CN105253917A - 一种化学气相沉积金属铼用前驱体的制备方法 - Google Patents
一种化学气相沉积金属铼用前驱体的制备方法 Download PDFInfo
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Abstract
本发明公开一种化学气相沉积金属铼用前驱体的制备方法，属于材料制备技术领域；本发明所述方法将ReCl5在氧化气氛中反应，并通过砂芯滤球对反应物、产物进行高效固液气分离，将反应物、反应产物以及废气有效分离，同时将反应产物ReOCl4和ReO3Cl集中于油浴锅加热的收集容器中，待反应完毕后，关闭氧气，保持惰性气体流通，并将管式炉降温，同时加热油浴锅使ReO3Cl挥发进入精馏单元收集，提纯ReOCl4，获得化学气相沉积金属铼用高纯前驱体ReOCl4。本发明所述方法反应效率高，ReOCl4和ReO3Cl通过精馏的方法很进行分离，提高了产物ReOCl4的纯度。
Description
技术领域
本发明公开一种化学气相沉积金属铼用前驱体的制备方法，属于材料制备技术领域，应用于航空用铼铱喷嘴。
背景技术
金属铼熔点高，具有优异的高温力学、抗热疲劳、耐磨、抗腐蚀以及催化等特性，广泛应用于国防、航空航天、电子以及石油化工等领域，如：热离子发射材料，高温发动机推力室喷管等。但由于金属铼熔点较高，一般采用粉末冶金法加工；对于航空用金属铼管，由于工况条件恶劣，采用粉末冶金法制备的材料内部缺陷较多，因此容易生成裂纹失效，有效工作时间减少。化学气相沉积是近年来发展起来的制备高温难加工金属的一种近终成型工艺，所得制品纯度较高，密度接近理论值。美国等技术先进国家采用化学气相沉积法制备成功性能优良的金属铼管，已成功应用于火箭、卫星以及导弹的高温喷管。
目前公开报道的文献指出，一般采用ReCl5作为前驱体，虽然化合物ReCl5沸点为300℃，但其在180℃即开始分解，得到金属铼的另外一种化合物ReCl3。即使温度升到600℃开始化学气相沉积时，化合物ReCl5分解除了得到金属铼外，仍然有产物ReCl3。化合物ReCl3在400℃左右时，又可能得到化合物ReCl5，只有达到1000℃以上时，化合物ReCl3才可能分解为金属铼，而化合物ReCl3可稳定存在于2000℃及以上。因而在整个化学气相沉积工艺中，参数的控制必须兼顾两种化合物的分解，极易影响金属铼的组织结构及性能，以及金属铼的沉积速率和原料的利用率。
而ReOCl4，沸点在220℃，且其气相可一直稳定到700℃不分解。在700℃以上开始分解为金属铼和化合物ReO3Cl，相对化合物ReCl5而言，化合物ReOCl4作为化学气相沉积的前驱体具有以下优点：（1）工艺参数控制简单，因化合物ReO3Cl即使在2000℃以上也不会分解；（2）原料利用率高，可到到60%以上，接近理论利用率66%；（3）沉积速率快，是采用化合物ReCl5的10倍。从此性能以及其饱和蒸汽压的特点考虑，化合物ReOCl4是替代化合物ReCl5作为金属铼气相沉积前驱体的理想替代品。
目前制法ReOCl4的制法较多。其中，一种较好的制备方法是用过量的氯化硫酰在300℃时作用于金属铼，但是该方法制备温度较高且在高温下氯化硫酰容易分解，所以制备效率也较低。此外还可以ReO3与ReCl5、反应制得ReOCl4。但是采用前采用上述方法制备ReOCl4时，ReOCl4会与ReO3反应生成ReCl3和ReO3Cl，使产率降低。
发明内容
本发明的目的在于提供一种化学气相沉积金属铼用前驱体的制备方法，具体包括以下步骤：
