CN110387534A - 一种纳米金刚石涂层硬质合金材料的制备方法 - Google Patents
一种纳米金刚石涂层硬质合金材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种纳米金刚石涂层硬质合金材料的制备方法,采用化学气相沉积法在上述硬质合金基体前处理体表面沉积纳米金刚石层,制得纳米金刚石涂层,具体工艺为:在压力为2~15kPa,温度为600℃~2500℃条件下,以H2、CH4或H2、C2H6和Ar为反应气体源在硬质合金基体前处理体上反应5~10小时形成纳米金刚石涂层,其中,CH4和C2H6气体体积分别占总反应气体源体积的1%~5%;所述纳米金刚石涂层中的纳米金刚石颗粒的平均粒径小于100nm;所述纳米金刚石厚度达到6μm以上。本发明通过改变沉积气体压力、气体种类和含量、沉积温度来调控金刚石涂层晶粒大小,通过金刚石涂层晶粒纳米化,实现金刚石涂层韧性和金刚石涂层与硬质合金基体结合性的提升,得到高结合强度。
Description
技术领域
本发明属于材料制备技术领域,主要是涉及一种纳米金刚石涂层硬质合金材料的制备方法。
背景技术
硬质合金材料因具有超高硬度特性被制作成为刀具材料,广泛的应用于机械器件等加工行业中。为了延长硬质合金刀具的使用寿命,通常在其表面覆盖一层金刚石涂层,金刚石涂层硬质合金工具不仅具有金刚石硬度高、摩擦系数低的特点,而且兼备了硬质合金韧性好、成本低、形状适应性强的特点,可以延长刀具的使用寿命,提高加工效率和加工精度。
然而,金刚石涂层与硬质合金基体之间的附着力并不高,很难在硬质合金基体上沉积出附着性很好的金刚石薄膜,从而极大阻碍了该刀具的应用。而导致金刚石薄膜在切削刀具上的粘附性不足的主要原因有:(1)硬质合金基体中的粘结金属钴催化金刚石向石墨转变;(2)金刚石膜与硬质合金基体之间的物理特性(如热膨胀系数、弹性模量等)差异较大,并且两者之间存在较强的残余热应力,造成金刚石薄膜与基体的结合力变差,产生分层。
发明内容
本发明要解决的问题是提供一种通过金刚石涂层晶粒纳米化,实现金刚石涂层韧性和金刚石涂层与机体结合性提升的纳米金刚石涂层硬质合金材料的制备方法。
为解决上述技术问题,本发明采用的技术方案是:一种纳米金刚石涂层硬质合金材料的制备方法,包括以下步骤:
(1)硬质合金基体前处理:将硬质合金基体置于纳米金刚石悬浮液中进行超声清洗30~60min,经干燥处理后获得硬质合金基体前处理体;
(2)沉积纳米金刚石涂层:采用化学气相沉积法在上述硬质合金基体前处理体表面沉积纳米金刚石层,制得纳米金刚石涂层,具体工艺为:在压力为2~15kPa,温度为600℃~2500℃条件下,以H2、CH4或H2、C2H6和Ar为反应气体源在硬质合金基体前处理体上反应5~10小时形成纳米金刚石涂层,其中,CH4和C2H6气体体积分别占总反应气体源体积的1%~5%;所述纳米金刚石涂层中的纳米金刚石颗粒的平均粒径小于100nm;所述纳米金刚石厚度达到6μm以上。
混合气体中氢、碳、氩各元素的比例范围为100∶1~5∶0.5~1。
所述化学气相沉积法为热丝化学气相沉积法或微波等离子体化学气相沉积法。
所述纳米金刚石涂层的表面粗糙度为50~100nm。
本发明通过改变沉积气体压力、气体种类和含量、沉积温度来调控金刚石涂层晶粒大小。同时,本发明采用纳米金刚石悬浮液对其进行超声处理,由于纳米金刚石悬浮液中的金刚石颗粒的粒径比较小,硬质合金基体经过纳米金刚石悬浮液超声清洗后,其表面容易吸附可以作为后续沉积纳米金刚石涂层晶核的小粒径的纳米金刚石颗粒;从而增加纳米金刚石的成核量,有利于纳米金刚石涂层的沉积,通过金刚石涂层晶粒纳米化,实现金刚石涂层韧性和金刚石涂层与硬质合金基体结合性的提升,得到高结合强度。
具体实施方式
下面结合实施例进一步叙述本发明:
实施例1:一种纳米金刚石涂层硬质合金材料的制备方法,包括以下步骤:
