CN115582544A - 一种高抗冲击韧性聚晶金刚石复合片的制备方法 - Google Patents
一种高抗冲击韧性聚晶金刚石复合片的制备方法 Download PDFInfo
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Abstract
本发明涉及一种高抗冲击韧性聚晶金刚石复合片的制备，属于超硬材料领域。所述制备方法包括以下步骤：a、将多壁碳纳米管置于无水乙醇中进行超声波分散处理；b、将一定量的碳化钨和钴粉均匀混合作为基体原料；将金刚石微粉、钴粉和分散过的多壁碳纳米管均匀混合作为工作层原料，使工作层各物质质量百分比：金刚石为90‑92%，钴粉6%，碳纳米管为2‑4%；聚晶金刚石复合片基体层各物质质量百分比：碳化钨84‑90%，钴10‑16%。c、将混合好的原料分层装入石墨模具中，施加一定压力后进行抽真空处理，通过放电等离子烧结炉制备预复合片。d、将制备好的预复合片置于叶蜡石模具中，在模具外加装叶蜡石环、导电钢圈和触媒片，在六面顶压机中进行高温高压合成实验。通过这种方法制备的聚晶金刚石复合片基体与工作层之间结合紧密，抗冲击韧性相较未添加碳纳米管的聚晶金刚石复合片提高了5‑8.4倍。同时使工作层中金刚石颗粒间“金刚石‑金刚石”键数量增加，增强增韧作用提高。
Description
技术领域
本发明涉及一种高抗冲击韧性聚晶金刚石复合片的制备，属于超硬材料领域。
背景技术
聚晶金刚石复合片（Polystalline Diamond Compacts，简称PDC）是由硬质合金基底和聚晶金刚石层在高温高压的条件下合成的，兼有聚晶金刚石的高耐磨性以及硬质合金的韧性和可焊接性。因其高效率的切割和加工性能被广泛的应用在机械加工、油井钻探、地质勘探和电子元器件封装贴片机等领域。
当前PDC的磨耗比与金刚石的磨耗比已经比较接近，限制PDC应用的主要原因是金刚石层的冲击破坏。想要高耐磨性要求PDC具有高的强度，想要高冲击韧性要求PDC具有一定变形的能力，这两者相互矛盾。想要得到两种性能兼得的PDC材料已经成为当前研究的热点和亟待开拓的领域。
以金属作为粘结剂合成聚晶金刚石复合片在实际应用中存在一定问题：金刚石晶粒之间残存的金属粘结剂的热膨胀系数和金刚石热膨胀系数相差较大，这是金刚石复合片抗冲击韧性下降的主要原因。碳纳米管的弹性模量实验平均值为1.8Tpa。弯曲强度为14.2Gpa，是目前已知的最强纤维。同时，碳纳米管在高温高压条件下能保持自身性能，这就使碳纳米管增强PDC称为可能。碳纳米管增强PDC材料在增韧机理上除了常规的裂纹偏转、拔出效应等之外，还具有其特殊优势。（1）碳纳米管的存在可以增加聚晶金刚石复合片颗粒间直接结和的可能性，以“金刚石-金刚石”键代替“金刚石-金属-金刚石”键，改进颗粒间连接结构，从而起到增强增韧作用。（2）碳纳米管的加入填补了由于热膨胀系数不同导致的粘结剂与金刚石之间的空隙，在金刚石之间形成了“粘结剂-碳纳米管骨架”，从而提高其抗冲击韧性。
发明内容
本发明所要解决的技术问题是提出一种使金刚石复合片具有高冲击韧性的碳纳米管增强聚晶金刚石复合片的制备方法。
为了解决上述技术问题，本发明的高抗冲击韧性聚晶金刚石复合片的合成方法包括以下步骤：
a、将多壁碳纳米管置于无水乙醇中进行超声波分散处理；
b、按照比例准备一定量的金刚石微粉、碳化钨粉末、钴粉和多壁碳纳米管。将一定量的碳化钨和钴粉均匀混合作为基体原料；将金刚石微粉、钴粉和多壁碳纳米管均匀混合作为工作层原料；
c、将步骤b中混合好的原料分层装入石墨模具中，施加一定压力后进行抽真空处理，通过放电等离子烧结炉制备预复合片。
d、将步骤c中制备好的预复合片置于叶蜡石模具中，在模具外加装叶蜡石环、导电钢圈和触媒片，在六面顶压机中进行高温高压合成实验。
本发明所述的聚晶金刚石复合片制备方法中：工作层各物质质量百分比：金刚石为90-92%，钴粉6%，碳纳米管为2-4%；聚晶金刚石复合片基体层各物质质量百分比：碳化钨84-90%，钴10-16%。
本发明所述的聚晶金刚石复合片制备方法中：原料的混合方式为高能球磨。