（1）将ReCl5置于砂芯滤球的砂芯表面，均匀铺平；
（2）将砂芯滤球置于炉中，通入惰性气体清洗管路，管路清洗结束后稳定通入氧气≥2分钟，启动管式炉，持续通入氧气，以1-5℃/分钟升温速度从室温升温到反应温度120-220℃保温，直至反应结束，反应结束以不产生黄绿色气体Cl2判断；
（3）待反应完毕后，关闭氧气，通入惰性气体直到反应结束，并将管式炉降温至90-100℃保温，同时并将油浴锅温度升高至130-220℃加热使ReO3Cl挥发进入精馏单元收集冷凝为无色液态，分离ReOCl4和ReO3Cl，获得化学气相沉积金属铼用高纯前驱体ReOCl4；最后在保持惰性气体流通状况下，将整个系统降温至室温，分别收集化合物ReOCl4及化合物ReO3Cl；化合物ReOCl4与化合物ReO3Cl以液态形式分别存在于收集器Ⅰ5、收集器Ⅱ6底部。
优选的，本发明所述ReCl5，纯度≥99%。
优选的，本发明所述惰性气体为氮气、氩气或者氦气；在清洗管路过程中，惰性气体压力为0.1-0.6MPa，流量为0.1-2L/分钟，清洗整个管路≥10min。
优选的，本发明所述氧气的纯度≥99.9%，氧气压力为0.1-0.6MPa，流量为0.01-1L/分钟。
在反应过程中可以加热收集容器的油浴锅至温度温度为40-100℃，在反应过程中慢慢收集产物，减少最终精馏过程的时间。
本发明的另一目的在于提供所述的化学气相沉积金属铼用前驱体的制备方法所用装置，包括惰性气体收集器1、氧气收集器2、砂芯滤球3、管式炉4、收集器Ⅰ5、收集器Ⅱ6、精馏管7、加热浴锅8，惰性气体收集器1、氧气收集器2均和砂芯滤球3的一端连通，砂芯滤球3位于管式炉4内，砂芯滤球3的另一端和收集器Ⅰ5连通；收集器Ⅰ5位于加热浴锅8内，收集器Ⅰ5和精馏管7连通，精馏管7的底部和收集器Ⅱ6连通。
优选的，本发明所述惰性气体收集器1出口处设有阀门Ⅰ9、氧气收集器2阀门Ⅱ10，惰性气体收集器1、氧气收集器2汇集后通过阀门Ⅲ11控制。
优选的，本发明所述其特征在于：整个管路系统密闭连接。
本发明采用砂芯滤球装置，构建固液气分离系统，将固态化合物ReCl5与产物ReOCl4和ReO3Cl，以及产物气体Cl2、反应废气进行高效分离；一方面反应物接触面积大，反应效率高，产率高；同时通过精馏系统，将产物ReOCl4和ReO3Cl进行分离，提高产物ReOCl4的纯度；由于整个系统为封闭式气路，工艺参数控制简便，反应速率快，产率高，无杂质污染，产物纯度高。
本发明的技术原理为将ReCl5置于砂芯滤球的砂芯表面，并将砂芯滤球置于管式炉中加热至反应温度，通过调整高纯惰性气体和高纯氧气压力、流量使ReCl5与氧充分反应，并利用砂芯将反应物、产物进行有效的固液气分离，同时将反应产物ReOCl4和ReO3Cl集中于油浴锅加热的收集容器中，待反应完毕后，关闭氧气，保持惰性气体流通，并将管式炉降温，同时加热油浴锅使ReO3Cl挥发进入精馏单元收集，提纯ReOCl4，获得化学气相沉积金属铼用高纯前驱体ReOCl4。
本发明的有益效果：
采用本发明制备ReOCl4使用的ReCl5（熔点226~263℃）性质稳定，在反应温度下为固体粉末且不会发生分解，提高反应的产率；ReCl5与O2反应生成的产物只有ReOCl4和ReO3Cl，在反应温度下为液体，很容易通过砂芯球与未反应的ReCl5分离，从而有利于反应，相对于产物与原料不能及时分离的传统的制备方法，具有反应效率高的特点；此外，ReOCl4和ReO3Cl通过精馏的方法很进行分离，提高了产物ReOCl4的纯度。
