CN114804869A - 一种溶胶凝胶法合成Hf6Ta2O17粉体的制备方法 - Google Patents
一种溶胶凝胶法合成Hf6Ta2O17粉体的制备方法 Download PDFInfo
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Abstract
本发明涉及一种溶胶凝胶法合成Hf6Ta2O17粉体的制备方法，根据铪元素与钽元素摩尔比为3:1的计量比称取四氯化铪HfCl4和五氯化钽TaCl5，并溶于无水乙醇中，充分搅拌后加入一定量的浓硝酸、聚乙二醇(PEG)和水，在50～70℃条件下加热搅拌形成溶胶；将上述溶胶置于温度为80℃的鼓风干燥箱中充分干燥，并在600～1500℃条件下热处理2～3h，即可获得Hf6Ta2O17粉体。与现有技术相比，本工艺具有操作简单，制备周期短、均匀性好和可制备纳米尺度粉体等优点。
Description
技术领域
本发明属于粉末合成领域，涉及一种溶胶凝胶法合成Hf6Ta2O17粉体的制备方法。
背景技术
碳/碳(C/C)复合材料具有一系列优异的性能，如低密度、高比强和随温度升高不降反升的力学性能，因而广泛应用于航空航天等领域。随着高超声速飞行器的快速发展，机翼前缘、喉衬和发动机喷管等热端部件将会承受更加严苛的环境。但是，C/C复合材料的氧化敏感性严重制约着其在上述领域的应用。在C/C复合材料表面制备超高温陶瓷涂层被认为是一种改善其氧化烧蚀防护性能的有效方式。但是，单相超高温陶瓷涂层因氧化后形成的多孔结构不利于阻碍氧气的扩散，所以其防护效果并不能满足要求。为此，一些低熔点的改性相，如碳化硅(SiC)、碳化钛(TiC)等，在烧蚀后可以形成玻璃相以达到阻碍氧气扩散的效果，因而通常被引入超高温陶瓷涂层。但是，随着烧蚀时间的延长，这些低熔点的玻璃相会出现严重的蒸发，从而导致涂层材料不能为基体提供长时有效的保护。因此，制备一种具有低氧扩散系数和高熔点的改性相成为了解决该问题的有效途径。
文献1“Wang Y,Xiong X,Li G,et al.Preparation and ablation propertiesof Hf(Ta)C co-deposition coating for carbon/carbon composites[J].CorrosionScience,2013,66:177-182.”报道了采用化学气相沉积工艺制备Hf(Ta)C涂层，并发现烧蚀后氧化层中可以检测到Hf6Ta2O17单相固溶体。该固溶体较高的熔点(～2450℃)，较低的热导(～2.89W/m·K)和氧扩散系数是涂层表现出良好烧蚀性能的主要原因。
文献2“Tong M,Chen C,Fu Q,et al.Exploring Hf-Ta-O precipitation uponablation of Hf-Ta-Si-C coating on C/C composites,Journal of the EuropeanCeramic Society,2022,42:2586-2596.”采用化学气相沉积法制备了Hf-Si-C和Hf-Ta-Si-C涂层，并发现Hf-Ta-O玻璃相较Hf-Si-O玻璃相具有更好的化学稳定性。
文献3“Tan Z,Yang Z,Zhu W,et al.Mechanical properties and calcium-magnesium-alumino-silicate(CMAS)corrosion behavior of a promisingHf6Ta2O17ceramic for thermal barrier coatings,Ceramics International,2020,46:25242-25248.”报道了采用固相反应法制备了Hf6Ta2O17陶瓷，该工艺以氧化铪(HfO2)和五氧化二钽(Ta2O5)为原料，在压力为120MPa，温度为1600℃下烧结8h。其缺点是合成温度高、能源消耗大且生产成本高。
