CN101084169B - 立方氮化硼压块 - Google Patents

立方氮化硼压块 Download PDF

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CN101084169B
CN101084169B CN200580041693.8A CN200580041693A CN101084169B CN 101084169 B CN101084169 B CN 101084169B CN 200580041693 A CN200580041693 A CN 200580041693A CN 101084169 B CN101084169 B CN 101084169B
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N·卡恩
S·A·安德森
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No Six Element Trademark Co
Element Six Abrasives SA
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Abstract

本发明涉及包含CBN和基质相的CBN压块，该基质相结合了选自TiCN、TiC、TiN、其混合物与固溶体的第二硬质相和最大量的二硼化钛，其中(101)二硼化钛峰(在背景校正之后)的XRD峰高小于(111)CBN峰的峰高的12％。

Description

立方氮化硼压块
发明背景
本发明涉及立方碳化硼(CBN)磨料压块。
氮化硼通常以三种晶体形式存在，即立方氮化硼(CBN)、六方氮化硼(hBN)和纤锌矿型(wurtzitic)立方氮化硼(wBN)。立方氮化硼为结构类似于金刚石的氮化硼的硬质闪锌矿形式。在CBN结构中，原子之间形成的键是坚固的，主要为共价四面体键。
CBN压块包括CBN颗粒的烧结物质。当CBN含量大于该压块的80体积％时，存在大量的CBN-CBN接触和粘结。当CBN含量较低，例如范围在该压块的40-60体积％，那么直接的CBN-CBN接触是有限的。CBN压块通常也含有粘合剂相，例如铝、硅、钴、镍、和钛。
当压块的CBN含量小于70体积％时，基质相、即无CBN的相，将通常也包含另一硬质相，即第二相，其可以是陶瓷质的。适宜的陶瓷硬质相的实例为第4、5或6族过渡金属(依据新的IUPAC形式)的碳化物、氮化物、硼化物和碳氮化物，氧化铝，和碳化物如碳化钨及其混合物。该基质构成组合物中除CBN之外的全部组分。
CBN压块可以在形成工具插件(tool insert)或工具时直接粘结于工具体。但是，对于许多应用，优选地将该压块粘结于基体/载体材料，形成负载的压块结构，随后将该负载的压块结构粘结于工具体。该基体/载体材料通常为硬质金属碳化物，其与粘合剂如钴、镍、铁或其混合物或合金粘结在一起。金属碳化物颗粒可以包括钨、钛或钽碳化物颗粒或其混合物。
制造CBN压块和负载的压块结构的已知方法包括，使CBN颗粒的未烧结物质经受高温和高压条件(即CBN在结晶学上稳定的条件)适当的时间段。可以利用粘合剂相增强颗粒的粘结。所用的典型高温和高压条件为1100℃或更高的温度和2GPa或更高数量级的压力。保持这些条件的时间段通常为约3-120分钟。
CBN在加工工具等中具有广泛的商业应用。其可以用作砂轮、切削工具等中的磨粒，或者采用常规电镀技术将其粘结于工具体以形成工具插件。CBN也可以以粘结形式用作CBN压块。CBN压块趋于具有良好的磨损性，是热稳定的，具有高导热性，良好的抗冲性和与含铁的金属接触时具有低的摩擦系数。该CBN压块，具有或者不具有基体，经常被切割为期望的尺寸和/或待用的特定切削或钻孔工具的形状，并随后利用钎焊技术将其安装在工具体上。
CBN压块广泛地应用于制造用于硬化钢精加工的切削工具，如容器硬化钢、滚珠钢和通过硬化的工程钢。除了使用条件之外，如切削速度、切削的进送和深度，通常已知CBN工具的性能取决于加工件的几何形状，且特别地，是否该工具长期不变地接合于加工件，本领域公知为“连续切削”，或者是否该工具以断续方式接合于加工件，本领域通常公知为“断续切削”。
依据加工件几何形状，通常CBN工具在加工循环之内同时经历连续的和断续的切削，另外，连续/断续切削比例在该领域中大大地变化.在对该领域广泛研究之后发现，这些不同模式的切削对构成工具切削边的CBN材料产生非常不同的需求.主要问题是，工具趋于由于破裂或碎裂而灾难性地失效，其由于市场中对于通过增加切削速度的更高产能的日益增加的需求而加剧.这点通常导致工具寿命降低，使得必须经常更换该工具.反过来，这点通常导致生产成本增加，这点是不利的.期望开发出改进的CBN基材料，其功能更有效，例如显示改进的抗失效性和磨损强度.
