CN110431247A - 烧结的聚晶立方氮化硼材料 - Google Patents

烧结的聚晶立方氮化硼材料 Download PDF

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Publication number
CN110431247A
CN110431247A CN201880017876.3A CN201880017876A CN110431247A CN 110431247 A CN110431247 A CN 110431247A CN 201880017876 A CN201880017876 A CN 201880017876A CN 110431247 A CN110431247 A CN 110431247A
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cbn
particle
boron nitride
particle size
sintering
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CN201880017876.3A
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A·坎
A·M·M·莫特切拉霍
M·米兰达-费尔南德斯
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Element Six UK Ltd
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Element Six UK Ltd
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Abstract

提供一种制造聚晶立方氮化硼(PCBN)材料的方法。基质前体粉末包含铝化合物。该方法包括混合基质前体粉末与30‑40体积％的立方氮化硼(cBN)颗粒，该基质前体粉末包含平均颗粒尺寸不大于250nm的颗粒，该立方氮化硼(cBN)颗粒具有至少4μm的平均颗粒尺寸，和然后使混合颗粒进行放电等离子体烧结。在至少500MPa的压力、不低于1050℃且不高于1500℃的温度和不小于1分钟且不大于3分钟的时间下进行该放电等离子体烧结。

Description

烧结的聚晶立方氮化硼材料
技术领域
本发明涉及烧结的聚晶立方氮化硼材料领域，以及制造此类材料的方法。
背景技术
聚晶超硬材料，如聚晶金刚石(PCD)和聚晶立方氮化硼(PCBN)，可用于各种工具，用于切削、机加工、钻孔或降解硬质材料或磨蚀性材料，如岩石、金属、陶瓷、复合材料和含木材料。
磨料压块广泛用于切削、铣削、磨削、钻孔和其它研磨操作。它们通常含有分散在第二相基质中的超硬磨料颗粒。基质可以是金属或陶瓷或金属陶瓷。超硬磨料颗粒可以是金刚石、立方氮化硼(cBN)、碳化硅或氮化硅等。在通常使用的高压和高温压块制造工艺期间这些颗粒可以彼此结合，从而形成聚晶物质，或者可以通过第二相材料的基质结合从而形成烧结聚晶物体。此类物体通常称为PCD或PCBN，其中它们分别含有金刚石或cBN作为超硬磨料。
美国专利US 4,334,928教导了一种用于工具的烧结压块，该工具基本上由20至80体积％的立方氮化硼组成；且余量是至少一种基质化合物材料的基质，所述基质化合物材料选自周期表的IVa或Va过渡金属的碳化物、氮化物、碳氮化物、硼化物和硅化物，它们的混合物和它们的固溶体化合物。该基质在烧结体中形成连续的结合结构，高压氮化硼散布在连续基质中。该专利中概述的方法都涉及使用机械磨制/混合技术如球磨、砂浆等将期望的材料组合。
对用于基质相的前体粉末进行磨制以减小它们的颗粒尺寸，以便更紧密地混合并改善它们之间的结合，因为较小的颗粒更具反应性。然而，PCBN的典型烧结工艺使用至少1100℃的温度和至少3.5GPa的压力来形成PCBN材料。在这些条件下，可以发生晶粒生长并且一些基质颗粒的颗粒尺寸能够大大增加，从而具有典型高达1μm的尺寸。这对所得PCBN的性质具有不利影响。
