CN112853280A - 一种汽轮机叶片的TiSi基纳米复合多层耐水蚀薄膜及其应用 - Google Patents
一种汽轮机叶片的TiSi基纳米复合多层耐水蚀薄膜及其应用 Download PDFInfo
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- 229910008484 TiSi Inorganic materials 0.000 title claims abstract description 56
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Abstract
本发明公开了一种汽轮机叶片的TiSi基纳米复合多层耐水蚀薄膜及其应用，包括依次沉积于汽轮机叶片表面的金属Cr底层、TiSi过渡层、TiSiN耐氧化过渡层及TiCrSiCN耐水蚀薄膜层；TiCrSiCN耐水蚀薄膜层为Ti(CN)和CrN纳米晶与Si3N4和C非晶相的纳米复合结构。清洗汽轮机叶片的表面，再将汽轮机叶片放置到真空腔室内的旋转装置上进行旋转，并进行等离子体清洗，然后再在汽轮机叶片表面采用多弧离子镀物理气相沉积法，依次沉积金属Cr底层、TiSi过渡层、TiSiN耐氧化过渡层及TiCrSiCN耐水蚀薄膜层，完成汽轮机叶片的TiSi基纳米复合多层耐水蚀薄膜制备，操作简单、成本低、绿色环保。
Description
技术领域
本发明涉及材料表面强化、防腐防磨领域，具体为一种汽轮机叶片的TiSi基纳米复合多层耐水蚀薄膜及其应用。
背景技术
作为汽轮机关键部件的叶片在服役工况下经受苛刻的腐蚀和磨损。叶片易发生水蚀、冲蚀磨损，进而诱发裂纹，发生疲劳破坏。常用的汽轮机部件表面防护（或改性）技术主要有扩散处理和表面涂覆层技术。扩散处理是通过改变部件表面的化学成分、渗入或注入某些元素，也可同时附加热处理手段，使表面得以改性，实现耐水蚀、汽蚀、冲蚀磨损，如渗碳、渗氮、渗硼等。表面涂覆层技术是在材料表面镀、涂或用各种物理、化学方法覆盖一层强化层，通常使用的有镀层、堆焊、喷涂、熔覆等。汽轮机尤其是超临界以上汽轮机叶片经常会受到水蚀、汽蚀、固体颗粒冲蚀损伤。国内外大多采用较高硬度的表面渗硼层、离子复合镀膜和热喷涂层等有效抵抗水蚀和固体颗粒冲蚀。渗硼层太薄是其主要缺陷，渗硼工艺需进一步提高。电弧喷涂、超音速火焰喷涂和等离子喷涂层的喷涂过程涉及的步骤多、控制环节多，尤其防腐领域，还需要喷涂封孔剂，显著增加施工量；尤其等离子喷涂的设备较昂贵，灵活性较差，而且高合金粉末材料成本也高，使其工艺的应用受到一定限制。
PVD离子镀膜具备如下优点：镀膜中入射粒子能量高、硬质薄膜的致密度高，可采用多个电弧的蒸发源，提高沉积速率，基材与硬质薄膜界面产生原子扩散构成的过渡层可改善界面性能，降低内应力，膜/基结合强度高，镀膜过程无环境污染。借助大型工业化PVD离子镀设备，采用多元多层和元素梯度化设计，薄膜中各层的成分及性能是逐渐变化的，可增强薄膜与基材的相互匹配，可大大提高薄膜与基体之间的结合强度。多个膜层的界面有效限制柱状晶的生长，而且阻碍位错的运动，改变裂纹的发展方向，提高薄膜的硬度和韧性。相比于单层薄膜，多元多层硬质膜具有更优异的综合性能。
因此研发一种汽轮机叶片表面的纳米复合结构多层耐水蚀薄膜材料及其应用，以提高汽轮机叶片的使用寿命具有重大意义。
发明内容
本发明的目的在于克服现有技术中存在的上述不足，而提供一种汽轮机叶片的TiSi基纳米复合多层耐水蚀薄膜及其应用，操作简单，成本低，并且绿色环保、无污染废水废气产生。
本发明解决上述问题所采用的技术方案是：一种汽轮机叶片的TiSi基纳米复合多层耐水蚀薄膜，其特征在于，包括依次沉积于汽轮机叶片表面的金属Cr底层、TiSi过渡层、TiSiN耐氧化过渡层及TiCrSiCN耐水蚀薄膜层；所述TiCrSiCN耐水蚀薄膜层为Ti(CN)和CrN纳米晶与Si3N4和C非晶相的纳米复合结构。