附图说明
图1为本发明所用装置的结构示意图。
图中：1-惰性气体收集器；2-氧气收集器；3-砂芯滤球；4-管式炉；5-收集器Ⅰ；6-收集器Ⅱ；7-精馏管；8-加热浴锅；9-阀门Ⅰ；10-阀门Ⅱ；11-阀门Ⅲ。
具体实施方式
下面结合附图和具体实施例对本发明作进一步详细说明，但本发明的保护范围并不限于所述内容。
本发明实施例1~3所用装置如图1所示，包括惰性气体收集器1、氧气收集器2、砂芯滤球3、管式炉4、收集器Ⅰ5、收集器Ⅱ6、精馏管7、加热浴锅8，惰性气体收集器1、氧气收集器2均和砂芯滤球3的一端连通，砂芯滤球3位于管式炉4内，砂芯滤球3的另一端和收集器Ⅰ5连通；收集器Ⅰ5位于加热浴锅8内，收集器Ⅰ5和精馏管7连通，精馏管7的底部和收集器Ⅱ6连通；惰性气体收集器1出口处设有阀门Ⅰ9、氧气收集器2阀门Ⅱ10，惰性气体收集器1、氧气收集器2汇集后通过阀门Ⅲ11控制；本发明所述其特征在于：整个管路系统密闭连接。
实施例1
本实施例所述化学气相沉积金属铼用前驱体的制备方法，具体包括以下步骤：
（1）称取100粉末状ReCl5（纯度≥99%）置于砂芯滤球中，均匀铺平。
（2）将砂芯滤球置于管式炉中，将整个系统管路密闭连接，磨口接头皆用不锈钢夹头固定，检查气密性；启动阀门通入氮气（≥99.9%），进行清洗工艺，氮气压力：0.1MPa，流量：0.1L/分钟，清洗整个管路50分钟；启动阀门通入高纯氧气（≥99.9%），氧气压力：0.1MPa，流量：0.05L/分钟，惰性气体与氧气流量比控制为2：1，稳定供气2分钟；启动管式炉，以1℃/min升温速度从室温升温到120℃保温。
（3）油浴锅温度控制在20℃，化合物ReOCl4与化合物ReO3Cl以液态形式存在于收集容器底部；直至不产生黄绿色气体Cl2，反应结束；关闭高纯氧气阀门，继续通入惰性气体20分钟，管式炉降温至90℃保温；将油浴锅温度升高至130℃，使化合物ReO3Cl挥发进入精馏系统冷凝为无色液态，收集器Ⅰ5底部为深褐色ReOCl4；在保持氮气流通状况下，将整个系统降温至室温，分别收集化合物ReOCl4及化合物ReO3Cl，分别得到61克固态化合物ReOCl4，和22克液态化合物ReO3Cl，ReOCl4产率为96%。
实施例2
本实施例所述化学气相沉积金属铼用前驱体的制备方法，具体包括以下步骤：
（1）称取200粉末状ReCl5（纯度≥99%）置于砂芯滤球中，均匀铺平。
（2）将砂芯滤球置于管式炉中，将整个系统管路密闭连接，磨口接头皆用不锈钢夹头固定，检查气密性；启动阀门通入氩气（≥99.9%），进行清洗工艺，氩气压力：0.6MPa，流量：0.5L/分钟，清洗整个管路20分钟；启动阀门通入高纯氧气（≥99.9%），氧气压力：0.6MPa，流量：0.1L/分钟，惰性气体与氧气流量比控制为5：1，稳定供气10分钟；启动管式炉，以5℃/分钟升温速度从室温升温到220℃保温。
（3）油浴锅温度控制在100℃，化合物ReOCl4与化合物ReO3Cl以液态形式存在于收集容器底部；直至不产生黄绿色气体Cl2，反应结束；关闭高纯氧气阀门，继续通入惰性气体60分钟，管式炉降温至100℃保温；将油浴锅温度升高至220℃，使化合物ReO3Cl挥发进入精馏系统冷凝为无色液态，收集器Ⅰ5底部为深褐色ReOCl4；在保持氩气流通状况下，将整个系统降温至室温，分别收集化合物ReOCl4及化合物ReO3Cl，分别得到120克固态化合物ReOCl4，和90克液态化合物ReO3Cl，ReOCl4产率为95%。
实施例3
本实施例所述化学气相沉积金属铼用前驱体的制备方法，具体包括以下步骤：