发明概述
目的是提供一种烧结的PCBN材料，其具有更均匀的基质晶粒尺寸以提供改善的工具性能。
根据本发明，提供了一种制造聚晶立方氮化硼PCBN材料的方法。该方法包括混合基质前体颗粒与30-40体积％的立方氮化硼cBN颗粒，该基质前体颗粒包括平均颗粒尺寸不大于250nm的颗粒，该基质前体粉末包含铝化合物，该立方氮化硼cBN颗粒具有至少4μm的平均颗粒尺寸。使混合颗粒在至少500MPa的压力、不低于1050℃且不高于1500℃的温度和不小于1分钟且不大于3分钟的时间下进行放电等离子体烧结。
作为选择，压力为至少1GPa。
作为选择，温度选自以下任何：不超过1400℃和不超过1300℃。
作为选择，时间不超过2分钟。
该方法任选地还包括以每分钟100至500℃的加热速率升温至所述温度。
作为选择，基质材料还包含碳和氮中任何的钛化合物。
作为选择，基质材料包含碳氮化钛、碳化钛、氮化钛、二硼化钛、氮化铝和氧化铝中的任何。
将基质粉末和cBN粉末混合的步骤任选地包括湿法声学混合、干法声学混合和碾磨中的任何。
该方法任选地包括提供平均尺寸在0.2和15μm之间的cBN颗粒。
该方法任选地包括提供具有选自以下任何的平均尺寸的cBN颗粒：大于1μm和大于4μm。
该方法任选地包括提供具有多模态平均尺寸分布的cBN颗粒。
附图简述
现在将通过示例并参考附图来描述非限制性的实施方案，其中：
图1是在H15条件下以5.5GPa和6.8GPa烧结的PCBN工具的工具寿命的坐标图；
图2是在H10条件下以5.5GPa和6.8GPa烧结的PCBN工具的工具寿命的坐标图；
图3是在6.8GPa和1300℃下烧结的PCBN样品的扫描电子显微图；
图4是在5.5GPa和1300℃下烧结的PCBN样品的扫描电子显微图；
图5是说明预压实步骤的流程图；
图6示出在不同温度下烧结的低cBN样品的XRD线图；
图7示出在不同温度下烧结的高cBN样品的XRD线图；
图8示出在不同温度下烧结的高cBN样品的重度间断工具寿命；
图9示出通过放电等离子体烧结制备的示例性PCBN材料的XRD光谱；
图10示出通过放电等离子体烧结制备的其它示例性PCBN材料的XRD光谱；
图11示出实施例35至43的维氏硬度数据；
图12示出实施例44至53的维氏硬度数据；
图13示出实施例35至43的密度数据；
图14示出实施例44至53的密度数据；
图15示出使用SPS在80MPa下烧结的实施例53至58和63至68的硬度数据；
图16示出使用SPS在1GPa下烧结的实施例59至62和69至72的硬度数据；
图17示出各种样品的拉曼光谱；和
图18是通过放电等离子体烧结在1GPa制备的扫描电子显微图。
详细描述
已经发现，当使用细粒基质前体粉末时，d90小于100nm(当使用线性截距技术测量时)，在烧结期间使用极高压力限制了烧结过程期间的晶粒生长。
使用线性截距法，通过显微图绘制随机直线，并计数与该线相交的晶界数目。通过将交点数除以实际线长度得到平均晶粒尺寸。使用多于一条随机线对结果进行平均来提高结果的准确性。平均晶粒尺寸由下式给出：
为了该分析的目的，对于每个图像分析五条水平线和5条垂直线以获得线性截距平均晶粒尺寸。
类似地，还发现在某些条件下的放电等离子体烧结(SPS)限制晶粒生长。限制晶粒生长是有利的，因为基质相中较小的晶粒改善由PCBN制成的工具的性能。这些性能包括增加的工具和减少的月牙洼磨损。
首先考虑使用高压高温(HPHT)技术制造的PCBN，已发现对于给定的烧结温度，较高的压力改善性能。这被认为是由于在烧结过程期间因加速的质量传输而引起的晶粒生长抑制和更有效的烧结的组合。
通过碾磨粉末加工途径制备具有TiC0.5N0.5 Al基质相的55体积％的1.3μm cBN含量的粉末组合物。在约8吨下将粉末压入金属杯中以产生17mm直径的生坯并在带式高压高温设备中烧结。
