CN113941708A - 一种增强PcBN复合片界面结合能力的制备方法 - Google Patents
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Abstract
本发明提供了一种增强PcBN复合片界面结合能力的制备方法，将立方氮化硼微粉、钛粉、铝粉一起在球磨罐中混合均匀，然后干燥处理，高温真空处理，还原处理，再和表面磁控溅射镀钛的碳化钨‑钴硬质合金组装成块后在六面顶压机中进行高温高压烧结合成聚晶立方氮化硼复合片。钛在烧结体界面处，可与上下层各元素(硼、氮、铝、碳、钴)反应形成化学键合、冶金结合，在过渡层处生成一系列增强相(二硼化钛、碳化钛、氮化碳、钛铝合金、钛钴合金等)，可以平衡聚晶立方氮化硼层与硬质合金层间存在的膨胀系数之差和弹性模量之差，减少界面结合处存在的较大组织应力，根本上解决界面结合不良，增强界面结合能力，提升整体力学性能。
Description
技术领域
本发明属于超硬材料领域，特别涉及一种增强PcBN复合片界面结合能力的制备方法。
背景技术
聚晶立方氮化硼(PcBN)复合片是由cBN微粉、结合剂和硬质合金基体在高温高压下烧结而成。结合了陶瓷层cBN陶瓷相的高硬度、高耐磨性及硬质合金基底层的高韧性、高耐热性，作为高速切削、高效高精加工的超硬刀具被广泛应用于铁族金属加工领域。随着科技的进步以及现代刀具材料的日益发展，数控车床对刀具的要求也是越来越高，国内外对聚晶立方氮化硼复合材料的研究也越来越重视，我国对超硬复合材料的需求不断增加，目前使用的中高端产品目基本需要进口，因此研究PcBN复合片的制备具有重要的意义。
由于陶瓷层和基体合金层的物相差异导致热膨胀系数、弹性模量差异较大，PcBN复合片在高温烧结制备过程容易出现开裂、脱层问题，在连续加工一些加工难度大的材料过程中容易出现崩刃问题，严重情况下甚至会危及生产操作人员的生命安全。
设计在基体表面增加一层强硼强氮化物的金属材料，使陶瓷层与基体层之间生成一层具有梯度结构、耐腐蚀性、细化晶粒及热膨胀系数缓冲作用的过渡层。Ti作为金属，熔点较低，一方面可以起到液态传质作用，从而提高材料的致密性。另一方面在高温下熔融后还可以与基体层中的WC、Co和陶瓷层中的Ti、Al发生物理冶金结合和化学键合。由此可增强聚晶立方氮化硼层和基体层的界面结合。
发明内容
本发明为一种增强PcBN复合片界面结合能力的制备方法，将cBN微粉、Ti粉、Al粉与表面镀钛的硬质合金基体高温高压烧结合成PcBN复合片，在界面处生成由陶瓷层到合金层不同种类的各物相，使其形成一个物相浓度、热膨胀系数、弹性模量梯度过渡的区域，缓解并平衡上下层存在的热膨胀系数和弹性模量差异，减小界面间的残余应力使其结合力加强，界面结合更为紧密。
为实现上述目的，本发明采用如下技术方案来实现。根据本发明提出的一种增强PcBN复合片界面结合能力的制备方法，其包含以下步骤：将立方氮化硼微粉、钛粉、铝粉一起在球磨罐中，加入无水乙醇混合均匀，然后干燥处理，高温真空处理，还原处理。在碳化钨-钴硬质合金表面进行磁控溅射镀钛。最后将混合均匀的粉料与基体合金组装成块在六面顶压机中进行高温高压烧结合成聚晶立方氮化硼复合片。
具体步骤如下：
(1)将立方氮化硼微粉(cBN)、钛粉(Ti)、铝粉(Al)与无水乙醇加入到球磨罐中球磨，得到润湿的混合物料；
(2)将步骤(1)制得的混合物料放入鼓风干燥箱内于高温真空下烘干后取出得到干燥的混合物料；
(3)使用还原性气体对步骤(2)制得的混合物料做还原处理，得到纯净的混合物料；
(4)使用磁控溅射镀膜仪在硬质合金基体表面镀覆一层钛膜，得到表面被钛附着的硬质合金基体；
(5)将步骤(3)制得的混合物料与步骤(4)制得的合金基体组装成标准试样块；
(6)将步骤(5)得到的标准试样块放在六面顶压机中进行高温高压烧结合成，得到界面结合能力增强的聚晶立方氮化硼复合片。
优选的，所述步骤(1)中立方氮化硼微粉(cBN)、钛粉(Ti)、铝粉(Al)在陶瓷层反应生成TiB2-TiN-AlN陶瓷相，牢固的粘结氮化硼颗粒。
优选的，所述步骤(1)中球磨所用球料比为(3～5):1，转速200～250r/min，时间6～8h。
优选的，所述步骤(2)中烘干温度为70～80℃，时间为12～24h，真空度为10-1～10-3Pa。
优选的，所述步骤(3)中还原气体可以是任意一种具有还原性气体，可以是氢气、一氧化碳、硫化氢等。
优选的，所述步骤(4)中所用硬质合金基体为碳化钨-钴硬质合金基体。
优选的，所述步骤(4)中磁控溅射在硬质合金基体表面所镀钛层的厚度为0.6～2.5μm。
优选的，所述步骤(5)中标准试样块的组装方法为隔热式方法。
优选的，所述步骤(6)中烧结工艺参数为：烧结压力为5～5.5GPa，烧结温度为1400～1600℃，保温时间为180～300s。