US6,316,094公开了CBN烧结体，其中单一平均粒度的CBN颗粒通过粘结相粘结。将粉状组合物烧结制得烧结体。该粉状组合物是采用各种混合方法如超声混合和砂磨粉碎制备的。US6,316,094中，声称砂磨粉碎是最差的混合方法。
US4,334,928公开了包含CBN颗粒和各种含钛化合物的氮化硼烧结压块。典型地将含钛化合物预反应并且形成为烧结压块，随后压碎。该CBN压块进一步含有单一平均粒度的CBN。烧结过程中采用较低温度来制备该CBN压块。
发明概述
依据本发明，CBN压块包含CBN和基质相，该基质相结合了选自TiCN、TiC、TiN、其混合物与固溶体的第二硬质相和最大量的二硼化钛，其中(101)二硼化钛峰的XRD峰高(在背景校正之后)小于(111)CBN峰的峰高的12％、优选小于CBN峰高的10％且更优选小于CBN峰高的5％。
进一步依据本发明，如在XRD分析中所测量的，对于钛基第二硬质相，其半宽度(FWHM)为至少0.2度2θ，优选为至少0.25度2θ，更优选为至少0.3度2θ。
该CBN压块通常含有35-75体积％、优选35-65体积％的CBN。
该基质相可以进一步包含粘合剂相。该粘合剂相可以为铝。将意识到的是，铝可以作为铝或者作为键合形式的铝存在，如氮化铝、二硼化铝、铝化钛和/或其组合。该基质相可以进一步包括碳化钨和/或Al2O3。
依据本发明的另一方面，提供了含有如上所定义的CBN压块的工具插件。
优选实施方案的详述说明
本发明涉及CBN压块，更具体地，涉及包含CBN和基质相的CBN压块，该基质相结合了钛基第二硬质相和极低量的二硼化钛，如上所定义。
二硼化钛通常由于CBN与含有钛化合物如碳氮化钛的第二硬质相之间的反应而存在于CBN压块中。TiB2通常作为CBN颗粒与第二硬质相颗粒之间的粘结剂。但是，如果CBN材料中存在过高量的二硼化钛，材料的耐磨性通常将增加；但是抗破裂性和抗碎裂性将降低。具有高TiB2含量的CBN材料的耐磨性增加可能归因于TiB2的高硬度。抗破裂性和抗碎裂性的降低可能与材料热膨胀系数的各向异性相关。由于TiB2具有六方晶体结构，(CBN、AlN、碳氮化钛都具有立方晶体结构)，TiB2由热膨胀系数的各向异性而在CBN与第二硬质相材料之间引入了残余应力。这样导致CBN与第二硬质相之间界面的弱化，导致强度损失和由此在要求抗破裂性和抗碎裂性的应用中性能大大降低。
本发明首次认识了该问题，并且通过将CBN与第二硬质相之间的TiB2含量降低到可以最优化该材料性能的水平，由此解决了该问题。已采用材料中TiB2与CBN的测量峰高的X-射线衍射峰高比例，量化了该CBN压块中TiB2的这些最佳水平。
本发明的另一方面在于，该CBN材料含有显示高XRD峰加宽的第二硬质相.该第二硬质相的XRD峰加宽(低衍射角下)表明，该第二硬质相具有极细的粒度，且也可以包括化学性方面的变化.这些独特的方面改进了材料性能和由此提供了要求抗破裂性和抗碎裂性的应用中的性能增强.采用第二硬质相材料的XRD峰的半宽度(Full-Width-Half-Maximum)(FWHM)测量，定义该第二硬质相的特征.