本发明所述的聚晶金刚石复合片制备方法中：球磨时间为24h，球磨后干燥温度为80-90℃，球磨干燥时间为12-18h。
本发明所诉的聚晶金刚石复合片制备方法中：预复合片工艺参数：烧结温度范围为1400-1600℃；压力为30-50Mpa；真空度1×10-3pa；保温保压时间为5-10min；
本发明所述的聚晶金刚石复合片制备方法中：成品PDC合成工艺参数：烧结温度范围为1400-1600℃；压力为4.0-6.0Gpa；保温保压时间为3-5min。
本发明所述的聚晶金刚石复合片制备方法中：预复合片的制备是采用放电等离子烧结；成品PDC的制备是将预复合片通过六面顶压机再次烧结。
与现有的聚晶金刚石复合片制备方法相比，本发明的优点在于：
（1）采用二次烧结工艺，先烧制预复合片，再将预复合片置于六面顶压力中进行二次烧结。这种方法可以提高基体和工作层的致密度，从而进一步提高耐磨性。
（2）金属粘结剂和金刚石之间相差较大的热膨胀系数会使聚晶金刚石复合片的抗冲击韧性降低。引入碳纳米管作为增强相可以填补由热膨胀系数差异所引起的空隙，形成“粘结剂-碳纳米管高强骨架”，改善空隙中粘结剂的分布形式，从而提高复合片的抗冲击韧性。
（3）碳纳米管的添加使聚晶金刚石颗粒间的间隙显著减少。导致大量聚晶金刚石颗粒直接连接，改善颗粒间连接结构，起到增强增韧作用。
具体实施方式
实施例1：
（1）多壁碳纳米管的分散处理
将多壁碳纳米管放置于200ml无水乙醇溶液中，进行超声波震荡分散，最后放入烘箱内烘干；
（2）合成原料制备
合成原料配方：工作层组成为质量分数为2%的多壁碳纳米管，92%的金刚石，6%的钴粉；基体层组成为质量分数为84%的WC粉和16%钴粉。在使用之前将金刚石表面进行净化处理；组装前的叶蜡石块、叶蜡石环必须先进行焙烧处理，将叶蜡石内部的水分除去；将工作层和基体层的各种粉料分别用无水乙醇湿混，烘干后再进行干混，保存混合后的原料；
（3）预复合片的合成
将均匀混合的工作层和基体层的粉料分别装入石墨模具先进行预压处理：压力为30Mpa，预压制完成后进行抽真空：真空条件为：1×10-3pa，最后进行放电等离子烧结：烧结温度1500℃，升温速率100℃/min，保温保压时间为6min；
(4) 超高压合成
将预复合片放置于叶蜡石块模具中，在模具外加装上叶蜡石环、导电钢圈和触媒片，在六面顶压机中进行超高压高温合成：合成工艺参数为：烧结温度1500℃，烧结压力5Gpa，保温保压时间2.5min。
样品效果：该聚晶金刚石复合片相对于传统烧结方式制备的金刚石复合片，抗冲击韧性约为不添加碳纳米管复合片的5倍。
实施例2：
（1）多壁碳纳米管的分散处理
将多壁碳纳米管放置于200ml无水乙醇溶液中，进行超声波震荡分散，最后放入烘箱内烘干；
（2）合成原料制备
合成原料配方：工作层组成为质量分数为3%的多壁碳纳米管，91%的金刚石，6%的钴粉；基体层组成为质量分数为87%的WC粉和13%钴粉。在使用之前将金刚石表面进行净化处理；组装前的叶蜡石块、叶蜡石环必须先进行焙烧处理，将叶蜡石内部的水分除去；将工作层和基体层的各种粉料分别用无水乙醇湿混，烘干后再进行干混，保存混合后的原料；
（3）预复合片的合成
将均匀混合的工作层和基体层的粉料分别装入石墨模具先进行预压处理：压力为40Mpa，预压制完成后进行抽真空：真空条件为：1×10-3pa，最后进行放电等离子烧结：烧结温度1500℃，升温速率100℃/min，保温保压时间为7min；
(4)超高压合成
将预复合片放置于叶蜡石块模具中，在模具外加装上叶蜡石环、导电钢圈和触媒片，在六面顶压机中进行超高压高温合成：合成工艺参数为：烧结温度1500℃，烧结压力5.5Gpa，保温保压时间3min。
样品效果：该聚晶金刚石复合片相对于传统烧结方式制备的金刚石复合片，抗冲击韧性约为不添加碳纳米管复合片的5.8倍。
实施例3：
（1）多壁碳纳米管的分散处理
将多壁碳纳米管放置于200ml无水乙醇溶液中，进行超声波震荡分散，最后放入烘箱内烘干；
（2）合成原料制备
