Ti/AlN/Ti/AlN复合涂层的制备和阻氘性能研究

Preparation and Deuterium Permeation Properties of Ti/AlN/Ti/AlN Multiple Coatings Deposited by Magnetron Sputtering

摘要:

为提高AlN涂层的稳定性和阻氚性能，提出“Ti-AlN”复合结构涂层。采用磁控溅射法在316L不锈钢基体表面制备了结构致密、总厚度约500 nm的Ti/AlN/Ti/AlN复合涂层。对涂层样品进行不同的真空热处理后，采用SEM、XRD、AES等手段分析涂层样品在热处理前后的微观形貌和结构变化，并对样品在200-600 ℃的阻氘性能进行测试和分析。结果表明，仅热处理温度为760 ℃时，Ti-AlN界面反应生成少量的Al3Ti相。在所有涂层样品中，热处理温度为700 ℃、升温速率为1.5 ℃/min的复合涂层表现出最优的阻氘性能，其600 ℃的PRF（Permeation Reduction Factor）高达536。当热处理温度升高至760 ℃或升温速率达到2.5 ℃/min时，表层AlN层的开裂程度更为严重，并导致涂层的阻氘性能显著降低。另外，所有涂层样品的PRF（阻氘性能）均随渗透温度的降低而急剧减小，表明氘气渗透过程中的温度变化会导致复合涂层阻氘性能失效。

Abstract:

To improve the stability and tritium permeation resistance of the AlN single-layer coating, a Ti-AlN system coating is proposed. Ti/AlN/Ti/AlN multiple coatings with a total thickness of about 500 nm were prepared on the substrate surfaces of 316L stainless steel by magnetron sputtering. The coated samples were heat-treated under different conditions, and the microstructure and phase composition before and after heat treatment were analyzed by SEM, XRD, and AES. The deuterium permeation experiment was then conducted for all the samples. The results show that only some amount of Al3Ti products are formed at the Ti-AlN interface for all the coated samples heated at 700 ℃ or 760 ℃ for 4 h. Among all the coated samples, the coated sample with a heating temperature of 700 ℃ and heating rate of 1.5 ℃/min exhibits the best deuterium resistance performance, and its PRF (Permeation Reduction Factor) value at 600 ℃ is 536. When the heating temperature is increased to 760 ℃ or the heating rate increased to 2.5 ℃/min, the cracking of the coating will be aggravated, which lowers the deuterium permeation resistance. On the other hand, with the decrease of the penetration temperature, the PRF values of all the coated samples also decreased sharply, indicating that the deuterium gas penetration process had an obvious failure effect on the coating structure, the mechanism of which needs to be further studied.