采用装配有发生器设定为40kV和45mA的Cu辐射的立式衍射计，进行CBN压块材料的X-射线检测。通常在20-65度2θ角范围之间进行XRD扫描，步长为0.02度2θ，每步5秒钟。在FWHM测量之前将收集的XRD扫描进行背景校正和Ka-2剥离。在曲线拟合数据和确定峰位置之后，进行FWHM测量。在具有(111)和(200)平面的碳氮化钛、氮化钛和碳化钛上进行FWHM测量。在鉴别峰位置之后立即测量峰高。在(111)平面上测量CBN峰高；但是在(101)平面上测量TiB2高度。
本发明的CBN压块通过制备粉状形式的CBN颗粒和基质相的混合物来制得。该混合物中的CBN颗粒可以是单峰的，即，全部CBN颗粒具有相同的平均粒度；或者是多峰的，即，该CBN颗粒由至少两种平均粒度的颗粒的混合物组成。当该CBN为多峰的时，该CBN优选地为双峰的，即，该CBN由具有两种平均粒度的颗粒组成。
该基质相可以进一步包含粘合剂相，例如但并非限定于铝。将意识到的是，铝可以作为铝或者作为键合形式的铝存在，如氮化铝、二硼化铝、铝化钛和/或其组合。
当碳氮化钛为第二硬质相时，其可以是亚化学计量的，即Ti(C1-xNx)y，其中x显示氮相对于碳的固溶体浓度；且y显示全部碳氮化物相对于钛的比例。通常在烧结之前，可以将TiCN与粘合剂相例如铝(存在时)预反应。这样将导致化学计量的碳氮化钛、铝化钛和任意未反应的相的反应产物。
已发现，一种获得细粒度第二硬质相的方法是采用砂磨粉碎(attrition milling)制备CBN和基质相的混合物。砂磨粉碎机(attrition mill)由具有搅拌器的密封研磨室组成，该搅拌器在垂直或水平方向上高速旋转。所用研磨介质通常尺寸范围为0.2-15mm，且在粉碎为主要目的时，研磨介质通常为高密度的硬质合金。搅拌器的高旋转速度，与高密度、小直径的介质一起，提供了极高的能量。另外，砂磨粉碎中高能量获得了浆料中的高剪切，提供了极成功的粉末的辅助分散、或共混。相对于所述其它方法如常规球磨机、滚筒式球磨机、行星式球磨机、搅拌式(agitated)或搅拌式(stirred)球磨机，砂磨粉碎通常在烧结压块中获得了更细的颗粒和更好的均质性。由此，特别是在砂磨粉碎用于“两步”工艺时，采用砂磨粉碎法研磨第二相和粉状粘合剂相，制得细混合物，该混合物通常由纳米级颗粒(通常粒度范围为约200-约500nm的颗粒)组成。将获得的细混合物和CBN颗粒进一步进行砂磨粉碎以制得均质的混合物。
利用“两步”砂磨粉碎的优点在于，通常获得极细的用于烧结的起始材料。较细的第二硬质相和粘合剂相颗粒优选地具有高比表面积和由此高的反应性，导致CBN和第二硬质相颗粒之间极佳的烧结。类似地，第二硬质相颗粒的小尺寸赋予它们高的比表面积，且由此也具有第二硬质相颗粒之间良好的粘结。另外，第二硬质相颗粒的小尺寸获得更均质的压块，该压块用于形成工具插件时，通常获得更好的工具插件性能。
使CBN和粉状基质相的混合物经受CBN在结晶学上稳定的高温和高压条件，由此制得CBN压块。该条件和方法是本领域中众所周知的。
但是，将意识到的是，可以利用其它有效方法来制备依据本发明的CBN压块且制备该压块的方法并非限定于上述那些。
以下列方式测量压块的CBN含量：采用金属丝EDM切削样品件并随后抛光.采用扫描电子显微镜分析该CBN压块的抛光表面.依据估算的平均CBN粒度选择在适当放大倍数(3000、5000和7000放大倍数)下的背散射电子图像.(如果平均粒度小于1微米，采用7000放大倍数；如果平均CBN粒度大于1微米且小于2微米，采用5000放大倍数.如果平均粒度大于2微米且小于3微米，采用3000放大倍数.)利用至少30个图像进行分析以统计表达该样品.
