CN116590689B - 一种细长金属管内孔中SiC-ZrC复合涂层的制备方法 - Google Patents
一种细长金属管内孔中SiC-ZrC复合涂层的制备方法 Download PDFInfo
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Abstract
本发明公开了一种细长金属管内孔中SiC‑ZrC复合涂层的制备方法，属于涂层制备技术领域。本发明以硅粉和二氧化硅粉为蒸镀粉料，与CH4或C3H6经原位反应制备内涂层；再以锆粉、氯化钾和氯化锂为蒸镀粉料，与CH4或C3H6经原位反应制备外涂层，形成SiC‑ZrC复合涂层。相较于传统真空蒸镀方法，本发明方法无需高的真空环境，同时降低了生成涂层的反应温度，极大地降低了设备要求。本发明工艺简单，设备要求较低，可快速、高效的制备高性能、耐高温、耐辐照的SiC‑ZrC复合涂层。
Description
技术领域
本发明属于涂层制备技术领域，特别是涉及一种细长金属管内孔中SiC-ZrC复合涂层的制备方法。
背景技术
核燃料元件是核电厂反应堆的核心部件，燃料元件包壳材料是加压水慢化冷却反应堆的关键核心材料之一。反应堆的先进性、安全可靠性和经济性与所用燃料包壳材料的性能密切相关。由于包容着燃料，因此在反应的过程中包壳需要忍受高温、高压、高中子通量的考验。
锆在水中具有优良的耐腐蚀性，中子俘获截面小，是优质的包壳材料，在商业反应堆中得到广泛应用。但在极端情况下，如核电站水冷核反应堆所使用的核燃料棒包壳管材料为锆合金，海啸导致核电站冷却系统故障，锆合金包壳在高温下发生锆水反应，致使燃料棒受损，且在温度高于500℃时，锆合金会丧失其所有的强度。如何提高反应堆的安全性越来越受到大家的广泛关注。
SiC陶瓷具有熔点高，工作温度极限高，在冷却剂丧失事故发生时不会发生危险。同时具有更低的中子吸收截面，可以节省燃料。ZrC陶瓷具有高熔点、导热性好，特别是具有较小的中子吸收能力、耐辐射等特点，使其在高温结构陶瓷材料、复合材料、以及核反应堆包覆燃料颗粒阻挡层等领域中得到了较好的应用。因此，在金属管内径制备具有低中子俘获截面的高性能陶瓷涂层，是目前改进事故容错燃料(ATF，Accident Tolerant Fuel)的候选材料之一。
然而，目前制备SiC-ZrC复合涂层的方法有：采用传统化学气相沉积法进行制备，多采用ZrCl4作为前驱锆源，CH4作为碳源；三氯甲基硅烷(MTS)作为硅源、碳源。但是MTS极易氧化吸潮形成HCl，ZrCl4在空气中极易发生潮解，所以说前面备料等工序需要严格的在真空手套箱中进行操作，步骤繁琐，同时ZrCl4升华温度为300℃左右，极易冷凝在炉膛内或者气路中导致设备堵塞。传统热蒸镀+原位反应法，所需温度较高通常在1800℃以上，易造成金属管变形。上述两种方法，相较于在基体外表面而言，在细长管内表面的涂层制备难度较高，受其尺寸限制(细管径，大长径比)，涂层物质难以进入管腔内部，即使进入，也较难保证涂层的均匀性。
发明内容
针对现有技术中存在的不足，本发明提供一种细长金属管内孔中SiC-ZrC复合涂层的制备方法，本发明方法无需高的真空环境，同时降低了生成涂层的反应温度，极大地降低了设备要求，可快速、高效的制备高性能、耐高温、耐辐照的SiC-ZrC复合涂层。
为实现上述目的，本发明提供了如下方案：
本发明目的之一是提供一种细长金属管内孔中SiC-ZrC复合涂层的制备方法，以硅粉和二氧化硅粉为蒸镀粉料，与CH4或C3H6经原位反应制备内涂层；再以锆粉、氯化钾和氯化锂为蒸镀粉料，与CH4或C3H6经原位反应制备外涂层，形成SiC-ZrC复合涂层。
