CN113718216A - 一种三元共晶靶材及其制备方法 - Google Patents

一种三元共晶靶材及其制备方法 Download PDF

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CN113718216A
CN113718216A CN202110955085.9A CN202110955085A CN113718216A CN 113718216 A CN113718216 A CN 113718216A CN 202110955085 A CN202110955085 A CN 202110955085A CN 113718216 A CN113718216 A CN 113718216A
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涂溶
章嵩
李其仲
张联盟
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Advanced Engineering Technology Institute Of Zhongshan City And Wuhan University Of Technology
Chaozhou Branch Center Of Guangdong Provincial Laboratory Of Chemistry And Fine Chemicals
Zhongshan Gas Phase Technology Co ltd
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Advanced Engineering Technology Institute Of Zhongshan City And Wuhan University Of Technology
Chaozhou Branch Center Of Guangdong Provincial Laboratory Of Chemistry And Fine Chemicals
Zhongshan Gas Phase Technology Co ltd
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Abstract

本发明公开了一种三元共晶靶材及其制备方法，包括A组分、B组分和C组分粉末，A组分含量为30～50mol％，B组分含量为10～50mol％，C组分含量为20～40mol％，所述A组分为B4C粉末，B组分为TiB2、ZrB2、HfB2、TaB2或NbB2粉末，C组分为SiC粉末。本发明制备的共晶靶材具有更高的致密度，含有更多的元素种类，相分散更均匀，单个靶材就可以引入四种元素，能够减少多元涂层制备时所需工作靶位的数量，降低了镀膜的功耗以及镀膜装备的成本；本发明三元共晶靶材具有良好的导电导热性，可作为常用物理气相沉积技术的靶材使用；同时，靶材自身已具有高硬度、高韧性，使用本发明制备的靶材进行涂层制备时，无需额外加入氮气、乙炔等反应气体，即可使制备的涂层具备与靶材相同的优异性能。