合成原料配方：工作层组成为质量分数为4%的多壁碳纳米管，90%的金刚石，6%的钴粉；基体层组成为质量分数为85%的WC粉和16%钴粉。在使用之前将金刚石表面进行净化处理；组装前的叶蜡石块、叶蜡石环必须先进行焙烧处理，将叶蜡石内部的水分除去；将工作层和基体层的各种粉料分别用无水乙醇湿混，烘干后再进行干混，保存混合后的原料；
（3）预复合片的合成
将均匀混合的工作层和基体层的粉料分别装入石墨模具先进行预压处理：压力为50Mpa，预压制完成后进行抽真空：真空条件为：1×10-3pa，最后进行放电等离子烧结：烧结温度1500℃，升温速率100℃/min，保温保压时间为8min；
(5) 超高压合成
将预复合片放置于叶蜡石块模具中，在模具外加装上叶蜡石环、导电钢圈和触媒片，在六面顶压机中进行超高压高温合成：合成工艺参数为：烧结温度1550℃，烧结压力6Gpa，保温保压时间3.5min。
样品效果：该聚晶金刚石复合片相对于传统烧结方式制备的金刚石复合片，抗冲击韧性约为不添加碳纳米管复合片的7倍。
实施例4：
（1）多壁碳纳米管的分散处理
将多壁碳纳米管放置于200ml无水乙醇溶液中，进行超声波震荡分散，最后放入烘箱内烘干；
（2）合成原料制备
合成原料配方：工作层组成为质量分数为5%的多壁碳纳米管，89%的金刚石，6%的钴粉；基体层组成为质量分数为84%的WC粉和16%钴粉。在使用之前将金刚石表面进行净化处理；组装前的叶蜡石块、叶蜡石环必须先进行焙烧处理，将叶蜡石内部的水分除去；将工作层和基体层的各种粉料分别用无水乙醇湿混，烘干后再进行干混，保存混合后的原料；
（3）预复合片的合成
将均匀混合的工作层和基体层的粉料分别装入石墨模具先进行预压处理：压力为50Mpa，预压制完成后进行抽真空：真空条件为：1×10-3pa，最后进行放电等离子烧结：烧结温度1500℃，升温速率100℃/min，保温保压时间为10min；
(6) 超高压合成
将预复合片放置于叶蜡石块模具中，在模具外加装上叶蜡石环、导电钢圈和触媒片，在六面顶压机中进行超高压高温合成：合成工艺参数为：烧结温度1600℃，烧结压力6Gpa，保温保压时间4min。
样品效果：该聚晶金刚石复合片相对于传统烧结方式制备的金刚石复合片，抗冲击韧性约为不添加碳纳米管复合片的8.4倍。
Claims (7)
1.一种高抗冲击韧性聚晶金刚石复合片的制备方法，其特征在于：所述合成方法包括以下步骤：
a、将多壁碳纳米管置于无水乙醇中进行超声波分散处理；
b、按照比例准备一定量的金刚石微粉、碳化钨粉末、钴粉和多壁碳纳米管；
将一定量的碳化钨和钴粉均匀混合作为基体原料；将金刚石微粉、钴粉和多壁碳纳米管均匀混合作为工作层原料；
c、将步骤b中混合好的原料分层装入石墨模具中，施加一定压力后进行抽真空处理，通过放电等离子烧结炉制备预复合片；
d、将步骤c中制备好的预复合片置于叶蜡石模具中，在模具外加装叶蜡石环、导电钢圈和触媒片，在六面顶压机中进行高温高压合成实验。
2.根据权利要求1所述的制备聚晶金刚石复合片的方法，其特征在于：工作层各物质质量百分比：金刚石为90-92%，钴粉6%，碳纳米管为2-4%；聚晶金刚石复合片基体层各物质质量百分比：碳化钨84-90%，钴10-16%。
3.根据权利要求1所述的制备聚晶金刚石复合片的方法，其特征在于：原料的混合方式为高能球磨。
4.根据权力要求1所述的制备高抗冲击韧性聚晶金刚石复合片的方法，其特征在于：球磨时间为24h，球磨后干燥温度为80-90℃，球磨干燥时间为12-18h。
5.根据权力要求1所述的制备高抗冲击韧性聚晶金刚石复合片的方法，其特征在于：预复合片工艺参数：烧结温度范围为1400-1600℃；压力为30-50Mpa；真空度1×10-3pa；保温保压时间为5-10min。
6.根据权力要求1所述的制备高抗冲击韧性聚晶金刚石复合片的方法，其特征在于：成品PDC合成工艺参数：烧结温度范围为1400-1600℃；压力为4.0-6.0Gpa；保温保压时间为3-5min。
7.根据权力要求1所述的制备高抗冲击韧性聚晶金刚石复合片的方法，其特征在于：预复合片的制备是采用放电等离子烧结；成品PDC的制备是将预复合片通过六面顶压机再次烧结。
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