进一步地，包括如下步骤：
(1)将硅粉和二氧化硅粉于无水乙醇中分散，磁力搅拌30min并超声振荡10min，经干燥得到混合均匀的热蒸镀硅粉料；将热蒸镀硅粉料均匀铺在打孔石墨管内部，将打孔石墨管置于金属管内径，用碳纸将打孔石墨管两端垫高，将金属管放入管式炉中进行蒸镀；
(2)反应结束后取出金属管，将锆粉、氯化钾和氯化锂均匀铺在另一根打孔石墨管内部，将打孔石墨管置于金属管中，用碳纸将打孔石墨管两端垫高，将金属管放入管式炉中进行第二次蒸镀，形成SiC-ZrC复合涂层。
进一步地，所述硅粉纯度≥99.9％，粒度为200目；所述二氧化硅粉纯度≥99％，粒度为200目；所述锆粉纯度≥99.5％，粒度为200目；所述氯化钾和氯化锂纯度均为分析纯，无粒度要求。
进一步地，所述打孔石墨管与金属管等长，内部有较细的孔径。
进一步地，步骤(1)所述硅粉和二氧化硅粉的质量比为1:1。
进一步地，步骤(1)所述蒸镀的条件为：先将炉内真空抽至100Pa以下，以5℃/min的升温速率升温至1250-1600℃，通入气体流量为60-100sccm的CH4或C3H6，调节炉内压力至0.5-1atm，保温0.5-4h，然后随炉冷却，全程使用氩气作为保护气氛。
进一步地，步骤(2)所述锆粉、氯化钾和氯化锂的质量比为80-98:1-10:1-10。
进一步地，步骤(2)所述第二次蒸镀的条件为：先将炉内真空抽至100Pa以下，以5℃/min的升温速率升温至1250-1600℃，通入气体流量为60-100sccm的CH4或C3H6，调节炉内压力至0.5-1atm，保温0.5-4h，然后随炉冷却，全程使用氩气作为保护气氛。
本发明所制备的SiC-ZrC复合涂层主要应用于耐高温、耐辐照反应堆用包壳管材料的制备。
本发明的有益效果：
本发明利用热蒸镀+化学气相沉积的原理，采用物理化学的方法降低了硅源、锆源的蒸发温度，使其在较低温度下可以发生反应，防止高温可能导致的金属软化变形问题。本发明所需粉末无需球磨，整个过程不产生对人体有毒有害的物质。
本发明采用打孔石墨管作为蒸发源，可以有效解决涂层物质难以进入管腔内部，或者即使进入，也较难保证涂层的均匀性问题，等长打孔石墨管保证了涂层物质在细长金属管孔内的均匀性，保证了生成涂层的质量。
本发明的制备方法对设备要求较低，解决了传统真空蒸镀方法需要极高的真空度的气体压力环境，以及物质源不与基材发生反应导致基体结合力弱的问题，克服了传统化学气相沉积过程中，复杂的原料准备操作，以及大量副反应产物生成的不足。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例中所需要使用的附图作简单的介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1为本发明实施例1中SiC涂层的扫描电镜照片；
图2为本发明实施例1中SiC-ZrC复合涂层的扫描电镜照片；
图3为本发明实施例1中SiC涂层的XRD衍射图谱；
图4为本发明实施例1中SiC-ZrC复合涂层的XRD衍射图谱。
具体实施方式
为使本领域技术人员更好地理解本发明的技术方案，下面结合实施例对本发明作进一步详细描述。
实施例1
(1)准备细长钼管，超声清洗30min，鼓风烘干后备用。将硅粉和二氧化硅粉按照1:1的质量比于无水乙醇中分散，使用磁力搅拌器搅拌30min，超声振荡10min，鼓风干燥机中干燥过筛，获得混合均匀的热蒸镀硅粉料；