在下列步骤中分析所收集的灰度图像。首先，将灰度图像在电子学上处理以鉴别微结构中的CBN颗粒。该处理包括利用对于CBN的临界灰度值将灰度图像转化为二进制图像，其中CBN颗粒被鉴别为一个相。剩余相为基质相(无-CBN的相)。随后，测量全部所鉴别的CBN颗粒的总面积，并且对于每个图像计算全部CBN的百分比面积。随后，取通常大于30个图像的全部测量的平均值，计算CBN面积的平均值。该CBN面积百分比对应于材料的整体CBN含量。
该基质相可以进一步包括碳化钨和/或Al2O3。这些材料通常起到颗粒生长抑制剂的作用，其防止/降低高温高压烧结期间第二硬质相颗粒的颗粒生长。
本发明的CBN压块特别适用作为加工硬化钢、冷热水操作工具钢、模具钢、容器硬化钢、高速钢和可锻铸灰铁辊的工具插件。但是，将意识到的是，本发明的CBN压块的应用并非限定于上面所列的那些。
实施例
现在将参照下列非限定性实施例阐述本发明。
实施例1
将亚化学计量的平均粒度为1.4微米的碳氮化钛粉末(Ti(C0.7N0.3)0.8)与平均粒度为5微米的Al粉混合。Ti(C0.7N0.3)0.8与Al之间的质量比为90∶10。将该粉末混合压制成钛杯以形成压块坯，并且在真空下加热到1025℃下30分钟并随后压碎和研磨成粉。随后将该粉末混合物砂磨粉碎4小时。将含有约30wt％平均粒度为0.7微米的CBN和平均粒度为2微米的其它CBN的CBN粉末混合物，以一定量加入浆料中以获得整体65体积％的CBN。采用砂磨粉碎将含CBN的浆料研磨和混合1小时。将该浆料在真空下干燥并成形为压块坯，并且在55kbar(5.5GPa)和约1300℃下烧结以制得CBN压块。
依据X-射线衍射分析，该烧结材料除了含有CBN和碳氮化钛之外，还含有少量的TiB2、AlN、Al2O3和WC。表示为(111)平面中CBN峰高的百分比的、(101)平面中的XRD TiB2峰高为3.68％。(111)和(200)平面的碳氮化钛的FWHM值分别为0.315和0.331度2θ。
通过图像分析测量的CBN含量为53.4％面积，其为在5000放大倍数下获得的40个背散射电子SEM图像的分析平均值。面积百分比实质上等同于体积百分比。
实施例2
将亚化学计量的平均粒度为1.4微米的碳氮化钛粉末(Ti(C0.7N0.3)0.8)与平均粒度为5微米的Al粉混合。Ti(C0.7N0.3)0.8与Al之间的质量比为90∶10。将该粉末混合压制成钛杯以形成压块坯，并且在真空下加热到1025℃下30分钟并随后压碎和研磨成粉。随后将该粉末混合物砂磨粉碎4小时。将含有约30wt％平均粒度为0.7微米的CBN和平均粒度为2微米的其它CBN的CBN粉末混合物，以一定量加入浆料中以获得整体45体积％的CBN。采用砂磨粉碎将含CBN的浆料研磨和混合1小时。将该浆料在真空下干燥并成形为压块坯，并且在55kbar(5.5GPa)和约1300℃下烧结以制得CBN压块。
依据X-射线衍射分析，该烧结材料除了含有CBN和碳氮化钛之外，还含有少量的TiB2、AlN、Al2O3和WC。表示为(111)平面中CBN峰高的百分比的、(101)平面中的XRD TiB2峰高为4.19％。(111)和(200)平面的碳氮化钛的FWHM(半宽度)值分别为0.522和0.582度2θ。
通过图像分析测量的CBN含量为38.5％面积，其为在5000放大倍数下获得的50个背散射电子SEM图像的分析平均值。面积百分比实质上等同于体积百分比。
实施例3
