石永亮,陈存广,郭志猛.Co掺杂ZnO薄膜的制备及其红外反射性能研究[J].表面技术,2020,49(11):184-190.
SHI Yong-liang,CHEN Cun-guang,GUO Zhi-meng.Preparation and Infrared Reflection Properties of Co2+ Doped ZnO Thin Films[J].Surface Technology,2020,49(11):184-190 |
| Co掺杂ZnO薄膜的制备及其红外反射性能研究 |
| Preparation and Infrared Reflection Properties of Co2+ Doped ZnO Thin Films |
| 投稿时间：2019-10-22 修订日期：2020-01-06 |
| DOI：10.16490/j.cnki.issn.1001-3660.2020.11.020 |
| 中文关键词: sol-gel 红外反射率 Co掺杂 ZnO薄膜 |
| 英文关键词:sol-gel method infrared reflectivity Co2+doped ZnO films |
| 基金项目:河北工业职业技术学院预研项目(yzk2020004) |
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| 中文摘要: |
| 目的 提高真空保温管道中红外反射层的红外反射性能。方法 以四水合醋酸钴和二水合乙酸锌为金属离子源，利用溶胶-凝胶法制备了不同Co掺杂量的ZnO溶胶(Zn1–xCoxO，x=0, 0.02, 0.04, 0.06, 0.08, 0.10)。进一步采用提拉法在镜面316L不锈钢表面制备薄膜，经450 ℃退火处理3 h后得到所需样品。利用热重-差示扫描量热法(TG-DSC)表征Zn1–xCoxO凝胶在热处理时发生的干燥、晶化过程。利用X射线衍射仪(XRD)分析表征不同Co掺杂量的薄膜中的物相组成。利用场发射扫描电子显微镜(FE-SEM)观察薄膜表面的微观形貌。利用能谱仪分析(EDS)热处理后薄膜表面的元素分布情况。利用UV-Vis-NIR分光光度计测试涂层的红外反射性能。结果 所得的Zn1–xCoxO溶胶在基体表面铺展良好，经热处理后晶粒分布均匀，表面致密无明显缺陷;涂敷Zn1–xCoxO薄膜后，样品红外反射性能得到明显改善，由纯基体的0.6355提升至最佳值0.8131(其中，x=0.06)。同时，XRD结果表明掺杂并未导致样品物相的改变，薄膜材料仍然保持稳定的六角纤锌矿结构，但随着Co掺杂量的提高，样品在(101)晶面发生择优取向。经28 d 400 ℃有氧热处理后，试样仍能保持0.8018的较高反射率。结论 通过在红外反射层表面涂敷Zn1–xCoxO薄膜，不但可有效提高其红外反射率，还可对内部金属基体起到良好的保护作用，从而提高热力管道的隔热性能和使用寿命。 |
| 英文摘要: |
| The work aims to improve the infrared reflectance of the infrared reflective layer in the vacuum insulation pipeline. ZnO sol doped with different amounts of Co (Zn1–xCoxO, x=0, 0.02, 0.04, 0.06, 0.08, 0.10) were prepared by sol-gel method with cobalt acetate tetrahydrate and zinc acetate dihydrate as metal ion sources. Furthermore, the thin film was prepared on the surface of mirror 316L stainless steel by dipping-coating method, and the final sample was obtained after annealing at 450 ℃ for 3 hours. Thermogravimetric-differential scanning calorimetric (TG-DSC) analysis was used to characterize the drying and crystallization process of Zn1–xCoxO gel during heating treatment. X-ray diffraction (XRD) was used to analyze the phase composition of films with different Co doping amounts. Field emission scanning electron microscope (FE-SEM) was used to observe the microscopic morphology of the film surface. Energy dispersive spectrometer (EDS) was used to analyze the element distribution of the film surface after thermal treatment. UV-Vis-NIR spectrophotometer was used to analyze the infrared reflection performance of the films. The obtained Zn1–xCox sol spread well on the substrate surface, and the crystalline grains were uniformly distributed to form the dense surface after thermal treatment. With the Zn1–xCoxO film, the infrared reflectance of the sample was significantly improved from 0.6355 to the optimum value of 0.8131 (where x=0.06). At the same time, the XRD results showed that the doped sample still maintained a stable hexagonal wurtzite structure. However, with the increase of Co doped amount, the (101) crystal plane showed a preferential orientation. In addition, after aerobic heat treatment at 400 ℃ for 28 days, the sample still maintained a high reflectance of 0.8018. With Zn1–xCoxO film, the infrared reflectance of the reflective layer can be effectively improved, and the internal metallic matrix can also be well protected, thereby the heat insulation performance and service life of the vacuum insulation pipeline are expected to be improved. |
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