(1)硬质合金基体前处理:将硬质合金基体置于纳米金刚石悬浮液中进行超声清洗40min,经干燥处理后获得硬质合金基体前处理体;纳米金刚石悬浮液的制备:将平均粒径为20nm的超纳米金刚石颗粒悬浮在溶剂中,配制成颗粒数目浓度为1020/g的浓超纳米金刚石悬浮液;然后取3mL所述浓超纳米金刚石悬浮液滴入30mL的超纯水中,搅拌均匀进行稀释从而制得所述纳米金刚石悬浮液。
(2)沉积纳米金刚石涂层:采用热丝化学气相沉积法在上述硬质合金基体前处理体表面沉积纳米金刚石层,制得纳米金刚石涂层,具体工艺为:在压力为3kPa,温度为2400℃条件下,以H2、CH4为反应气体源在硬质合金基体前处理体上反应9小时形成纳米金刚石涂层,其中,CH4气体体积分别占总反应气体源体积的3%;所述纳米金刚石涂层中的纳米金刚石颗粒的平均粒径为90nm;所述纳米金刚石厚度达到8μm;混合气体中氢、碳元素的比例范围为100∶3;所述纳米金刚石涂层的表面粗糙度为80nm。
实施例2:一种纳米金刚石涂层硬质合金材料的制备方法,包括以下步骤:
(1)硬质合金基体前处理:将硬质合金基体置于纳米金刚石悬浮液中进行超声清洗50min,经干燥处理后获得硬质合金基体前处理体;纳米金刚石悬浮液的制备:将平均粒径为10nm的超纳米金刚石颗粒悬浮在溶剂中,配制成颗粒数目浓度为1018/g的浓超纳米金刚石悬浮液;然后取4mL所述浓超纳米金刚石悬浮液滴入40mL的超纯水中,搅拌均匀进行稀释从而制得所述纳米金刚石悬浮液。
(2)沉积纳米金刚石涂层:采用微波等离子体化学气相沉积法在上述硬质合金基体前处理体表面沉积纳米金刚石层,制得纳米金刚石涂层,具体工艺为:在压力为14kPa,温度为900℃条件下,以H2、C2H6和Ar为反应气体源在硬质合金基体前处理体上反应9小时形成纳米金刚石涂层,其中,微波功率为10kw,C2H6气体体积分别占总反应气体源体积的1%;所述纳米金刚石涂层中的纳米金刚石颗粒的平均粒径为80nm;所述纳米金刚石厚度达到9μm;混合气体中氢、碳、氩各元素的比例范围为100∶2∶0.5;所述纳米金刚石涂层的表面粗糙度为70nm。
试验证明:(1)本发明所形成的刀具加工石墨材料寿命达到CTF12D水平。(2)本发明所形成的刀具钻削纤维复合材料时,刀具寿命达到国外先进(例如cemecon公司)同类涂层水平。
以上对本发明的实施例进行了详细说明,但所述内容仅为本发明的较佳实施例,不能被认为用于限定本发明的实施范围。凡依本发明范围所作的均等变化与改进等,均应仍归属于本专利涵盖范围之内。
Claims (4)
1.一种纳米金刚石涂层硬质合金材料的制备方法,其特征在于:包括以下步骤:
(1)硬质合金基体前处理:将硬质合金基体置于纳米金刚石悬浮液中进行超声清洗30~60min,经干燥处理后获得硬质合金基体前处理体;
(2)沉积纳米金刚石涂层:采用化学气相沉积法在上述硬质合金基体前处理体表面沉积纳米金刚石层,制得纳米金刚石涂层,具体工艺为:在压力为2~15kPa,温度为600℃~2500℃条件下,以H2、CH4或H2、C2H6和Ar为反应气体源在硬质合金基体前处理体上反应5~10小时形成纳米金刚石涂层,其中,CH4和C2H6气体体积分别占总反应气体源体积的1%~5%;所述纳米金刚石涂层中的纳米金刚石颗粒的平均粒径小于100nm;所述纳米金刚石厚度达到6μm以上。
2.根据权利要求1所述的纳米金刚石涂层硬质合金材料的制备方法,其特征在于:混合气体中氢、碳、氩各元素的比例范围为100∶1~5∶0.5~1。
3.根据权利要求1所述的纳米金刚石涂层硬质合金材料的制备方法,其特征在于:所述化学气相沉积法为热丝化学气相沉积法或微波等离子体化学气相沉积法。
4.根据权利要求1所述的纳米金刚石涂层硬质合金材料的制备方法,其特征在于:所述纳米金刚石涂层的表面粗糙度为50~100nm。
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CN117305805A (zh) * | 2023-09-27 | 2023-12-29 | 上海交通大学 | 基于纳米金刚石涂层的核燃料包壳改性方法 |
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