使用五种不同的烧结循环烧结粉末，如表1所示。对于每个烧结循环，使用19分钟的最高温度保持时间。
表1
样品 压力 温度
实施例1 6.8GPa 1300℃
实施例2 6.8GPa 1450℃
实施例3 5.5GPa 1300℃
实施例4 5.5GPa 1450℃
实施例5 5.0GPa 1300℃
通过X射线衍射(XRD)和扫描电子显微术(SEM)分析烧结材料，发现烧结良好。对于实施例1和3，使用边缘倒角和珩磨制备10×10mm正方形样品，3.2mm厚，以产生用于温和间断(所谓的H15)硬质零件机加工测试的工具。采用稍微更连续的条件(所谓的H10间断机加工)并且在这些条件下测试相同的样品，在工件上进行20个道次并测量月牙洼磨损最大深度(Kt)作为所谓化学磨损的指示。
连续机加工由连续接触工件持续连续时间段的工具定义，导致在工具尖端处的热量和压力产生。这种与工件的接合导致切削作用，该切削作用以切屑形式去除工件材料，该切屑流过PCBN工具顶面的表面(称为前刀面)。通过各种机制，包括cBN的氧化、hBN形成和从PCBN基质相到工件的质量传输，在工具前刀面上的PCBN工具磨损被称为月牙洼磨损。由于所提出的磨损机制主要是扩散和化学性质，因此月牙洼磨损通常与化学磨损同义。存在较高程度的连续机加工的应用中，与较高cBN含量的材料相比，用于机加工这些工件的PCBN中的较低cBN含量通常表现地更好。这与在工具-工件界面处的高温条件下hBN形成和与硬化钢工件接触的cBN的氧化有关。
许多切削操作需要工具以连续模式和间断模式机加工零件。工件几何结构中的间隙或空隙称为间断，间断长度与连续机加工的比率连同接合角度决定了机加工操作中的间断程度。
1-40的间断标度定义如下：连续应用在1-5范围内，10-20表示工件中的温和间断，以及25-40表示较激烈的间断条件。
在温和间断的应用中(H15/H20)，化学磨损导致深月牙洼形成，当PCBN工具遇到被机加工工件中的间隙或间断时，该深月牙洼产生锐利的边缘，有碎裂的危险。这对于温和间断应用提出了大的挑战，其中PCBN工具的成功取决于化学磨损耐受性和抗冲击性或强度之间的平衡。
使用AISI4340硬化钢工件进行温和间断的机加工测试(在间断标度的H15区域中)，在它们中有六个钻孔，表面切削速度为150米/分钟，进给速率为0.15毫米/转并且切削深度为0.2mm。用20微米的磨石，按照SNMN090308S0220样品刀刃规格准备PCBN刀刃。
使用与H15测试类似的条件，但使用三孔面而不是六孔面，进行低间断机加工测试(在间断标度的H10区域中)。
图1比较了在六孔钻孔测试中使用H15条件测试时实施例1和3的工具寿命。这表明在比实施例3更高的压力下烧结的实施例1的性能比实施例3好约50％。
图2比较了在三孔钻孔测试中使用H10条件测试时实施例1和3的月牙洼磨损。这表明以比实施例3更高的压力烧结的实施例1具有显著更低的月牙洼磨损。
对于实施例1至5，使用谢乐计算方法将XRD峰宽度与基质相中的微晶尺寸相关联。表2中所示的结果表明温度是影响陶瓷基质的微晶尺寸的最重要因素。然而，还可以看出，在最高压力下烧结时获得了最低的微晶尺寸。可以看出，温度对微晶尺寸的影响大于压力。应注意，微晶尺寸可以小于晶粒尺寸，因为烧结晶粒可以由多于一个微晶组成。
表2
通过碾磨粉末加工途径制备在Ti0.5N0.5 Al基质组合物中的30体积％cBN和45体积％cBN含量的粉末。以约8吨将粉末压入金属杯中以产生17mm直径的生坯并在带式高压高温设备中烧结。
利用三种不同的烧结循环和两种不同的cBN含量来烧结这些粉末，如表3所示。对于每个实施例，将样品在最高温度下保持19分钟。
表3
样品 cBN体积％ 压力 温度
实施例6 30 6.8GPa 1300℃
实施例6a 45 6.8GPa 1300℃
实施例7 30 6.8GPa 1450℃
实施例7a 45 6.8GPa 1450℃
实施例8 30 5.5GPa 1300℃
实施例8a 45 5.5GPa 1300℃