（1）称取100粉末状ReCl5（纯度≥99%）置于砂芯滤球中，均匀铺平。
（2）将砂芯滤球置于管式炉中，将整个系统管路密闭连接，磨口接头皆用不锈钢夹头固定，检查气密性；启动阀门通入氦气（≥99.9%），进行清洗工艺，氦气压力：0.3MPa，流量：2L/分钟，清洗整个管路20分钟；启动阀门通入高纯氧气（≥99.9%），氧气压力：0.3MPa，流量：0.5L/分钟，惰性气体与氧气流量比控制为4：1，稳定供气10分钟；启动管式炉，以3℃/分钟升温速度从室温升温到180℃保温。
（3）油浴锅温度控制在95℃，化合物ReOCl4与化合物ReO3Cl以液态形式存在于收集容器底部；直至不产生黄绿色气体Cl2，反应结束；关闭高纯氧气阀门，继续通入惰性气体60分钟，管式炉降温至100℃保温；将油浴锅温度升高至200℃，使化合物ReO3Cl挥发进入精馏系统冷凝为无色液态，收集容器底部为褐红色ReOCl4；在保持氩气流通状况下，将整个系统降温至室温，分别收集化合物ReOCl4及化合物ReO3Cl，分别得到62克固态化合物ReOCl4，和20克液态化合物ReO3Cl，ReOCl4产率为98%。
Claims (7)
1.一种化学气相沉积金属铼用前驱体的制备方法，其特征在于，具体包括以下步骤：
（1）将ReCl5置于砂芯滤球的砂芯表面，均匀铺平；
（2）将砂芯滤球置于炉中，通入惰性气体清洗管路，管路清洗结束后稳定通入氧气≥2分钟，启动管式炉，持续通入氧气，以1-5℃/分钟升温速度从室温升温到反应温度120-220℃保温，直至反应结束；
（3）待反应完毕后，关闭氧气，通入惰性气体直到反应结束，并将管式炉降温至90-100℃保温，同时并将油浴锅温度升高至130-220℃加热使ReO3Cl挥发进入精馏单元收集冷凝为无色液态，分离ReOCl4和ReO3Cl，获得化学气相沉积金属铼用高纯前驱体ReOCl4。
2.根据权利要求1所述化学气相沉积金属铼用前驱体的制备方法，其特征在于：所述ReCl5，纯度≥99%。
3.根据权利要求1所述化学气相沉积金属铼用前驱体的制备方法，其特征在于：所述惰性气体为氮气、氩气或者氦气；在清洗管路过程中，惰性气体压力为0.1-0.6MPa，流量为0.1-2L/分钟，清洗整个管路≥10min。
4.根据权利要求1所述的化学气相沉积金属铼用前驱体的制备方法，其特征在于：所述氧气的纯度≥99.9%，氧气压力为0.1-0.6MPa，流量为0.01-1L/分钟。
5.权利要求1~3所述的化学气相沉积金属铼用前驱体的制备方法所用装置，其特征在于：包括惰性气体收集器（1）、氧气收集器（2）、砂芯滤球（3）、管式炉（4）、收集器Ⅰ（5）、收集器Ⅱ（6）、精馏管（7）、加热浴锅（8），惰性气体收集器（1）、氧气收集器（2）均和砂芯滤球（3）的一端连通，砂芯滤球（3）位于管式炉（4）内，砂芯滤球（3）的另一端和收集器Ⅰ（5）连通；收集器Ⅰ（5）位于加热浴锅（8）内，收集器Ⅰ（5）和精馏管（7）连通，精馏管（7）的底部和收集器Ⅱ（6）连通。
6.根据权利要求5所述化学气相沉积金属铼用前驱体的制备方法所用装置，其特征在于：惰性气体收集器（1）出口处设有阀门Ⅰ（9）、氧气收集器（2）阀门Ⅱ（10），惰性气体收集器（1）、氧气收集器（2）汇集后通过阀门Ⅲ（11）控制。
7.根据权利要求5所述化学气相沉积金属铼用前驱体的制备方法所用装置，其特征在于：整个管路系统密闭连接。
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