本发明通过硬质合金基体磁控溅射镀钛增强了PcBN复合片界面结合能力，制备所得的复合片具有硬度高、强度好、韧性高和高的耐磨性等优点，并且有利于提高聚晶立方氮化硼复合片刀具的使用寿命，为相关超硬材料的研究提供有效的实验依据。
附图说明
图1为本发明实施例1制得硬质合金基体镀钛的PcBN复合片超声波扫描图。
图2为本发明对比例1制得硬质合金基体未镀钛的PcBN复合片超声波扫描图。
具体实施方式
以下通过优选实例对本发明工艺做进一步的详细说明，但本发明的保护范围并不局限于此。
实施例1：
本发明一种增强PcBN复合片界面结合能力的制备方法包含以下步骤：
(1)配料：按比例配置cBN、Al、Ti粉。其中立方氮化硼微粉由三个粒度组成，分别为1-2μm、6-8μm、20-25μm，三者重量比为2：1：7，三者占总重的78.67％；铝粉平均粒度为5μm，钛粉平均粒度为5μm，二者占粉末总重的21.33％。
(2)混料：在球磨机上进行球磨，加入乙醇作为混合介质，球磨球料比为5:1，转速250r/min，时间8h；在80℃干燥12h，干燥后过100目筛。
(3)装模：将粉体装入高压合成用的钼杯模具中，直径为14mm。
(4)高温真空处理：在温度为1000℃，真空度为10-2Pa条件下对样品进行处理，时间1小时。
(5)还原处理：在温度为450℃，气氛为氢气的条件下对样品进行氢还原处理，时间0.5h。
(6)表面镀钛：碳化钨-钴硬质合金由92wt％的碳化钨和8wt％的钴组成，直径为14mm，厚度为2.6mm，在其表面进行磁控溅射镀钛，镀钛厚度为1μm。
(7)组装：处理后的样品按照压机所需的组装方式进行组装。
(8)合成：组装好的样品在六面顶压机中经高温高压合成聚晶立方氮化硼复合片，压力5.5GPa，温度1500℃，保温时间5min。
对比例1：
(1)配料：按比例配置cBN、Al、Ti粉。其中立方氮化硼微粉由三个粒度组成，分别为1-2μm、6-8μm、20-25μm，三者重量比为2：1：7，三者占总重的78.67％；铝粉平均粒度为5μm，钛粉平均粒度为5μm，二者占粉末总重的21.33％。
(2)混料：在球磨机上进行球磨，加入乙醇作为混合介质，球磨球料比为5:1，转速250r/min，时间8h；在80℃干燥12h，干燥后过100目筛。
(3)装模：将粉体装入高压合成用的钼杯模具中，直径为14mm。
(4)高温真空处理：在温度为1000℃，真空度为10-2Pa条件下对样品进行处理，时间1小时。
(5)还原处理：在温度为450℃，气氛为氢气的条件下对样品进行氢还原处理，时间0.5h。
(6)组装：处理后的样品与硬质合金基体按照压机所需的组装方式进行组装。
(7)合成：组装好的样品在六面顶压机中经高温高压合成聚晶立方氮化硼复合片，压力5.5GPa，温度1500℃，保温时间5min。
Claims (9)
1.一种增强PcBN复合片界面结合能力的制备方法，其包括以下步骤：
(1)将立方氮化硼微粉(cBN)、钛粉(Ti)、铝粉(Al)与无水乙醇加入到球磨罐中球磨，得到润湿的混合物料；
(2)将步骤(1)制得的混合物料放入鼓风干燥箱内于高温真空下烘干后取出得到干燥的混合物料；
(3)使用还原性气体对步骤(2)制得的混合物料做还原处理，得到纯净的混合物料；
(4)使用磁控溅射镀膜仪在硬质合金基体表面镀覆一层钛膜，得到表面被钛附着的硬质合金基体；
(5)将步骤(3)制得的混合物料与步骤(4)制得的合金基体组装成标准试样块；
(6)将步骤(5)得到的标准试样块放在六面顶压机中进行高温高压烧结合成，得到界面结合能力增强的聚晶立方氮化硼复合片。
2.根据权利要求1所述的制备方法，其特征在于，所述步骤(1)中立方氮化硼微粉(cBN)、钛粉(Ti)、铝粉(Al)在陶瓷层反应生成TiB2-TiN-AlN陶瓷相，牢固的粘结氮化硼颗粒。
3.根据权利要求1所述的制备方法，其特征在于，所述步骤(1)中球磨所用球料比为(3～5):1，转速200～250r/min，时间6～8h。
4.根据权利要求1所述的制备方法，其特征在于，所述步骤(2)中烘干的温度为70～80℃，时间为12～24h，真空度为10-1～10-3Pa。
5.根据权利要求1所述的制备方法，其特征在于，所述步骤(3)中还原气体可以是任意一种具有还原性气体，可以是氢气、一氧化碳、硫化氢等。
6.根据权利要求1所述的制备方法，其特征在于，所述步骤(4)中硬质合金基体为碳化钨-钴硬质合金基体。
7.根据权利要求1所述的制备方法，其特征在于，所述步骤(4)中磁控溅射在硬质合金基体表面所镀钛层的厚度为0.6～2.5μm。
8.根据权利要求1所述的制备方法，其特征在于，所述步骤(5)中标准试样块的组装方法为隔热式方法。
9.根据权利要求1所述的制备方法，其特征在于，所述步骤(6)中高温高压烧结的工艺参数为：烧结压力为5～5.5GPa，烧结温度为1400～1600℃，保温时间为180～300s。
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