CN106591799B - 金刚石涂层的制备方法及金刚石涂层刀片 - Google Patents

金刚石涂层的制备方法及金刚石涂层刀片 Download PDF

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CN106591799B
CN106591799B CN201611233975.4A CN201611233975A CN106591799B CN 106591799 B CN106591799 B CN 106591799B CN 201611233975 A CN201611233975 A CN 201611233975A CN 106591799 B CN106591799 B CN 106591799B
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赵亚晴
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Funik Ultrahard Material Co Ltd
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Abstract

本发明提供了一种金刚石涂层的制备方法,包括以下步骤:先对硬质合金基体进行碱洗处理,然后用水清洗并干燥,得到干净硬质合金基体;将所述干净硬质合金基体放入质量分数为10%~20%的硫酸铜溶液中处理5~30 min,制得含铜过渡层的硬质合金基体;将所述含铜过渡层的硬质合金基体置于纳米金刚石有机悬浮液中超声清洗,得到硬质合金前处理体;采用化学气相沉积法在所述硬质合金前处理体的表面形成金刚石涂层。本发明还提供一种金刚石涂层刀片,其包括采用上述方法制得的铜过渡层和金刚石涂层,由上述方法制备的金刚石涂层与所述硬质合金基体具有较强的结合力,从而使得所述金刚石涂层刀片具有较高的精度和较长的使用寿命。

