邢爽,张敏,杨佳,李秀华,高悦,李亚泽,李思雨,王震.硫酸铜浓度及反应时间对LA103Z镁锂合金PEO膜层热控性能的影响[J].表面技术,2023,52(1):285-297.
XING Shuang,ZHANG Min,YANG Jia,LI Xiu-hua,GAO Yue,LI Ya-ze,LI Si-yu,WANG Zhen.#$NP Effect of CuSO4 Concentration and Reaction Time on the Thermal Control Performance of PEO Coatings on LA103Z Mg-Li Alloy[J].Surface Technology,2023,52(1):285-297
硫酸铜浓度及反应时间对LA103Z镁锂合金PEO膜层热控性能的影响
#$NP Effect of CuSO4 Concentration and Reaction Time on the Thermal Control Performance of PEO Coatings on LA103Z Mg-Li Alloy
  
DOI:10.16490/j.cnki.issn.1001-3660.2023.01.029
中文关键词:  硫酸铜  等离子体电解氧化  热控涂层  LA103Z镁锂合金  色度值  黑色陶瓷膜
英文关键词:CuSO4  plasma electrolytic oxidation  thermal control coating  LA103Z Mg-Li alloy  chroma value  black ceramic coatings
基金项目:国家自然科学基金(51101080);兴辽英才计划青年拔尖人才项目(XYLC1807170);辽宁省百千万人才工程资助项目;大连市科技创新基金项目(2021JJ13FG97)
作者单位
邢爽 辽宁师范大学 物理与电子技术学院,辽宁 大连 116029 
张敏 辽宁师范大学 物理与电子技术学院,辽宁 大连 116029 
杨佳 辽宁师范大学 物理与电子技术学院,辽宁 大连 116029 
李秀华 辽宁师范大学 物理与电子技术学院,辽宁 大连 116029 
高悦 辽宁师范大学 物理与电子技术学院,辽宁 大连 116029 
李亚泽 辽宁师范大学 物理与电子技术学院,辽宁 大连 116029 
李思雨 辽宁师范大学 物理与电子技术学院,辽宁 大连 116029 
王震 辽宁师范大学 物理与电子技术学院,辽宁 大连 116029 
AuthorInstitution
XING Shuang School of Physics and Electronic Technology, Liaoning Normal University, Liaoning Dalian 116029, China 
ZHANG Min School of Physics and Electronic Technology, Liaoning Normal University, Liaoning Dalian 116029, China 
YANG Jia School of Physics and Electronic Technology, Liaoning Normal University, Liaoning Dalian 116029, China 
LI Xiu-hua School of Physics and Electronic Technology, Liaoning Normal University, Liaoning Dalian 116029, China 
GAO Yue School of Physics and Electronic Technology, Liaoning Normal University, Liaoning Dalian 116029, China 
LI Ya-ze School of Physics and Electronic Technology, Liaoning Normal University, Liaoning Dalian 116029, China 
LI Si-yu School of Physics and Electronic Technology, Liaoning Normal University, Liaoning Dalian 116029, China 
WANG Zhen School of Physics and Electronic Technology, Liaoning Normal University, Liaoning Dalian 116029, China 
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中文摘要:
      目的 在LA103Z镁锂合金表面原位生长高吸收率高发射率的黑色陶瓷膜,研究硫酸铜浓度及反应时间对该膜层热防护性能的影响规律,同时建立膜层的色度值与其热控性能的联系。方法 采用等离子体电解氧化技术(PEO),在Na2SiO3电解液体系中,通过调节硫酸铜浓度及反应时间优化膜层性能。采用扫描电镜(SEM)、X射线光电子能谱仪(XPS)、X射线衍射仪(XRD)、CIE颜色系统和能谱仪(EDS)研究膜层的组成和结构。采用分光光度计和红外发射率仪研究膜层的热控性能。结果 PEO膜层主要由MgO和Mg2SiO4相组成。随反应时间及CuSO4浓度的增加,MgO和Mg2SiO4相的衍射峰峰强增加,基体的衍射峰峰强减弱。PEO膜层主要由Mg、O、Si、Na、Cu元素组成,且Cu元素含量随CuSO4浓度的增加而增加。XPS结果表明,膜层中铜主要以一价和二价离子形式存在,可推断膜层中铜是以非晶氧化铜和氧化亚铜的形式存在。PEO膜层具备典型的多孔火山口形貌,孔洞周围稍微突起,膜层与基体紧密结合,无裂缝,具有良好的膜基结合力。膜层微孔数量和孔隙率随CuSO4浓度的增加而增加,随反应时间的延长而减少。随反应时间的延长和CuSO4浓度的增加,膜层厚度和粗糙度增大,反射率降低(0.25~2.5 μm),色度值(L*)由81降低至29,膜层颜色由银灰色逐渐变为浅红,最终变为黑色。当CuSO4质量浓度为1.25 g/L和反应时间为20 min时,膜层吸收率和发射率分别高达0.815 0、0.907 2,此时其热控性能最佳。结论 在电解液中添加CuSO4和适当延长反应时间,可提高LA103Z镁锂合金表面PEO膜层的热控性能,为镁锂合金在航空航天领域的进一步应用奠定了基础。
英文摘要:
      In this work, the black ceramic coatings with high absorption and high emission were grown in situ on the surface of LA103Z magnesium-lithium alloy. The influences of CuSO4 concentration and reaction time on the thermal protection performance of the coatings were studied, and the relationship between the chromaticity value of the coating and its thermal control performance was established. Using plasma electrolytic oxidation technology (PEO), in Na2SiO3 electrolyte system, the coating performance was optimized by adjusting CuSO4 concentration and reaction time. The composition and microstructure of the coatings were determined by using scanning electron microscopy (SEM), X-ray photoelectron spectrometer (XPS), X-ray diffraction (XRD), CIE color system and energy spectrometer (EDS). The thermal control performance of the coatings was investigated by using the Perkin Elmer Lambda ultraviolet-visible near infrared spectrophotometer and TEMP 2000 solar absorption reflectometer. The coatings prepared were mainly composed with MgO and Mg2SiO4 phases. The copper-related compounds, lithium crystalline substances and sodium salts in the coatings all exist in amorphous form. With the increasing of reaction time and CuSO4 concentration, the intensity of diffraction peaks for crystalline phase MgO and Mg2SiO4 in the coatings increased, and that of the matrix Li0.92Mg4.08 decreased. The reason is that the ceramic coatings became thicker. And the position of MgO peak at 42.916° is slightly shifted to the right relative to the standard peak position. The lattice parameter and cell volume corresponding to the (200), (220) and (222) planes of MgO phase increase. The main elements of the PEO coatings are Mg, O, Si, Na, Cu, and the Cu content increases with the increase of CuSO4 concentration. XPS results show that copper exists in the form of monovalent and bivalent ion, indicating that amorphous Cu2O and CuO exist in the coatings. The PEO coatings have a typical porous crater-like structure, with a slight prominent terrace around the pores. The coating is tightly adherent to the substrate without cracks, indicating a higher adhesion force. The number and porosity of micro pores increased with the increase of CuSO4 concentration, but decreased with the prolongation of the reaction time. With the increasing of reaction time and CuSO4 concentration, the thickness and roughness of the coatings increased and the reflectivity decreased (0.25-2.5 μm). The chromaticity value (L) decreased from 81 to 29, and accordingly the coating color gradually transformed from silver gray to light red, finally into black. It is found that the increasing of the thickness and roughness of the PEO coating has a positive effect on the thermal control performance. When the CuSO4 concentration is 1.25 g/L and the reaction time is 20 min, the absorptivity and emissivity of the coating are as high as 0.815 0 and 0.907 2. At this time, the thermal control performance of the coating is the best. Adding CuSO4 into the electrolyte and extending the reaction time appropriately can improve the thermal control performance of the PEO coatings on the surface of LA103Z magnesium lithium alloy, which lays an experimental foundation for the further application of the magnesium-lithium alloy in the aerospace field.
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