文献4“Yang Y,Perepezko J,Zhang C.Oxidation synthesis ofHf6Ta2O17superstructures,Materials Chemistry and Physics,2017,197:154-162.”以Hf和Ta合金为原材料，通过电弧熔炼获得铸块，再经过1500℃的氧化获得Hf6Ta2O17超结构。但该工艺存在操作复杂，成分均匀性难以保证等缺点。
文献5“Li H,Yu Y,Wang S,et al,Low thermal conductivity Hf6Ta2O17ceramics fabricated by solvothermal and pressure-less sintering,CeramicsInternational,2021,47:17711-17718.”通过水热法制备了Hf6Ta2O17粉体，该方法涉及高温高压过程且温压控制严格，因而对生产设备的依赖性较强、技术难度大，很难进行工业化生产。
发明内容
要解决的技术问题
为了避免现有技术的不足之处，本发明提出一种溶胶凝胶法合成Hf6Ta2O17粉体的制备方法，用以克服现有合成工艺操作复杂、合成温度高、制备周期长等问题。此外，相较于现有技术合成的微米级粉体，溶胶凝胶法制备出的Hf6Ta2O17粉体具有纳米尺寸，作为改性相引入超高温陶瓷时可有效提高其剪切强度和断裂韧性。
技术方案
一种溶胶凝胶法合成Hf6Ta2O17粉体的制备方法，其特征在于步骤如下：
步骤1：以摩尔比为3:1的铪元素与钽元素的计量比，称取四氯化铪HfCl4和五氯化钽TaCl5，并溶于无水乙醇中形成混合溶液，将浓硝酸、聚乙二醇PEG和水依次缓慢地添加到混合溶液中并搅拌；
步骤2：将上述混合溶液置于磁力加热搅拌器上加热搅拌至形成溶胶，随后置于鼓风干燥箱中充分干燥；
步骤3：经干燥后的粉末置于刚玉方舟中，放入600～1500℃的马弗炉中热处理2～3h，将处理好的粉末冷却至室温，进行研磨得到Hf6Ta2O17粉体。
所述浓硝酸的浓度为65％～68％。
所述聚乙二醇PEG的相对分子量在180～220。
所述步骤2加热搅拌器的温度为50～70℃。
所述步骤2鼓风干燥箱的温度为80℃。
所述步骤3热处理时的升温速率为4℃/min～10℃/min。
有益效果
本发明提出的一种溶胶凝胶法合成Hf6Ta2O17粉体的制备方法，根据铪元素与钽元素摩尔比为3:1的计量比称取四氯化铪HfCl4和五氯化钽TaCl5，并溶于无水乙醇中，充分搅拌后加入一定量的浓硝酸、聚乙二醇(PEG)和水，在50～70℃条件下加热搅拌形成溶胶；将上述溶胶置于温度为80℃的鼓风干燥箱中充分干燥，并在600～1500℃条件下热处理2～3h，即可获得Hf6Ta2O17粉体。
与现有技术相比，本工艺具有操作简单，制备周期短、均匀性好和可制备纳米尺度粉体等优点，有益效果在于：
1.相较于微米尺度的粉末，本工艺所得为纳米级，作为第二相引入超高温陶瓷中可以有效解决其韧性差的问题；
2.操作简单、制备周期短、不涉及高温高压过程，安全性高；
3.工艺稳定，易于大规模生产。
图1为合成的Hf6Ta2O17粉体的宏观形貌图，从图1可知，本发明制备的陶瓷粉末为白色颗粒；
图2为合成的Hf6Ta2O17粉体的XRD图谱，从图2可知，本发明制备得到的陶瓷粉末纯度和结晶度都较高，且为单相结构。
图3为合成的Hf6Ta2O17粉体的TEM形貌图，从图3可知，粉体尺寸呈纳米级，且Hf、Ta和O元素均匀地分布在颗粒粉体。
附图说明
图1为合成的Hf6Ta2O17粉体的宏观形貌图
图2为合成的Hf6Ta2O17粉体的XRD图谱
图3为合成的Hf6Ta2O17粉体的TEM形貌图
具体实施方式