将亚化学计量的平均粒度为1.4微米的碳氮化钛粉末(Ti(C0.5N0.5)0.8)与平均粒度为5微米的Al粉混合。Ti(C0.5N0.5)0.8与Al之间的质量比为90∶10。将该粉末混合压制成钛杯以形成压块坯，并且在真空下加热到1025℃下30分钟并随后压碎和研磨成粉。随后将该粉末混合物砂磨粉碎4小时。将含有约30wt％平均粒度为0.7微米的CBN和平均粒度为1.4微米的其它CBN的CBN粉末混合物，以一定量加入浆料中以获得整体55体积％的CBN。采用砂磨粉碎将含CBN的浆料研磨和混合1小时。将该浆料在真空下干燥并成形为压块坯，并且在55kbar(5.5GPa)和约1300℃下烧结以制得CBN压块。
依据X-射线衍射分析，该烧结材料除了含有CBN和碳氮化钛之外，还含有少量的TiB2、AlN、Al2O3和WC。表示为(111)平面中CBN峰高的百分比的、(101)平面中的XRD TiB2峰高为2.52％。对于(111)平面的碳氮化钛峰的FWHM(半宽度)值为0.593度2θ。
通过图像分析测量的CBN含量为48.1％面积，其为在5000放大倍数下获得的40个背散射电子SEM图像的分析平均值。面积百分比实质上等同于体积百分比。
实施例4
将亚化学计量的平均粒度为1.4微米的碳化钛粉末TiC0.8与平均粒度为5微米的Al粉混合。TiC0.8与Al之间的质量比为90∶10。将该粉末混合压制成钛杯以形成压块坯，并且在真空下加热到1025℃下30分钟并随后压碎和研磨成粉。随后将该粉末混合物砂磨粉碎4小时。将含有约30wt％平均粒度为1.4微米的CBN的CBN粉末混合物，以一定量加入浆料中以获得整体50体积％的CBN。采用砂磨粉碎将含CBN的浆料研磨和混合1小时。将该浆料在真空下干燥并成形为压块坯，并且在55kbar(5.5GPa)和约1300℃下烧结以制得CBN压块。
依据X-射线衍射分析，该烧结材料除了含有CBN和碳化钛之外，还含有少量的TiB2、AlN、Al2O3和WC。表示为(111)平面中CBN峰高的百分比的、(101)平面中的XRD TiB2峰高为4.88％。(111)和(200)平面的碳氮化钛的FWHM值分别为0.392和0.389度2θ。
通过图像分析测量的CBN含量为43.98％面积，其为在5000放大倍数下获得的45个背散射电子SEM图像的分析平均值。面积百分比实质上等同于体积百分比。

Claims (10)

1.包含CBN颗粒和基质相的CBN压块，该基质相结合了选自TiCN、TiC、TiN、其混合物与固溶体的第二硬质相和最大量的二硼化钛，其中二硼化钛(101)峰的XRD峰高，在背景校正之后，小于(111)CBN峰的峰高的10％。
2.根据权利要求1的CBN压块，其中二硼化钛(101)峰的XRD峰高，在背景校正之后，小于(111)CBN峰的峰高的5％。
3.根据前述权利要求中任一项的CBN压块，其是由含有35-75体积％CBN的组合物制成的。
4.根据前述权利要求中任一项的CBN压块，其中第二硬质相的XRD峰具有至少0.2度2θ的半宽度。
5.根据权利要求1-3中任一项的CBN压块，其中第二硬质相的XRD峰具有至少0.25度2θ的半宽度。
6.根据权利要求1-3中任一项的CBN压块，其中第二硬质相的XRD峰具有至少0.3度2θ的半宽度。
7.根据前述权利要求中任一项的CBN压块，其中该第二硬质相为TiCN。
8.根据前述权利要求中任一项的CBN压块，其中该基质相进一步包括为铝或铝基化合物的粘合剂相。
9.根据前述权利要求中任一项的CBN压块，其中该基质相进一步包括碳化钨和/或Al2O3。
10.含有根据权利要求1-9中任一项的CBN压块的工具插件。
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