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以脉冲激光沉积法沉积制备了立方相负热膨胀ZrW1.5Mo0.5O8薄膜并利用X射线衍射仪(XRD)和场发射扫描电镜对其结构组分、表面形貌和厚度进行表征。采用变温XRD分析了ZrW1.5Mo0.5O8靶材和薄膜的负热膨胀特性。实验结果表明:在1080℃烧结6h制备得的立方相ZrW1.5Mo0.5O8陶瓷靶材,靶材具有较高的纯度和良好的负热膨胀性能,Mo离子掺入后,其α到β相转变温度降低,在30~600℃温度区间内,ZrW1.5Mo0.5O8陶瓷靶材的负热膨胀系数为-7.13×10-6K-1。利用该靶材在500℃时脉冲激光沉积的ZrW1.5Mo0.5O8薄膜为非晶态,薄膜表面平滑致密,厚度约为835nm;非晶膜在1180℃热处理7min后淬火得到立方相ZrW1.5Mo0.5O8薄膜;结晶后的ZrW1.5Mo0.5O8薄膜为多晶膜。在室温到600℃区间内,立方相ZrW1.5Mo0.5O8薄膜的热膨胀系数为-7.7×10-6K-1,α-ZrW1.5Mo0.5O8到β-ZrW1.5Mo0.5O8的相转变温度降至100℃以下。
The cubic negative thermal expansion ZrW1.5Mo0.5O8 thin films were deposited by pulsed laser deposition. The structure, surface morphology and thickness of ZrW1.5Mo0.5O8 films were characterized by X-ray diffraction (XRD) and field emission scanning electron microscopy (SEM). The negative thermal expansion characteristics of ZrW1.5Mo0.5O8 target and thin films were analyzed by XRD. The experimental results show that the cubic ZrW1.5Mo0.5O8 ceramic target sintered at 1080 ℃ for 6h has a high purity and good negative thermal expansion. After the Mo ions are doped, the α to β phase transition temperature Decreases, and the negative thermal expansion coefficient of the ZrW1.5Mo0.5O8 ceramic target is -7.13 × 10 -6 K-1 in the temperature range of 30 to 600 ° C. The ZrW1.5Mo0.5O8 thin film deposited by pulsed laser deposition at 500 ℃ is amorphous, the surface of the film is smooth and compact with a thickness of about 835nm. The amorphous film is quenched after heat treatment at 1180 ℃ for 7min to obtain cubic ZrW1.5Mo0. 5O8 thin film; the crystalline ZrW1.5Mo0.5O8 thin film is a polycrystalline film. The thermal expansion coefficient of the cubic ZrW1.5Mo0.5O8 thin film was -7.7 × 10-6K-1 at room temperature to 600 ℃, and the phase transformation temperature of α-ZrW1.5Mo0.5O8 to β-ZrW1.5Mo0.5O8 decreased to 100 ℃ below.