将热蒸镀硅粉料均匀铺在细长打孔石墨管内部，将细长打孔石墨管置于钼管内径，使用碳纸将石墨管两端垫高，将钼管放入管式炉中进行蒸镀，从室温开始以5℃/min的升温速率升温至1400℃，通入气体流量为80sccm的丙烯后保温2h，然后随炉冷却，全程使用氩气作为保护气氛，得到SiC涂层。SiC涂层的扫描电镜照片见图1，XRD衍射图谱见图3，由图1和图3可知，所制备的SiC涂层分布均匀无裂纹，物相为纯碳化硅相。
(2)反应结束后取出钼管，将锆粉、氯化钾和氯化锂按80:10:10的质量比均匀铺在另一根打孔石墨管内部，将打孔石墨管置于金属管中，使用碳纸将石墨管两端垫高，将钼管放入管式炉中进行蒸镀，从室温开始以5℃/min的升温速率升温至1400℃，通入气体流量为80sccm的丙烯后保温2h，然后随炉冷却，全程使用氩气作为保护气氛，形成SiC-ZrC复合涂层。SiC-ZrC复合涂层的扫描电镜照片见图2，XRD衍射图谱见图4，由图2和图4可知，在SiC涂层上蒸镀所得的ZrC涂层分布均匀且晶粒细小，物相分布为纯ZrC和很小部分的C颗粒。随后使用1.9x1016ion/cm2 Si离子对制备了SiC-ZrC复合内涂层的样品进行离子辐照，并对辐照后的样品进行了显微力学性能分析。辐照后，ZrC晶粒纳米硬度和弹性模量的增加率分别为3.85％、-3.09％；SiC晶粒纳米硬度和弹性模量的增加率分别为9.21％、-7.75％。辐照后SiC-ZrC复合涂层显微力学性能变化不大，表明辐照前后SiC、ZrC的弹性性质并未发生变化，表明碳化物涂层可以起到很好的防护作用。
实施例2
同实施例1，区别在于，步骤(1)和步骤(2)的蒸镀条件均为：从室温开始以5℃/min的升温速率升温至1600℃，通入气体流量为100sccm的CH4后保温4h。
实施例3
同实施例1，区别在于，锆粉、氯化钾和氯化锂的质量比为98:1:1。
以上所述的实施例仅是对本发明的优选方式进行描述，并非对本发明的范围进行限定，在不脱离本发明设计精神的前提下，本领域普通技术人员对本发明的技术方案做出的各种变形和改进，均应落入本发明权利要求书确定的保护范围内。
Claims (1)
1.一种细长金属管内孔中SiC-ZrC复合涂层的制备方法，其特征在于，以硅粉和二氧化硅粉为蒸镀粉料，与CH4或C3H6经原位反应制备内涂层；再以锆粉、氯化钾和氯化锂为蒸镀粉料，与CH4或C3H6经原位反应制备外涂层，形成SiC-ZrC复合涂层；
所述的细长金属管内孔中SiC-ZrC复合涂层的制备方法，包括如下步骤：
(1)将硅粉和二氧化硅粉于无水乙醇中分散，搅拌30min并振荡10min，经干燥得到混合均匀的热蒸镀硅粉料；将热蒸镀硅粉料均匀铺在打孔石墨管内部，将打孔石墨管置于金属管内径，用碳纸将打孔石墨管两端垫高，将金属管放入管式炉中进行蒸镀；
(2)反应结束后取出金属管，将锆粉、氯化钾和氯化锂均匀铺在另一根打孔石墨管内部，将打孔石墨管置于金属管中，用碳纸将打孔石墨管两端垫高，将金属管放入管式炉中进行第二次蒸镀，形成SiC-ZrC复合涂层；
所述步骤(1)中硅粉和二氧化硅粉的质量比为1:1；
所述步骤(1)中蒸镀的条件为：以5℃/min的升温速率升温至1250-1600℃，通入气体流量为60-100sccm的CH4或C3H6后保温0.5-4h，然后随炉冷却，全程使用氩气作为保护气氛；
所述步骤(2)中锆粉、氯化钾和氯化锂的质量比为80-98:1-10:1-10；
所述步骤(2)中第二次蒸镀的条件为：以5℃/min的升温速率升温至1250-1600℃，通入气体流量为60-100sccm的CH4或C3H6后保温0.5-4h，然后随炉冷却，全程使用氩气作为保护气氛。
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