Trimetallic layered double hydroxides (LDHs) solid solutions with the compositions Zn/Co-Al, Zn/Cu-Al, and Co/Cu-Al, intercalated with hydrated SO₄^2-/Na⁺ were synthesized by co-precipitation with increasing pH at room temperature, hydrothermally treated at 90 °C for 120 h and dried at 40 °C. The compounds were analyzed by XRD, where all the systems presented basal distances close to 11 Å, typical of the intercalation of sulfate in double-layer arrangements in the presence of hydrated sodium cations. FTIR indicated the presence of typical bands attributed to sulfate, water molecules and metal–oxygen lattice vibrations. SEM and TEM images of the Zn/Co-Al system indicated the presence of micrometric particles, homogeneous aspect and nanometric dimensions along the layer packing (basal directions), in the whole range of replacements. EDS spectra of all samples indicated the presence of the expected elements in all compounds. ICP-OES indicated that all system contained the elements close to the expected concentration, with slightly smaller contents of sulfate and sodium cations. SAED spectra of the Zn/Co-Al system indicated the presence of a√3 × a√3 superstructures in all samples, attributed to the ordering of divalent metals in the layer domains, typical of compounds with 2 M²⁺:1M³⁺ molar ratios. Homogeneous solid solutions were obtained for all systems, but a small contamination with carbonate was observed in some samples, producing compounds with the ideal formula [M²⁺_0.666Al_0.333(OH)₂][(SO₄)_0.222-x(CO₃)_xNa_0.111] nH₂O. This work increases the number of members of trimetallic LDH and opens a new avenue for future applications.

具有 Zn/Co-Al、Zn/Cu-Al 和 Co/Cu-Al 成分的三金属层状双氢氧化物 (LDH) 固溶体，插入水合 SO 4 _2- ^/ Na ⁺通过在室温下增加 pH 的共沉淀法合成，在 90°C 下水热处理 120 小时并在 40°C 下干燥。通过 XRD 分析这些化合物，其中所有系统的基距都接近 11 Å，这是在存在水合钠阳离子的情况下硫酸盐在双层排列中的典型插层。FTIR 表明存在归因于硫酸盐、水分子和金属-氧晶格振动的典型条带。Zn/Co-Al 系统的 SEM 和 TEM 图像表明在整个替换范围内沿层堆积（基本方向）存在微米级颗粒、均匀外观和纳米级尺寸。所有样品的 EDS 光谱表明所有化合物中都存在预期元素。ICP-OES 表明所有系统都含有接近预期浓度的元素，硫酸盐和钠阳离子的含量略低。Zn/Co-Al 系统的 SAED 光谱表明所有样品中都存在 a√3 × a√3 超结构，这归因于层域中二价金属的有序化，典型的化合物具有 2 M²⁺ :1M ³⁺摩尔比。所有系统都获得了均匀的固溶体，但在一些样品中观察到碳酸盐的少量污染，产生具有理想分子式的化合物 [M 2+ ^0.666 _Al 0.333 ₍ OH) ₂ ][(SO ₄ ) _0.222-x (CO ₃ ) _x Na _0.111 ] nH ₂ O。这项工作增加了三金属LDH的成员数量，为未来的应用开辟了一条新途径。