图3是实施例6a的扫描电子显微图，图4是实施例8a的扫描电子显微图。黑色颗粒是cBN并且较浅的颗粒是基质晶粒。可以看出，在与实施例6a相同的温度但较低的压力下烧结的实施例8a似乎具有在烧结期间生长的大基质晶粒的较宽扩展。可以推断，在烧结期间使用较高的压力限制了较大基质颗粒的生长。
使用SEM分析这些样品以评估陶瓷基质相的颗粒尺寸分布。表4显示了所选实施例的基质相的平均颗粒尺寸。
表4
从表4可以看出，温度对基质相晶粒尺寸的影响最大，但较高的压力能够减轻这种影响。
计划进行三种其它变化以开发用于PCBN的高压力合成途径。这些变化集中于材料组成和预压实方法(烧结前的压实)。预压实是必要的，以确保在最终烧结期间的体积变化最小化。如果在烧结之前密度没有被最大化，则增加的收缩可能导致烧结时压力降低，从而导致cBN转化为六方氮化硼(hBN)和样品开裂。
选择两种粉末组合物变体，一种高cBN含量和一种低cBN含量。高含量变体(实施例9)是平均颗粒尺寸为10μm的90重量％cBN，和平均颗粒尺寸为6μm的10重量％铝。使用共振声学混合器以80G将81g的10μm cBN和9g的铝混合2分钟。
较低含量变体(实施例10)是平均颗粒尺寸为1.3μm的60体积％cBN，具有TiC0.5N0.5的基于陶瓷的基质，向TiC0.5N0.5中添加10质量％的铝作为烧结助剂。使用Resodyn声学混合设备进行干法声学混合，以三个阶段将粉末混合。首先是3.9g铝和35.0g TiCN的基质预混物，随后混合42.2g 1.3μm cBN。然后将基质混合物添加到cBN罐中，然后再次混合。所有混合以80G进行2分钟。
选择三种途径用于预压实，产生三步工艺：手工压入陶瓷杯中，在六面顶压机中冷压实，然后再次在六面顶压机中最终热压实。然而，对于较低cBN含量的变体(实施例10)，在冷压实之前试行液压压实，因此区分实施例10(手工压实)和实施例11(液压压实)。压实步骤汇总在图5中。
液压压实获得2.42g/cm3的生坯密度。
将陶瓷杯置于外包壳中并使用六面顶压机进行压制而不进行任何直接加热，以避免在该阶段烧结。在600MPa下压制样品。提取样品，然后在约7GPa的压力下在1300℃、1800℃和2000℃下热压实。
在热压实之后测量密度时，实施例9的最终密度为3.36g/cm3，实施例10和11的最终密度为3.67g/cm3。较高密度是陶瓷TiC0.5N0.5基质及其较高密度的结果。
通过磨削将料块从它们的hBN杯中取出。然后将所得圆柱体磨成光滑的光洁度。在此之后，使用旋转轴和激光将它们切成圆片。将圆片抛光至3.2mm高度并切出10×10mm的正方形以进行磨损测试。切削另外的片以进行抛磨用于SEM分析。
在实施例10和11的情形中，当从杯中取出时料块破碎。这些碎片不能用于磨损测试，但是通过SEM分析了小的碎片。
使用烧结碎片，获得X射线衍射光谱，如图4和5中所示。由于与实施例10和11相比实施例9的粘合剂化学组成不同，不可能进行直接比较。然而，使用在较低温度下烧结的类似材料作为参考仍然可以得出一些结论。
烧结温度改变cBN与基质相反应的速率。在实施例10和11的情形中，如图6所示，可以看出，当烧结温度升高时，硼化物相变得普遍，这可能是由于硼到基质相中的扩散速率增加。在50.7°2θ处的cBN峰的减小存在也表明了这一点。在较高温度下AlN的相对强度也降低，可能有利于Al形成硼化物。
图7示出在1300℃和2000℃下烧结的实施例9的XRD光谱。除了AlN形成的大量增加之外，这里可以看到极少的差异。未检测到硼化物相。
图8示出使用0.3mm的进给速率、0.2mm的深度、180m/min的切削速度和D2工具钢的工件材料在高度间断条件下进行测试时，在1300℃、1800℃和2000℃下烧结的实施例9的工具寿命。由在2000℃下烧结的材料制成的样品在仅1个道次后遭受工具破裂。这种高度脆性的行为可能是由于基质相中的严重反应和过度的晶粒生长。
已发现，在高温下烧结可以改变PCBN的化学组成。进一步表明，如果采取必要的预压实步骤以减少最终烧结期间的塌缩，则大体积PCBN的烧结是可能的。
