压烧结条件下进行烧结。
[表1A]
表1
[表1B]
表1续
基本以与上述制造方法类似的方式,制造了S21和S22的陶瓷烧结体,不同之处在于除了碳化钨、氧化锆和氧化铝之外还添加碳化钛。此外,基本以与上述制造方法类似的方式,制造了S23~S26的陶瓷烧结体,不同之处在于添加碳化钨/钛固溶体、碳化钛、氮化钛和碳氮化钛中的一种代替碳化钨。
2.陶瓷烧结体的分析
通过利用SEM对S1~S20和S30~S36的陶瓷烧结体中的晶界进行观察,确认了,除了S35之外,锆元素都分布在氧化铝与碳化钨之间的晶界处。在快速升温下进行烧结的S35中,无锆元素分布在氧化铝与碳化钨之间的晶界处。
在S1~S26和S30~S36的各种陶瓷烧结体中,通过拉曼光谱对氧化锆的晶相进行测定。将结果示于上表1的“氧化锆的晶相”列中。在表1中,“T”表示正方晶,“M”表示单斜晶,“C”表示立方晶,且“T,M”表示正方晶与单斜晶的混晶。
在S1~S26和S30~S36的各种陶瓷烧结体中,对碳化钨的平均粒径、氧化锆的平均粒径和氧化铝的平均粒径进行测定。将结果示于上表1中。表1中所示的平均粒径是通过使用在1万倍以上的放大倍率下照相的SEM图像的截距法测定的值。
3.陶瓷烧结体的评价
(1)测定三点弯曲强度、维氏硬度(Vickers Hardness)和断裂韧性
利用S1~S26和S30~S36的各种陶瓷烧结体,制备3×4×15mm的试验片以测定其三点弯曲强度(跨度为10mm)、维氏硬度和断裂韧性(IF法)。此外,以预定形状测定在室温下的热导率和在600℃下的热膨胀。此外,以类似方式对可商购获得的氧化铝/晶须基工具(下文中称作S27)、SiAlON基工具(下文中称作S28)和氧化铝/TiC基工具(下文中称作S29)进行测定。将结果示于表2中。在表2中,将三点弯曲强度显示为“弯曲强度”,并将维氏硬度显示为“硬度”。
(2)切削试验
利用S1~S36的各种陶瓷烧结体,制备切削刀片以实施切削试验。实施如下两种切削试验。
(a)切削试验1(铸铁间歇切削试验)
(a-1)试验条件
刀片#形状:SNGN432-TN
切削工件:FC200
切削速度:200m/分钟
切削深度:1.5mm
进料速率:0.55~0.75mm/转
冷却剂:不存在
(a-2)评价方法
如果在固定进料速率下切削5次之后不发生破损,则在以0.05mm/转的步长升高的进料速率下重复所述过程,直至进料速率达到0.75mm/转。通过发生破损时的进料速率对耐破损性进行评价。更具体地,在表2的“切削试验1”中的“进料速率”列中,“O”表示在各进料速率下未发生破损的情况,且“破损”表示发生破损的情况。如表2的“切削试验1”中的“评价”列中所示,以“×”表示在0.65mm/转的进料速率下或在之前发生破损的情况、“△”表示在0.70mm/转的进料速率下发生破损的情况、“O”表示在0.75mm/转的进料速率下发生破损的情况和“◎”表示未发生破损的情况的方式进行评价。
(a-3)试验结果
将试验结果示于上表2中。S3~6、10~12、14、15、17、18、30~32和34的陶瓷烧结体与其他相比具有更高的耐破损性。
(b)切削试验2(耐热合金车削试验)
(b-1)试验条件
刀片形状:RCGX120700T01020
切削工件:INCONEL718锻造品
切削速度:240~480m/分钟
切削深度:1.0mm
进料速率:0.2mm/转
冷却剂:存在
(b-2)评价方法
基于在各速度下切削2次之后的边界磨损量、刀尖状态(存在或不存在崩刃等)以及精加工表面的状态,以如下三个等级对精加工表面的状态(美观)进行评价:O(良好)、△(中等)和×(差)。
对各陶瓷烧结体测定在240、360和480m/分钟的切削速度下的磨损量。
(b-3)试验结果
将试验结果示于上表2中。在表2中,(F)表示发生剥落。S3~6、10~12、14、15、17、18和30~36的陶瓷烧结体与其他相比具有更高的耐破损性和耐磨性。此外,S3~6、10~12、14、15、17、18和30~36的陶瓷烧结体与其他相比具有更美丽的精加工表面。
4.陶瓷烧结体所产生的效果
(1)S3~6、10~12、14、15、17、18和30~36的陶瓷烧结体具有优异的耐破损性和耐磨性。
(2)与S27相比,S3~6、10~12、14、15、17、18和30~36的陶瓷烧结体可在更低的成本下制造。
(3)使用S3~6、10~12、14、15、17、18和30~36的陶瓷烧结体能够在高速下并以高效率对耐热合金进行机械加工。
(4)使用S3~6、10~12、14、15、17、18和30~36的陶瓷烧结体提供高的精加工表面的精确度。
(5)使用S3~6、10~12、14、15、17、18和30~36的陶瓷烧结体能够对耐热合金进行机械加工。
鉴于上述结果确认了,S3~6、10~12、14、15、17、18和30~36的陶瓷烧结体可用于耐热合金的精加工。具体地,上述陶瓷烧结体在240m/分钟以上的切削速度下的精加工中显示优异的切削性能。因此,使用上述陶瓷烧结体能够高效地切削耐热合金。使用上述陶瓷烧结体还能够改善精加工表面的状态。