Description

一种三元共晶靶材及其制备方法
技术领域
本发明涉及涂层制备中所需的靶材技术领域，特别是一种三元共晶靶材及其制备方法。
背景技术
由于科学技术的发展，为提升工件整体性能以满足使用需求，采用物理气相沉积技术在基体表面镀覆一层保护涂层材料的技术手段已得到广泛应用。保护涂层由最初的仅含有两种元素的材料转变为含有四种以及四种以上元素的材料。B、C、Si、Y等元素引入涂层中可以有效提升涂层的硬度、耐磨性和抗氧化性等各方面性能。靶材是磁控溅射镀膜技术以及电弧离子镀膜技术制备涂层的原料。由于导电性差、脆性等各种因素，B、C、Si、B4C、SiC等材料通常难以作为上述两种涂层技术的靶材。传统固相烧结法制备的多组分靶材，致密性低，相分散不均匀，不利于涂层的制备。同时，固相烧结法烧结高熔点物质时，所需烧结温度高，对生产设备要求高，制备周期长。
综上所述，提出一种物理气相沉积用三元共晶靶材及其制备方法具有重要意义。
发明内容
针对现有技术中存在的问题，本发明的目的在于提供一种三元共晶靶材及其制备方法。
为解决上述问题，本发明采用如下的技术方案。
一种三元共晶靶材，包括A组分、B组分和C组分粉末，A组分含量为30～50mol％，B组分含量为10～50mol％，C组分含量为20～40mol％，三种组分含量之和为100％，所述A组分为B4C粉末，B组分为TiB2、ZrB2、HfB2、TaB2或NbB2粉末，C组分为SiC粉末。
一种三元共晶靶材的制备方法，包括以下步骤：
1)称取A组分、B组分和C组分粉末，初始A组分含量为30～50mol％，B组分含量为10～50mol％，C组分含量为20～40mol％，三种组分含量之和为100％，该配比范围内的粉末组合经熔炼后的各相分散均匀；
2)通过球磨机将三种组分粉末均匀混合后压制成块状；
3)将成型的块体转移至电弧熔炼炉中，关闭腔体抽真空，运行电弧熔炼炉使原料快速熔化，熔炼一段时间后，熔体随铜板迅速冷却，翻转试样重复熔化冷却步骤3～5次，即得到组分均匀的三元共晶靶材；
其中，所述A组分为B4C粉末，B组分为TiB2、ZrB2、HfB2、TaB2或NbB2粉末，C组分为SiC粉末。
作为本发明的进一步改进，所述A组分、B组分和C组分粉末原料纯度高于99.9wt.％以上，粒径为0.1～10μm。
作为本发明的进一步改进，在步骤2)中，球磨机的球磨混料工艺采用聚乙烯球磨罐、氧化锆球磨介质，球磨时间为1～2h。
作为本发明的进一步改进，在步骤3)中，所述电弧熔炼电流为40～150A，熔炼时间为15～60s。
作为本发明的进一步改进，采用步骤1)至步骤3)所制备的三元共晶靶材微观结构为层片状结构。
作为本发明的进一步改进，采用步骤1)至步骤3)所制备的三元共晶靶材应用于物理气相沉积的靶材。
本发明的有益效果
相比于现有技术，本发明的优点在于：
1.本发明制备的共晶靶材具有更高的致密度，含有更多的元素种类，相分散更均匀，单个靶材就可以引入四种元素，能够减少多元涂层制备时所需工作靶位的数量，降低了镀膜的功耗以及镀膜装备的成本。
2.本发明三元共晶靶材具有良好的导电导热性，可作为常用沉积技术(电弧离子镀膜、直流磁控溅射镀膜)的靶材使用。同时，靶材自身已具有高硬度、高韧性，使用本发明制备的靶材进行涂层制备时，无需额外加入氮气、乙炔等反应气体，即可使制备的涂层具备与靶材相同的优异性能。
附图说明
图1为本发明实施例1所得B4C-TaB2-SiC共晶靶材的背散射电子图像；
图2为本发明实施例2所得B4C-NbB2-SiC共晶靶材的背散射电子图像；
图3为本发明实施例3所得B4C-ZrB2-SiC共晶靶材的背散射电子图像；
图4为本发明实施例4所得B4C-TiB2-SiC共晶靶材的背散射电子图像。
具体实施方式
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述；显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例，基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
一种物理气相沉积用B4C-TaB2-SiC共晶靶材制备方法，具体步骤如下：
1)称取B4C、TaB2和SiC粉末，B4C含量为35mol％，TaB2含量为35mol％，SiC含量为30mol％，粉末原料纯度为99.9wt.％，B4C粉末粒径为5μm，TaB2粉末粉末粒径为5μm，SiC粉末粒径为1μm；
2)通过球磨机将三种组分粉末均匀混合，混合时间为1.5h，然后压制成块状；
3)将成型的块体转移至电弧熔炼炉中，关闭腔体抽真空，运行电弧熔炼炉使原料快速熔化，电流为80A，熔炼时间为30s，熔体随铜板迅速冷却，翻转试样重复熔化冷却步骤5次，即得到组分均匀的B4C-TaB2-SiC共晶靶材。
本实施例所得B4C-TaB2-SiC共晶靶材的背散射电子图见图1，根据B4C-TaB2-SiC材料的背散射电子像的衬度分析可知，图中白色相为TaB2相，黑色相为B4C相，灰色相为SiC相。显微组织为层片状结构，白色TaB2相和灰色SiC相均匀分布在黑色B4C相基质中。
实施例2
一种物理气相沉积用B4C-NbB2-SiC共晶靶材制备方法，具体步骤如下：
1)称取B4C、NbB2和SiC粉末，B4C含量为50mol％，NbB2含量为20mol％，SiC含量为30mol％，粉末原料纯度为99.95wt.％，B4C粉末粒径为0.5μm，NbB2粉末粉末粒径为2μm，SiC粉末粒径为5μm；
2)通过球磨机将三种组分粉末均匀混合，混合时间为1h，然后压制成块状；
3)将成型的块体转移至电弧熔炼炉中，关闭腔体抽真空，运行电弧熔炼炉使原料快速熔化，电流为100A，熔炼时间为30s，熔体随铜板迅速冷却，翻转试样重复熔化冷却步骤4次，即得到组分均匀的B4C-NbB2-SiC共晶靶材。
本实施例所得B4C-NbB2-SiC共晶靶材的背散射电子图见图2，根据B4C-NbB2-SiC材料的背散射电子像的衬度分析可知，图中白色相为NbB2相，黑色相为B4C相，灰色相为SiC相。显微组织为层片状结构，白色NbB2相和灰色SiC相均匀分布在黑色B4C相基质中。
实施例3
一种物理气相沉积用B4C-ZrB2-SiC共晶靶材制备方法，具体步骤如下：
1)称取B4C、ZrB2和SiC粉末，B4C含量为30mol％，ZrB2含量为50mol％，SiC含量为20mol％，粉末原料纯度为99.95wt.％，B4C粉末粒径为10μm，ZrB2粉末粉末粒径为1μm，SiC粉末粒径为1μm；
2)通过球磨机将三种组分粉末均匀混合，混合时间为1h，然后压制成块状；
3)将成型的块体转移至电弧熔炼炉中，关闭腔体抽真空，运行电弧熔炼炉使原料快速熔化，电流为65A，熔炼时间为60s，熔体随铜板迅速冷却，翻转试样重复熔化冷却步骤3次，即得到组分均匀的B4C-ZrB2-SiC共晶靶材。
本实施例所得B4C-ZrB2-SiC共晶靶材的背散射电子图见图3，根据B4C-ZrB2-SiC材料的背散射电子像的衬度分析可知，图中白色相为ZrB2相，黑色相为B4C相，灰色相为SiC相。显微组织为层片状结构，白色ZrB2相和灰色SiC相均匀分布在黑色B4C相基质中。
实施例4
一种物理气相沉积用B4C-TiB2-SiC共晶靶材制备方法，具体步骤如下：
1)称取B4C、TiB2和SiC粉末，B4C含量为40mol％，TiB2含量为10mol％，SiC含量为50mol％，粉末原料纯度为99.95wt.％，B4C粉末粒径为5μm，TiB2粉末粉末粒径为0.5μm，SiC粉末粒径为5μm；
2)通过球磨机将三种组分粉末均匀混合，混合时间为2h，然后压制成块状；
3)将成型的块体转移至电弧熔炼炉中，关闭腔体抽真空，运行电弧熔炼炉使原料快速熔化，电流为150A，熔炼时间为30s，熔体随铜板迅速冷却，翻转试样重复熔化冷却步骤3次，即得到组分均匀的B4C-TiB2-SiC共晶靶材。
本实施例所得B4C-TiB2-SiC共晶靶材的背散射电子图见图4，根据B4C-TiB2-SiC材料的背散射电子像的衬度分析可知，图中白色相为TiB2相，黑色相为B4C相，灰色相为SiC相。显微组织为层片状结构，白色TiB2相和灰色SiC相均匀分布在黑色B4C相基质中。
表1为实施例制备的三元共晶靶材的实验结果。根据测试结果可知，本发明所制备的靶材具有良好的导电导热性能，同时具备良好的韧性以及硬度，有利于靶材的装卸、运输，用其制备的涂层同样具备优异的韧性于硬度。
本发明所列举的各参数上下限取值、区间值都能实现本发明，在此不一一列举实施例。
Figure BDA0003220166350000061
表1
以上所述，仅为本发明较佳的具体实施方式；但本发明的保护范围并不局限于此。任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，根据本发明的技术方案及其改进构思加以等同替换或改变，都应涵盖在本发明的保护范围内。