进一步的，所述TiSi过渡层由Ti元素及Si元素组成。
进一步的，所述TiSiN耐氧化过渡层由Ti元素、Si元素及N元素组成。
进一步的，所述TiCrSiCN耐水蚀薄膜层由Ti元素、Si元素、Cr元素、C元素及N元素组成。
进一步的，金属Cr底层的厚度为0.3μm，TiSi过渡层的厚度为0.5μm，TiSiN耐氧化过渡层的厚度为2μm，TiCrSiCN耐水蚀薄膜层的厚度为10μm。
所述的汽轮机叶片的TiSi基纳米复合多层耐水蚀薄膜的应用，其特征在于，过程如下：清洗汽轮机叶片的表面，再将汽轮机叶片放置到真空腔室内的旋转装置上进行旋转，并进行等离子体清洗，然后再在汽轮机叶片表面采用多弧离子镀物理气相沉积法，依次沉积金属Cr底层、TiSi过渡层、TiSiN耐氧化过渡层及TiCrSiCN耐水蚀薄膜层，完成汽轮机叶片的TiSi基纳米复合多层耐水蚀薄膜制备。
进一步的，采用多弧离子镀物理气相沉积方法沉积金属Cr底层的过程中，向真空腔室内通入流量为300sccm、气压为1.6Pa的Ar气，沉积温度为300℃，沉积过程中以Cr作为沉积靶材，弧电流为56A，偏置电压为16V。
进一步的，采用多弧离子镀物理气相沉积方法沉积TiSi过渡层的过程中，向真空腔室内通入流量为300sccm、气压为1.6Pa的Ar气，沉积温度为300℃，沉积过程中以TiSi作为沉积靶材，弧电流为62A，偏置电压为17V。
进一步的，采用多弧离子镀物理气相沉积方法沉积TiSiN耐氧化过渡层的过程中，向真空腔室内通入N2气和Ar气的混合气体，其中，N2气的流量为380sccm，Ar气的流量为200sccm，混合气体的气压为1.6Pa，沉积温度为300℃，沉积过程中以TiSi合金作为沉积靶材，弧电流为68A，偏置电压18V。
进一步的，采用多弧离子镀物理气相沉积方法沉积TiCrSiCN耐水蚀薄膜层的过程中，向真空腔室内通入N2气、Ar气和CH4气的混合气体，其中，N2气的流量、Ar气的流量和CH4气的流量分别为500sccm、100sccm及200sccm，混合气体的气压为1.1Pa，沉积温度为300℃，沉积过程中以TiSi合金作为沉积靶材，弧电流为74A，偏置电压为19V；Cr作为沉积靶材，弧电流为70A，偏置电压为19V。
本发明采用Cr/TiSi/TiSiN/TiCrSiCN多元多层梯度化设计令薄膜的性能也呈梯度变化。其中TiSiN膜层中Si以非晶Si3N4相的形式存在，并以晶界形式分别包裹TiN晶粒，形成 nc-TiN/α-Si3N4/α-C纳米复合结构，抑制薄膜晶粒的长大趋势，从而得到细小的TiN纳米晶，形成致密态组织，有助于硬度、韧性和耐水蚀性能提高。TiN在2个TiN晶粒之间进行扩散时需要穿越界面上Si3N4和C阻碍，Si3N4和C为非晶结构，原子排列长程无序，在其单元结构中并没有适合粒子扩散的通道，对Ti、N扩散造成很大阻力。因此，TiSiN体系中的晶粒难通过晶粒之间的粒子扩散过程长大，这种纳米复合结构的多层薄膜可兼顾硬度和韧性，有助于耐水蚀性能提高。其中TiCrSiCN膜层中Si以非晶Si3N4相的形式存在，并以晶界形式分别包裹TiCN和CrN晶粒，形成nc-(TiCN+CrN)/α-(Si3N4+C)纳米复合结构，抑制薄膜晶粒的长大趋势，从而得到细小的TiCN和CrN纳米晶，形成致密态组织，有助于硬度、韧性和耐水蚀性能提高。Ti、C、N在TiCN和CrN晶粒之间进行扩散时需要穿越界面上Si3N4和C阻碍，Si3N4和C为非晶结构，原子排列长程无序，在其单元结构中并没有适合粒子扩散的通道，对Ti、Cr、C、N扩散造成很大阻力。因此，TiCrSiCN体系中的晶粒难通过晶粒之间的粒子扩散过程长大，这种纳米复合结构的多层薄膜可兼顾硬度和韧性，有助于薄膜结合强度和耐水蚀性能提高。
本发明与现有技术相比，具有以下优点和效果：