Description

金刚石涂层的制备方法及金刚石涂层刀片
技术领域
本发明涉及超硬材料领域,具体地,涉及一种金刚石涂层的制备方法及金刚石涂层刀片。
背景技术
金刚石涂层具有接近天然金刚石的硬度、高弹性模量、极高热导率及化学稳定性等优异性能,从而使其在加工铝合金、陶瓷、碳纤维、石墨等非铁材料领域具有广阔的应用前景。硬质合金与金刚石涂层结合,使刀具既表现出金刚石高的硬度和耐磨性,也表现出硬质合金本身良好的抗冲击性和强韧性,加之低制造成本,应用于超精密加工领域,是一种理想的刀具材料。
但是由于硬质合金中粘结相金属钴的催化作用,以及硬质合金与金刚石之间的物理性能的差异,加工过程中金刚石涂层刀片会存在涂层脱落的现象。因此在金刚石涂层前要对基体进行脱钴处理,降低基底表面钴含量。其中酸碱两步法应用最为广泛,但是经过两步法预处理之后,虽然基体表面的粘结相被去除,然而在随后金刚石的沉积过程中,基体内部深层的钴相会不断向沉积界面扩散,并对金刚石形成不良催化作用。此外,酸的腐蚀性较强,溶液配制具有一定的危险性,并且酸腐蚀时间较短通常容易处理不当造成硬质合金基底浪费。
发明内容
有鉴于此,本发明提供一种金刚石涂层的制备方法及一种利用上述制备方法制备的金刚石涂层刀片,以解决上述问题。
具体地,本发明采取如下技术方案:
一种金刚石涂层的制备方法,包括以下步骤:
碱洗 将硬质合金基体置于铁氰化钾、氢氧化钾的混合溶液进行碱洗处理,然后用水清洗并干燥,得到干净硬质合金基体;
铜过渡层制备 将所述干净硬质合金基体放入质量分数为10%~20%的硫酸铜溶液中处理5~30 min,然后用水清洗并干燥,得到含铜过渡层的硬质合金基体;
超声清洗 将所述含铜过渡层的硬质合金基体置于纳米金刚石有机悬浮液中超声清洗10~30 min,取出、干燥,得到硬质合金前处理体;
沉积金刚石 采用化学气相沉积法在所述硬质合金前处理体的表面形成金刚石涂层。
基于上述,在所述碱洗的步骤中,所述铁氰化钾、氢氧化钾的混合溶液中铁氰化钾的质量分数为5%~15%,氢氧化钾的质量分数为10%~25%。
基于上述,所述超声清洗的步骤包括:将平均粒径为20~80 nm的金刚石颗粒加入有机溶剂中,超声混合均匀,制得质量分数为0.1%~0.5%的所述纳米金刚石有机悬浮液;其中,所述有机溶剂为甲醇、乙醇或体积分数为30%叔丁醇溶液。
基于上述,所述沉积金刚石的步骤包括:在压力为1~3 kPa,温度为1000~1500℃的条件下,以H2、CH4为反应气体源,采用热丝化学气相沉积法在所述硬质合金前处理体的表面反应6~8 h,形成所述金刚石涂层。
一种金刚石涂层刀片,包括硬质合金基底刀体和依次设置于所述硬质合金基底刀体表面的铜过渡层和金刚石涂层;所述铜过渡层的厚度为2~4 μm;所述金刚石涂层的厚度为9~12 μm。
基于上述,所述铜过渡层和所述金刚石涂层是通过上述的金刚石涂层的制备方法制备的。
采用冲击磨损试验对所述金刚石涂层的结合能力进行测量,本发明提供的所述金刚石涂层对碳化硅粉的耐冲击时间可达15~20 s。
与现有技术相比,本发明提供的金刚石涂层的制备方法,在所述硬质合金基体表面发生置换反应形成铜过渡层,得到含铜过渡层的硬质合金基体,减少所述硬质合金中钴的含量;采用纳米金刚石有机悬浮液对所述含铜过渡层的硬质合金基体进行超声处理,所述纳米金刚石有机悬浮液使用甲醇、乙醇或体积分数为30%叔丁醇溶液作为溶剂,可以和未参与置换反应的钴发生反应,使所述硬质合金基体脱钴更彻底,从而减少所述硬质合金基体中的钴对金刚石涂层的生长影响;另外,由于所述纳米金刚石有机悬浮液中的金刚石颗粒的粒径比较小,容易被所述含铜过渡层的硬质合金基体的表面吸附,以作为后续沉积所述金刚石涂层的晶核,从而增加金刚石的成核量,有利于所述金刚石涂层的沉积,与所述铜过渡层一起提高了所述金刚石涂层与所述硬质合金基体之间的结合力;本发明还提供一种金刚石涂层刀片,它包括上述铜过渡层和上述金刚石涂层,可以有效提高所述金刚石涂层刀片的耐磨性和使用寿命。
附图说明
图1 是本发明中所述金刚石涂层刀片的结构示意图。
图中:1.硬质合金基底刀体;2.铜过渡层;3.金刚石涂层。
具体实施方式
下面通过具体实施方式,对本发明的技术方案做进一步的详细描述。
实施例1
本实施例提供一种金刚石涂层的制备方法,包括以下步骤:
碱洗 将硬质合金基体置于铁氰化钾、氢氧化钾的混合溶液进行碱洗处理,然后用水清洗并干燥,得到干净硬质合金基体;其中,所述铁氰化钾的质量分数为5%,所述氢氧化钾的质量分数为10%;
铜过渡层制备 将所述干净硬质合金基体放入质量分数为10%的硫酸铜溶液中处理10 min,然后用水清洗并干燥,得到含铜过渡层的硬质合金基体;
超声清洗 将平均粒径为50 nm的金刚石颗粒加入甲醇溶液中,超声混合均匀,制得制得质量分数为0.2%的纳米金刚石有机悬浮液;将所述含铜过渡层的硬质合金基体置于所述纳米金刚石有机悬浮液中超声清洗20 min,取出、干燥,得到硬质合金前处理体;
沉积金刚石 在压力为2 kPa,温度为1000℃的条件下,采用热丝化学气相沉积法,以H2、CH4为反应气体源在所述硬质合金前处理体的表面反应6 h,形成金刚石涂层。
如图1所示,本实施例还提供一种金刚石涂层刀片,包括所述硬质合金基底刀体1和通过本实施例提供的金刚石涂层的制备方法依次设置于所述硬质合金基底刀体表面的铜过渡层2和金刚石涂层3,所述铜过渡层2的厚度为2 μm,所述金刚石涂层3的厚度为10 μm。
实施例2
本实施例与实施例1的不同之处在于:
在所述碱洗的步骤中,所述铁氰化钾的质量分数为10%,所述氢氧化钾的质量分数为20%;
在所述铜过渡层制备的步骤中,将所述干净硬质合金基体放入质量分数为20%的硫酸铜溶液中处理5 min;
在所述超声清洗的步骤中,将平均粒径为80 nm的金刚石颗粒加入乙醇溶液中,超声混合均匀,制得制得质量分数为0.5%的纳米金刚石有机悬浮液;将所述含铜过渡层的硬质合金基体置于所述纳米金刚石有机悬浮液中超声清洗30 min;
所述沉积金刚石的步骤中,在压力为1 kPa,温度为1500℃的条件下,采用热丝化学气相沉积法,以H2、CH4为反应气体源在所述硬质合金前处理体的表面反应8 h,形成金刚石涂层;
如图1所示,所述金刚石涂层刀片中,所述铜过渡层2的厚度为3 μm,所述金刚石涂层3的厚度为12 μm。
实施例3
本实施例与实施例1的不同之处在于:
在所述碱洗的步骤中,所述铁氰化钾的质量分数为15%,所述氢氧化钾的质量分数为25%;
在所述铜过渡层制备的步骤中,将所述干净硬质合金基体放入质量分数为15%的硫酸铜溶液中处理30 min;
在所述超声清洗的步骤中,将平均粒径为20 nm的金刚石颗粒的加入乙醇溶液中,超声混合均匀,制得制得质量分数为0.2%的纳米金刚石有机悬浮液;将所述含铜过渡层的硬质合金基体置于所述纳米金刚石有机悬浮液中超声清洗20 min;
所述沉积金刚石的步骤中,在压力为3 kPa,温度为1250℃的条件下,采用热丝化学气相沉积法,以H2、CH4为反应气体源在所述硬质合金前处理体的表面反应7 h,形成金刚石涂层;
如图1所示,所述金刚石涂层刀片中,所述铜过渡层2的厚度为2 μm,所述金刚石涂层3的厚度为10 μm。
实施例4
本实施例与实施例1的不同之处在于:在所述超声清洗的步骤中,将平均粒径为80nm的金刚石颗粒加入30%叔丁醇溶液中,超声混合均匀,制得制得质量分数为0.1%纳米金刚石有机悬浮液;将所述含铜过渡层的硬质合金基体置于所述纳米金刚石甲醇悬浮液中超声清洗20 min。
对比试验
对比试验提供一种金刚石涂层的制备方法,其与实施例1的不同之处在于:对比试验中所述硬质合金基体直接进行所述沉积金刚石的步骤。
采用冲击磨损试验对实施例1~3和对比试验制得的金刚石涂层进行测试,测试结果如表1所示,实施例1~3制得的金刚石涂层对碳化硅粉的耐冲击时间远大于对比试验,说明本发明提供的金刚石涂层的制备方法可以有效提高所述金刚石涂层与所述硬质合金基体之间的结合力。
表1 实施例1~3和对比试验得到的金刚石涂层的耐冲击测试结果
实施例1 实施例2 实施例3 实施例4 对比试验
耐冲击时间 20 s 16 s 18 s 16 s 8 s
最后应当说明的是:以上实施例仅用以说明本发明的技术方案而非对其限制;尽管参照较佳实施例对本发明进行了详细的说明,所属领域的普通技术人员应当理解:依然可以对本发明的具体实施方式进行修改或者对部分技术特征进行等同替换;而不脱离本发明技术方案的精神,其均应涵盖在本发明请求保护的技术方案范围当中。