放电等离子体烧结(SPS)是一种允许快速烧结PCBN的技术。向生坯施加脉冲直流电流，这允许极高的加热速率和冷却速率。该工艺的快速性允许快速致密化，同时使烧结过程期间的晶粒生长最小化。当施加到PCBN时，SPS的另一个优点是该快速性减少cBN向hBN的转化，该转化原本在相对低的压力(小于3GPa)下发生。
进行初始实验，该实验表明，cBN含量大于约30体积％且细于5-10μm的SPS烧结样品产生显著的hBN形成。
表5示出使用SPS在80MPa的压力下制备的PCBN的示例性数据，表6示出在不同压力下使用SPS制备的PCBN的示例性数据。所有样品显示出在85重量％TiC/15重量％Al的基质中的cBN体积％，并且对于80MPa样品以20mm的样品尺寸进行，对于其它样品以6mm的样品尺寸进行。
表5
粉末中cBN的百分比以体积％给出。
图9示出实施例12-21的XRD光谱。在31°2θ附近的峰来自于hBN相，表明发生了cBN向hBN的一些转化。
此外，表5中所示的密度数据说明了SPS过程期间的致密化程度以及hBN的形成，因为hBN具有约2.1g cm-3的密度并且cBN具有约3.45g cm-3的密度；因此，较低的密度表明较高程度的hBN转化。
表6
表6的第三列中给出的时间是材料保持在最高温度下的时间，第2列中cBN的％以体积％给出。
考虑到表5和6以及图11和12中报道的PCBN压块的结果，随后cBN含量保持不高于30体积％并且使用10μm的平均颗粒尺寸。烧结的时间和压力如表7所示变化。
表7
实施例35至52使用30体积％的cBN。用30:70mol Ti:Al+85％(0.5:0.5mol TiN:TiC)的基质制备实施例35至43，使用2:3mol Ti:Si(金属粉末)和85％TiN/TiC的基质制备实施例44至52。对于实施例51，在1000℃和1200℃之间的温度将加热速率变为200℃/分钟。
图11示出实施例35至43的维氏硬度数据，图12示出实施例44至53的维氏硬度数据。从图11可以看出，较高的压力改善硬度，可能是由于改善的致密化，而在图12中较高的压力降低了硬度。这被认为是由不同的粘合剂化学成分引起的；在这种情况下，残留硅化合物的形成可能使材料更脆。
图13示出实施例35至43的密度数据，图14示出实施例44至53的密度数据。该趋势对应于图13和14中所示的硬度趋势。
通过碾磨途径制备包含平均颗粒尺寸为10μm的cBN颗粒的30体积％cBN含量粉末。基质材料的组成为85重量％的Ti(C0.5N0.5)0.8和15重量％的70mol％Al/30mol％Ti的组合。首先在1050℃下真空热处理基质材料，然后在己烷中碾磨4小时。将cBN添加到碾磨混合物中并混合另外10分钟。
将最终混合物干燥并在能够以两种不同压力水平(80MPa和1GPa)的SPS压机中以石墨杯装配置烧结。使用的加热速率为100℃/分钟，并且冷却速率为200℃/分钟。使用不同的时间和SPS最高温度，如表8所示：
表8
为了比较不同的基质化学成分，通过碾磨途径制备包含平均颗粒尺寸为10μm的cBN颗粒的30体积％cBN含量粉末。基质材料的组成为85重量％的30mol％TiC0.8和70mol％TiN0.7的组合，以及15重量％的70mol％Al/30mol％Ti的组合。首先在1050℃下真空热处理基质材料，然后在己烷中碾磨4小时。将cBN添加到碾磨混合物中并混合另外10分钟。
将最终混合物干燥并在能够以两种不同压力水平(80MPa和1GPa)的SPS压机中以石墨杯装配置烧结。使用的加热速率为100℃/分钟，并且冷却速率为200℃/分钟。使用SPS的不同时间和最高温度，如表9所示：
表9
图15示出使用SPS在80MPa下烧结的实施例53至58和63至68的硬度数据。图16示出使用SPS在1MPa下烧结的实施例59至62和69至72的硬度数据。图17示出各样品的拉曼光谱。似乎在中等温度(1000℃至1200℃)下使用较高压力(1GPa)的SPS限制了hBN的形成，从而导致改善的密度和硬度。