本发明汽轮机叶片的TiSi基纳米复合多层耐水蚀薄膜包括金属Cr底层、TiSi过渡层、TiSiN耐氧化过渡层及TiCrSiCN耐水蚀薄膜层，其中，通过金属Cr底层提高薄膜与汽轮机叶片的结合强度；TiSi过渡层、TiSiN耐氧化过渡层起到成分、组织和性能梯度变化的作用；通过TiCrSiCN耐水蚀薄膜层起到耐蚀作用，从而有效的提高汽轮机叶片的使用寿命。
附图说明
图1为本发明实例中汽轮机叶片的TiSi基纳米复合多层耐水蚀薄膜的结构示意图。
图2为本发明实例中TiCrSiCN耐水蚀薄膜层的XRD谱图。
图3为本发明实例中TiCrSiCN耐水蚀薄膜层中Si元素的XPS谱图。
图4为本发明实例中TiCrSiCN耐水蚀薄膜层中C元素的XPS谱图。
图中：汽轮机叶片1，金属Cr底层2，TiSi过渡层3，TiSiN耐氧化过渡层4，TiCrSiCN耐水蚀薄膜层5。
具体实施方式
下面结合附图并通过实施例对本发明作进一步的详细说明，以下实施例是对本发明的解释而本发明并不局限于以下实施例。
实施例。
参见图1，本实施例中，一种汽轮机叶片的TiSi基纳米复合多层耐水蚀薄膜，包括依次沉积于汽轮机叶片1表面的金属Cr底层2、TiSi过渡层3、TiSiN耐氧化过渡层4及TiCrSiCN耐水蚀薄膜层5；TiCrSiCN耐水蚀薄膜层5为Ti(CN)和CrN纳米晶与Si3N4和C非晶相的纳米复合结构。
具体的，TiSi过渡层3由Ti元素及Si元素组成。TiSiN耐氧化过渡层4由Ti元素、Si元素及N元素组成。TiCrSiCN耐水蚀薄膜层5由Ti元素、Si元素、Cr元素、C元素及N元素组成。金属Cr底层2的厚度为0.3μm，TiSi过渡层3的厚度为0.5μm，TiSiN耐氧化过渡层4的厚度为2μm，TiCrSiCN耐水蚀薄膜层5的厚度为10μm。
汽轮机叶片的TiSi基纳米复合多层耐水蚀薄膜的应用过程如下：清洗汽轮机叶片1的表面，再将汽轮机叶片1放置到真空腔室内的旋转装置上进行旋转，并进行等离子体清洗，然后再在汽轮机叶片1表面采用多弧离子镀物理气相沉积法，依次沉积金属Cr底层2、TiSi过渡层3、TiSiN耐氧化过渡层4及TiCrSiCN耐水蚀薄膜层5，完成汽轮机叶片1的TiSi基纳米复合多层耐水蚀薄膜制备。
其中，采用多弧离子镀物理气相沉积方法沉积金属Cr底层2的过程中，向真空腔室内通入流量为300sccm、气压为1.6Pa的Ar气，沉积温度为300℃，沉积过程中以Cr作为沉积靶材，弧电流为56A，偏置电压为16V。
采用多弧离子镀物理气相沉积方法沉积TiSi过渡层3的过程中，向真空腔室内通入流量为300sccm、气压为1.6Pa的Ar气，沉积温度为300℃，沉积过程中以TiSi作为沉积靶材，弧电流为62A，偏置电压为17V。
采用多弧离子镀物理气相沉积方法沉积TiSiN耐氧化过渡层4的过程中，向真空腔室内通入N2气和Ar气的混合气体，其中，N2气的流量为380sccm，Ar气的流量为200sccm，混合气体的气压为1.6Pa，沉积温度为300℃，沉积过程中以TiSi合金作为沉积靶材，弧电流为68A，偏置电压18V。
采用多弧离子镀物理气相沉积方法沉积TiCrSiCN耐水蚀薄膜层5的过程中，向真空腔室内通入N2气、Ar气和CH4气的混合气体，其中，N2气的流量、Ar气的流量和CH4气的流量分别为500sccm、100sccm及200sccm，混合气体的气压为1.1Pa，沉积温度为300℃，沉积过程中以TiSi合金作为沉积靶材，弧电流为74A，偏置电压为19V；Cr作为沉积靶材，弧电流为70A，偏置电压为19V。
旋转装置包括转架、支撑盘、支撑杆及电机，其中，电机的输出轴与转架相连接，支撑盘通过支撑杆固定于转架上，汽轮机叶片1放置于支撑盘上。
图2为TiCrSiCN耐水蚀薄膜层5的XRD谱图，从图2中可知，其相组成为面心立方结构的Ti(CN)和CrN相的混合物，未发现Si化合物出现。
为确定TiCrSiCN耐水蚀薄膜层5中元素的化学态，对薄膜表面进行XPS谱分析，结果如图3和图4所示。通过曲线数学拟合对元素化学价态进行分析，如图3所示，Si元素主要以非晶态Si3N4形式存在，如图4所示，C元素主要以非晶C为主。结合XRD和XPS结果，可知TiCrSiCN耐水蚀薄膜层5为Ti(CN)纳米晶和CrN纳米晶与非晶相Si3N4和非晶相C纳米复合结构。