Claims (5)

1.一种金刚石涂层的制备方法,包括以下步骤:
碱洗 将硬质合金基体置于铁氰化钾、氢氧化钾的混合溶液进行碱洗处理,然后用水清洗并干燥,得到干净硬质合金基体;
铜过渡层制备 将所述干净硬质合金基体放入质量分数为10%~20%的硫酸铜溶液中处理5~30 min,然后用水清洗并干燥,得到含铜过渡层的硬质合金基体;
超声清洗 将平均粒径为20~80 nm的金刚石颗粒加入有机溶剂中,超声混合均匀,制得质量分数为0.1%~0.5%的所述纳米金刚石有机悬浮液;将所述含铜过渡层的硬质合金基体置于纳米金刚石有机悬浮液中超声清洗10~30 min,取出、干燥,得到硬质合金前处理体;其中,所述有机溶剂为甲醇、乙醇或体积分数为30%叔丁醇溶液;
沉积金刚石 采用化学气相沉积法在所述硬质合金前处理体的表面形成金刚石涂层。
2.根据权利要求1所述的金刚石涂层的制备方法,其特征在于,在所述碱洗的步骤中,所述铁氰化钾、氢氧化钾的混合溶液中铁氰化钾的质量分数为5%~15%,氢氧化钾的质量分数为10%~25%。
3. 根据权利要求2所述的金刚石涂层的制备方法,其特征在于,所述沉积金刚石的步骤包括:在压力为1~3 kPa,温度为1000~1500℃的条件下,以H2、CH4为反应气体源,采用热丝化学气相沉积法在所述硬质合金前处理体的表面反应6~8 h,形成所述金刚石涂层。
4. 一种金刚石涂层刀片,其特征在于,它包括硬质合金基底刀体和依次设置于所述硬质合金基底刀体表面的铜过渡层和金刚石涂层;所述铜过渡层的厚度为2~4 μm;所述金刚石涂层的厚度为9~12 μm。
5.根据权利要求4所述的金刚石涂层刀片,其特征在于,所述铜过渡层和所述金刚石涂层是通过权利要求1~3任一项所述的金刚石涂层的制备方法制备的。
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