图18是实施例62的扫描电子显微图，示出均匀的晶粒分布。下表10示出所选实施例的基质晶粒尺寸。
表10
注意，使用振荡滑动测试在干燥条件下以球盘配置对实施例61和43进行测试以测量磨损率，连同在1350℃、5.5GPa下在HPHT工艺中烧结的45体积％cBN的类似参比样品。发现参比样品的磨损率为1.51×10-7mm3/Nm，而实施例43的磨损率为3.23×10-8mm3/Nm并且实施例61的磨损率为2.51×10-8mm3/Nm。因此，SPS样品的磨损率显著低于参比样品。
通常，已发现对于HPHT和SPS烧结，较低的温度抑制晶粒生长。然而，已发现高的压力改善密度并且还在抑制晶粒生长以及在较低温度下实现烧结同时仍然抑制hBN转化中起作用。当使用SPS时，已发现较低的cBN含量和较粗的(>5μm)cBN颗粒会减少hBN向cBN的转化。
注意，出于安全原因，Al(金属形式或预反应形式)在基质前体粉末中可以是粗的(>100nm)，从而导致前体粉末中的较高d90值。然而，在烧结期间，Al熔化并随后以较低的颗粒尺寸凝固。因此，起始粉末的d90值能够高于基质的最终晶粒尺寸。
定义
如本文所用，PCBN材料是指一类超硬材料，其包含分散在包含金属或陶瓷的基质内的cBN晶粒。
如本文所用，“PCBN结构”包括PCBN材料的物体。
“基质材料”应理解为意指完全或部分填充聚晶结构内的孔隙、间隙或间隙区域的基质材料。术语“基质前体粉末”用于指当经受高压高温烧结过程时变为基质材料的粉末。
大量晶粒的多模态尺寸分布应被理解为意指晶粒具有多于一个峰的尺寸分布，每个峰对应于各自的“模态”。可以通过提供多个晶粒的多于一个源来制造多模态聚晶物体，每个源包括具有显著不同的平均尺寸的晶粒，并将来自所述源的晶粒或颗粒混合在一起。在一个实施方案中，PCBN材料可包括具有多模态分布的cBN晶粒。
虽然已经参考实施方案具体显示和描述了本发明，但是本领域的技术人员将理解，在不脱离由所附权利要求书限定的本发明范围的情况下，可以在形式和细节上进行各种改变。例如，尽管所有实施例都使用cBN作为超硬相，但将理解的是，相同的技术可用于分散在基质材料中的其它类型的超硬材料。

Claims (11)

1.一种制造聚晶立方氮化硼PCBN材料的方法，该方法包括：
混合基质前体粉末与30-40体积％的立方氮化硼cBN颗粒，所述基质前体粉末包括平均颗粒尺寸不大于250nm的颗粒，所述基质前体粉末包含铝化合物，所述立方氮化硼cBN颗粒具有至少4μm的平均颗粒尺寸；
使混合颗粒在至少500MPa的压力、不低于1050℃且不高于1500℃的温度和不小于1分钟且不大于3分钟的时间下进行放电等离子体烧结。
2.根据权利要求1所述的方法，其中所述压力为至少1GPa。
3.根据权利要求1或2所述的方法，其中所述温度选自以下任何：不高于1400℃和不高于1300℃。
4.根据权利要求1至3中任一项所述的方法，其中所述时间不超过2分钟。
5.根据权利要求1至4中任一项所述的方法，还包括以每分钟100至500℃的加热速率升温至所述温度。
6.根据权利要求1至5中任一项所述的方法，其中所述基质材料还包含碳和氮中的任何的钛化合物。
7.根据权利要求1至6中任一项所述的方法，其中所述基质材料包括碳氮化钛、碳化钛、氮化钛、二硼化钛、氮化铝和氧化铝中的任何。
8.根据权利要求1至7中任一项所述的方法，其中将所述基质粉末和所述cBN粉末紧密混合的步骤包括湿法声学混合、干法声学混合和碾磨中的任何。
9.根据权利要求1至8中任一项所述的方法，包括提供平均尺寸在0.2和15μm之间的cBN颗粒。
10.根据权利要求1至9中任一项所述的方法，包括提供具有选自以下任何的平均尺寸的cBN颗粒：大于1μm和大于4μm。
11.根据权利要求1至10中任一项所述的制造PCBN材料的方法，包括提供具有多模态平均尺寸分布的cBN颗粒。
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