陈楠,卜晓晨,熊思琪,雒晓涛,李长久.粉末尺寸对等离子喷涂 Na3Zr2Si2PO12 电解质成分和组织结构的影响[J].热喷涂技术,2023,(1):1~12.
粉末尺寸对等离子喷涂 Na3Zr2Si2PO12 电解质成分和组织结构的影响
The Effect of Particle Size on Composition and Microstructure ofNa3Zr2Si2PO12 Electrolyte Deposited by Air Plasma Spraying
  
DOI:10.3969/j.issn.1674-7127.2023.01-001
中文关键词:  等离子喷涂  NASICON 电解质  Na3Zr2Si2PO12  元素优先蒸发  尺寸效应
英文关键词:Plasma spraying  NASICON electrolyte  Na3Zr2Si2PO12  Preferential vaporization  Particle size effect
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作者单位
陈楠 西安交通大学材料科学与工程学院
卜晓晨 西安交通大学材料科学与工程学院
熊思琪 西安交通大学材料科学与工程学院
雒晓涛 西安交通大学材料科学与工程学院
李长久 西安交通大学材料科学与工程学院
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中文摘要:
      全固态钠离子电池由于安全性和元素丰度等天然优势, 在大规模储能领域具有巨大的应用潜力。 全固态电 池的核心是固态电解质, NASICON 型的 Na3Zr2Si2PO12(NZSP) 电解质因为离子电导率高、 热稳定性与力学性能优 异等优点而受到广泛关注。 本研究采用大气等离子喷涂沉积单个 NZSP 扁平粒子和沉积体, 系统研究了粉末粒度 分布和喷涂参数对 NZSP 粒子元素蒸发和沉积体组织结构的影响。 通过沉积单个粒子, 揭示了等离子喷涂参数对 NZSP 粉末粒子的熔化程度和 Na、 P 元素优先蒸发的影响规律。 结果表明, 等离子电弧功率与氢气流量对其蒸发 影响显著, 元素蒸发损失量存在明显的粒子尺寸效应, 粒径小于约 35 μm 时, 随粒径的减小, Na 与 P 的蒸发损 失量显著增加, 当粒径增加至 35 μm 以上时, Na 与 P 的蒸发损失量受粒径的影响显著减小且整体损失量也有限; 通过对粒径范围的控制能够将等离子喷涂过程中 Na 元素的损失量控制在 10 % 以下, P 元素损失量控制在 20 % 以下。 采用粒径范围 30~50 μm 的 NZSP 粉末, 结合大气等离子喷涂参数控制可以得到无明显层状结构的良好层 间结合的组织结构致密电解质, 表明大气等离子喷涂在全固态钠离子电池固态电解质的制备中具有广阔的应用前 景。
英文摘要:
      Owning to its natural advantages of safety and element abundance, all-solid-state sodium-ion batteries have great potential for large-scale energy storage applications. Compared with traditional organic electrolyte sodium-ion batteries, solid-state sodium-ion batteries have the advantages of non-flammability and high thermal stability, and solid electrolytes exhibit good mechanical strength, which is conducive to the direct stacking of unit components, and is more in line with the safety and structural requirements of large-scale energy storage equipment. The core component of the all-solid-state battery is the solid electrolyte. The NASICON-type Na3Zr2Si2PO12 (NZSP) electrolyte has been widely studied due to its high ionic conductivity, thermal stability, and excellent mechanical properties. Air plasma spraying (APS) has been widely used in the field of ceramic coating deposition as a cost-effective, large-scale coating preparation process. Our previous investigations showed that for ceramic materials with melting points below about 1500 ℃ , dense coatings with fully bonded splats can be prepared by APS at room temperature. In this study, both single splats and NZSP coatings were deposited by APS using Ar-H2 plasma, and the influence of powder particle size distribution and spray parameters on the elemental preferential evaporation during spraying and microstructure of NZSP coatings were systematically investigated. By depositing individual isolated splats, the influence of plasma spray parameters on the NZSP particle melting degree and the preferential evaporation loss of Na and P elements were examined. The splats were deposited on a preheated substrate and thus the splats deposited from fully molten particles present a regular disk shape while splats from semi-molten droplets present a shape with splashed arms. The morphology of splats was examined by both scaning electron microscopy (SEM) and three dimensional conforcal laser microscopy. Accordingly, the fraction of molten droplets can be estimated based on test of the fraction of disk-shaped splats. The element contents of regular disk splats were estimated by energy dispersive spectroscopy (EDS). The microstructure of the NZSP deposits was examined by SEM and the phase structure of the deposits was characterized by X-ray diffraction (XRD). The results showed that the plasma arc power and hydrogen gas flow significantly affect the evaporation loss of Na and P, and there is an obvious particle size effect on the preferential evaporation loss of elements. With powders of particle size less than about 35 μm, the Na and P evaporization losses are significantly increased with the decrease of the particle size with respect to Zr. Thus, with a small NZSP particle of 20μm, Na and P present about 30% and 60% evaporation loss, respectively, with respect to Zr. When particle size is increased over to 35 μm, the Na and P preferential evaporation losses can be significantly suppressed. The results revealed plasma spraying deposition results in evolution of ZNSP in rhombic phase structure. By controlling the particle size range, the loss of Na elements during plasma spraying could be controlled below 10%, and the loss of P elements could be controlled below 20%. By using NZSP powder with a particle size range of 30~50 μm and controlling the APS parameters, a dense NZSP electrolyte with excellent inter-splat bonding and no obvious layered structure could be achieved, demonstrating the broad application prospects of APS for the preparation of solid electrolytes for all-solid-state sodium-ion batteries.
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