Claims (7)

1.一种三元共晶靶材，其特征在于，包括A组分、B组分和C组分粉末，A组分含量为30～50mol％，B组分含量为10～50mol％，C组分含量为20～40mol％，三种组分含量之和为100％，所述A组分为B4C粉末，B组分为TiB2、ZrB2、HfB2、TaB2或NbB2粉末，C组分为SiC粉末。
2.一种三元共晶靶材的制备方法，其特征在于，包括以下步骤：
1)称取A组分、B组分和C组分粉末，初始A组分含量为30～50mol％，B组分含量为10～50mol％，C组分含量为20～40mol％，三种组分含量之和为100％，该配比范围内的粉末组合经熔炼后的各相分散均匀；
2)通过球磨机将三种组分粉末均匀混合后压制成块状；
3)将成型的块体转移至电弧熔炼炉中，关闭腔体抽真空，运行电弧熔炼炉使原料快速熔化，熔炼一段时间后，熔体随铜板迅速冷却，翻转试样重复熔化冷却步骤3～5次，即得到组分均匀的三元共晶靶材；
其中，所述A组分为B4C粉末，B组分为TiB2、ZrB2、HfB2、TaB2或NbB2粉末，C组分为SiC粉末。
3.一种三元共晶靶材的制备方法，其特征在于：
所述A组分、B组分和C组分粉末原料纯度高于99.9wt.％以上，粒径为0.1～10μm。
4.根据权利要求2所述的一种三元共晶靶材的制备方法，其特征在于：
在步骤2)中，球磨机的球磨混料工艺采用聚乙烯球磨罐、氧化锆球磨介质，球磨时间为1～2h。
5.根据权利要求2所述的一种三元共晶靶材的制备方法，其特征在于：
在步骤3)中，所述电弧熔炼电流为40～150A，熔炼时间为15～60s。
6.根据权利要求2所述的一种三元共晶靶材的制备方法，其特征在于：
采用步骤1)至步骤3)所制备的三元共晶靶材微观结构为层片状结构。
7.根据权利要求2所述的一种三元共晶靶材的制备方法，其特征在于：
采用步骤1)至步骤3)所制备的三元共晶靶材应用于物理气相沉积的靶材。
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