实施例2
1.接合体5的制造方法
首先,如图1A中所示,单独制造由上述实施例1的陶瓷烧结体S5制成的第一构件1和由超硬合金(由WC和钴粘合剂制成)制成的第二构件3。第一构件1具有三角棱柱形状。第二构件3基本具有在其两个顶点3A和3B处具有与第一构件1成比例的切口(cutout)的长方体形状。
接下来,如图1B中所示,通过铜焊将第一构件1接合至第二构件3的顶点3A和3B中的各顶点,由此完成接合体5。接合体5具有与DNGA150408相对应的长方体形状。
2.接合体5的评价(部分1)
(1)试验条件
当接合体5的主要接触切削工件的部分为第一构件1时,使用接合体5作为刀片在如下条件下实施精加工。
此外,在类似条件下使用可商购获得的cBN刀片(由住友电工株式会社制造的cBN和超硬合金的接合体)和可商购获得的PVD涂布的超硬工具(由住友电工株式会社制造)实施精加工。然而,将在使用可商购获得的PVD涂布的超硬工具时的切削速度设定为56m/分钟。这是因为,240m/分钟的切削速度导致可商购获得的PVD涂布的超硬工具过度磨损。可商购获得的cBN刀片和可商购获得的PVD涂布的超硬工具各自具有与DNGA150408相对应的形状。
切削工件:INCONEL718锻造品
切削速度:240m/分钟
切削深度:0.4mm
进料速率:0.15mm/转
冷却剂:存在
(2)评价方法
在精加工之后对刀片的侧面磨损量和机械加工表面的表面粗糙度进行测定。关于刀片的侧面磨损量,将0.3mm定义为寿命终止磨损量。表面粗糙度为机械加工表面的凸起部和凹入部之间的距离。更小的表面粗糙度指示更好的机械加工表面状态。
(3)试验结果
当使用接合体5的刀片时,侧面磨损量在切削3次之后接近寿命终止磨损量的一半并在切削5次之后达到寿命终止磨损量。此外,当使用接合体5的刀片时,机械加工表面具有明显更小的表面粗糙度。
另一方面,当使用可商购获得的cBN刀片时,在切削3次之后侧面磨损量达到寿命终止磨损量。当使用PVD涂布的超硬工具时,在切削5次之后侧面磨损量达到寿命终止磨损量。此外,当使用PVD涂布的超硬工具时,机械加工表面具有比使用接合体的刀片时明显更大的表面粗糙度。
3.接合体5的评价(部分2)
(1)试验条件
当接合体5的主要接触切削工件的部分为第一构件1时,使用接合体5作为刀片在如下条件下实施精加工。
此外,在类似条件下使用可商购获得的cBN刀片(由住友电工株式会社制造的cBN和超硬合金的接合体)实施精加工。
切削工件:INCONEL718锻造品
切削速度:360m/分钟
切削深度:0.4mm
进料速率:0.15mm/转
冷却剂:存在
(2)评价方法
在精加工之后对刀片的侧面磨损量和机械加工表面的表面粗糙度进行测定。关于刀片的侧面磨损量,将0.3mm定义为寿命终止磨损量。表面粗糙度为精加工表面的凸起部和凹入部之间的距离。更小的表面粗糙度指示优越性。
(3)试验结果
当使用接合体5的刀片时,侧面磨损量在切削2次之后小于或等于寿命终止磨损量的一半且即使在切削4次之后仍未达到寿命终止磨损量。此外,当使用接合体5的刀片时,机械加工表面具有明显更小的表面粗糙度。
另一方面,当使用可商购获得的cBN刀片时,在切削2次之后侧面磨损量达到寿命终止磨损量。此外,当使用可商购获得的cBN刀片时,与使用接合体5的刀片的情况相比,机械加工表面具有明显更大的表面粗糙度。
4.接合体5所产生的效果
接合体5即使在高负载和高温条件下仍具有优异的耐破损性和耐磨性。因此,使用接合体5使得能够高效切削耐热合金。使用接合体5还能够改善机械加工表面的状态。
应理解,本发明不应被限制为上述实施例,而是可以在不背离本发明范围的条件下以各种形式实践。
例如,接合体5的形状不应被限制为上述形状,而是可以通过对具有如图2A中所示形状(具有向下变小的直径的圆柱形状)的第一构件1和第二构件3进行铜焊而进行接合,制造具有如图2B中所示形状的接合体5。第二构件3的材料可以为金属陶瓷。
包含在单个接合体5中的第一构件1的数目可以为单数或多数(例如2、3、4...)。
此外,根据本发明的陶瓷烧结体能够用于例如摩擦搅拌焊接或用作耐冲击构件。
对第一构件1和第二构件3进行接合的方法不应被限制为铜焊,而是能够适当使用其他接合方法(例如加压下的直接扩散法)。
Claims (3)
1.一种陶瓷烧结体,其包含碳化钨、氧化锆和氧化铝,
其中所述碳化钨的含量为20~50体积%,
其中所述氧化锆的含量为5~25体积%,
其中所述氧化锆的晶相为正方晶或者为正方晶与单斜晶的混晶,
其中所述陶瓷烧结体实质上不含Ti化合物,且
其中所述碳化钨的平均粒径、所述氧化锆的平均粒径和所述氧化铝的平均粒径都为1μm以下。
2.如权利要求1所述的陶瓷烧结体,
其中所述碳化钨的平均粒径为0.7μm以下。
3.如权利要求1或2所述的陶瓷烧结体,
其中锆元素分布在所述氧化铝与所述碳化钨之间的晶界处。
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