现结合实施例、附图对本发明作进一步描述：
实施例1：
步骤1：根据铪元素与钽元素摩尔比为3:1的计量比称取四氯化铪HfCl4和五氯化钽TaCl5，并溶于无水乙醇中，充分搅拌15min形成混合溶液；
将浓硝酸、聚乙二醇和水依次缓慢地添加到搅拌中的混合溶液，并剧烈搅拌；
上述浓硝酸的浓度为65％～68％，聚乙二醇(PEG)的相对分子量在180～220；
步骤2：将上述混合溶液置于50～70℃的磁力加热搅拌器上进行加热搅拌至形成溶胶，随后置于80℃的鼓风干燥箱中充分干燥；
步骤3：经干燥后的粉末置于刚玉方舟中，放入800℃的马弗炉中热处理2h，将处理好的粉末冷却至室温，进行充分研磨得到粉体；
所述的升温速率为4℃/min～10℃/min升至800℃，并以随炉冷却的方式降至室温。
实施例2：
步骤1：根据铪元素与钽元素摩尔比为3:1的计量比称取四氯化铪HfCl4和五氯化钽TaCl5，并溶于无水乙醇中，充分搅拌15min形成混合溶液；
将浓硝酸、聚乙二醇(PEG)和水依次缓慢地添加到搅拌中的混合溶液，并剧烈搅拌；
上述浓硝酸的浓度为65％～68％，聚乙二醇(PEG)的相对分子量在180～220；
步骤2：将上述混合溶液置于50～70℃的磁力加热搅拌器上进行加热搅拌至形成溶胶，随后置于80℃的鼓风干燥箱中充分干燥；
步骤3：经干燥后的粉末置于刚玉方舟中，放入1000℃的马弗炉中热处理2h，将处理好的粉末冷却至室温，进行充分研磨得到粉体；
所述的升温速率为4℃/min～10℃/min升至1000℃，并以随炉冷却的方式降至室温。
实施例3：
步骤1：根据铪元素与钽元素摩尔比为3:1的计量比称取四氯化铪HfCl4和五氯化钽TaCl5，并溶于无水乙醇中，充分搅拌15min形成混合溶液；
将浓硝酸、聚乙二醇(PEG)和水依次缓慢地添加到搅拌中的混合溶液，并剧烈搅拌；
上述浓硝酸的浓度为65％～68％，聚乙二醇(PEG)的相对分子量在180～220；
步骤2：将上述混合溶液置于50～70℃的磁力加热搅拌器上进行加热搅拌至形成溶胶，随后置于80℃的鼓风干燥箱中充分干燥；
步骤3：经干燥后的粉末置于刚玉方舟中，放入1500℃的马弗炉中热处理2h，将处理好的粉末冷却至室温，进行充分研磨得到粉体；
所述的升温速率为4℃/min～10℃/min升至1500℃，并以随炉冷却的方式降至室温。
Claims (6)
1.一种溶胶凝胶法合成Hf6Ta2O17粉体的制备方法，其特征在于步骤如下：
步骤1：以摩尔比为3:1的铪元素与钽元素的计量比，称取四氯化铪HfCl4和五氯化钽TaCl5，并溶于无水乙醇中形成混合溶液，将浓硝酸、聚乙二醇PEG和水依次缓慢地添加到混合溶液中并搅拌；
步骤2：将上述混合溶液置于磁力加热搅拌器上加热搅拌至形成溶胶，随后置于鼓风干燥箱中充分干燥；
步骤3：经干燥后的粉末置于刚玉方舟中，放入600～1500℃的马弗炉中热处理2～3h，将处理好的粉末冷却至室温，进行研磨得到Hf6Ta2O17粉体。
2.根据权利要求1所述溶胶凝胶法合成Hf6Ta2O17粉体的制备方法，其特征在于：所述浓硝酸的浓度为65％～68％。
3.根据权利要求1所述溶胶凝胶法合成Hf6Ta2O17粉体的制备方法，其特征在于：所述聚乙二醇PEG的相对分子量在180～220。
4.根据权利要求1所述溶胶凝胶法合成Hf6Ta2O17粉体的制备方法，其特征在于：所述步骤2加热搅拌器的温度为50～70℃。
5.根据权利要求1所述溶胶凝胶法合成Hf6Ta2O17粉体的制备方法，其特征在于：所述步骤2鼓风干燥箱的温度为80℃。
6.根据权利要求1所述溶胶凝胶法合成Hf6Ta2O17粉体的制备方法，其特征在于：所述步骤3热处理时的升温速率为4℃/min～10℃/min。
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