本说明书中未作详细描述的内容均属于本领域专业技术人员公知的现有技术。
虽然本发明已以实施例公开如上，但其并非用以限定本发明的保护范围，任何熟悉该项技术的技术人员，在不脱离本发明的构思和范围内所作的更动与润饰，均应属于本发明的保护范围。
Claims (10)
1.一种汽轮机叶片的TiSi基纳米复合多层耐水蚀薄膜，其特征在于，包括依次沉积于汽轮机叶片表面的金属Cr底层、TiSi过渡层、TiSiN耐氧化过渡层及TiCrSiCN耐水蚀薄膜层；所述TiCrSiCN耐水蚀薄膜层为Ti(CN)和CrN纳米晶与Si3N4和C非晶相的纳米复合结构。
2.根据权利要求1所述的汽轮机叶片的TiSi基纳米复合多层耐水蚀薄膜，其特征在于，所述TiSi过渡层由Ti元素及Si元素组成。
3.根据权利要求1所述的汽轮机叶片的TiSi基纳米复合多层耐水蚀薄膜，其特征在于，所述TiSiN耐氧化过渡层由Ti元素、Si元素及N元素组成。
4.根据权利要求1所述的汽轮机叶片的TiSi基纳米复合多层耐水蚀薄膜，其特征在于，所述TiCrSiCN耐水蚀薄膜层由Ti元素、Si元素、Cr元素、C元素及N元素组成。
5.根据权利要求1所述的汽轮机叶片的TiSi基纳米复合多层耐水蚀薄膜，其特征在于，金属Cr底层的厚度为0.3μm，TiSi过渡层的厚度为0.5μm，TiSiN耐氧化过渡层的厚度为2μm，TiCrSiCN耐水蚀薄膜层的厚度为10μm。
6.一种如权利要求1~5中任一项所述的汽轮机叶片的TiSi基纳米复合多层耐水蚀薄膜的应用，其特征在于，过程如下：清洗汽轮机叶片的表面，再将汽轮机叶片放置到真空腔室内的旋转装置上进行旋转，并进行等离子体清洗，然后再在汽轮机叶片表面采用多弧离子镀物理气相沉积法，依次沉积金属Cr底层、TiSi过渡层、TiSiN耐氧化过渡层及TiCrSiCN耐水蚀薄膜层，完成汽轮机叶片的TiSi基纳米复合多层耐水蚀薄膜制备。
7.根据权利要求6所述的汽轮机叶片的TiSi基纳米复合多层耐水蚀薄膜的应用，其特征在于，采用多弧离子镀物理气相沉积方法沉积金属Cr底层的过程中，向真空腔室内通入流量为300sccm、气压为1.6Pa的Ar气，沉积温度为300℃，沉积过程中以Cr作为沉积靶材，弧电流为56A，偏置电压为16V。
8.根据权利要求6所述的汽轮机叶片的TiSi基纳米复合多层耐水蚀薄膜的应用，其特征在于，采用多弧离子镀物理气相沉积方法沉积TiSi过渡层的过程中，向真空腔室内通入流量为300sccm、气压为1.6Pa的Ar气，沉积温度为300℃，沉积过程中以TiSi作为沉积靶材，弧电流为62A，偏置电压为17V。
9.根据权利要求6所述的汽轮机叶片的TiSi基纳米复合多层耐水蚀薄膜的应用，其特征在于，采用多弧离子镀物理气相沉积方法沉积TiSiN耐氧化过渡层的过程中，向真空腔室内通入N2气和Ar气的混合气体，其中，N2气的流量为380sccm，Ar气的流量为200sccm，混合气体的气压为1.6Pa，沉积温度为300℃，沉积过程中以TiSi合金作为沉积靶材，弧电流为68A，偏置电压18V。
10.根据权利要求6所述的汽轮机叶片的TiSi基纳米复合多层耐水蚀薄膜的应用，其特征在于，采用多弧离子镀物理气相沉积方法沉积TiCrSiCN耐水蚀薄膜层的过程中，向真空腔室内通入N2气、Ar气和CH4气的混合气体，其中，N2气的流量、Ar气的流量和CH4气的流量分别为500sccm、100sccm及200sccm，混合气体的气压为1.1Pa，沉积温度为300℃，沉积过程中以TiSi合金作为沉积靶材，弧电流为74A，偏置电压为19V；Cr作为沉积靶材，弧电流为70A，偏置电压为19V。
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