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Insights into the Synthesis of Layered Double Hydroxide (LDH) Nanoparticles: Part 1. Optimization and Controlled Synthesis of Chloride-Intercalated LDH

机译:层状双氢氧化物(LDH)纳米粒子合成的见解:第1部分。嵌入氯离子的LDH的优化和可控合成

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摘要

Layered double hydroxide (LDH) nanoparticles have excellent anion-intercalating property, and their potential as theranostic nanovectors is high. However, understanding of the control of the mean particle size (MPS) and achievement of monodispersed particle size distribution (PSD) remains elusive. Herein, with the aid of statistical design of experiments on a model system of Cl-intercalated (Zn, Al)-LDH, controlled synthesis of single crystalline nanoparticles using the coprecipitation method followed by hydrothermal treatment (HT) is achieved in three steps. First, a 24-1 design enabled the identification of influential parameters for MPS (i.e., salt concentration, molar ratio of carbonate to aluminum, solution addition rate, and interaction between salt concentration and stirring rate) and PSD (i.e., salt concentration and stirring rate), as well as the optimum coprecipitation conditions that result in a monodispersed PSD (i.e., low salt concentration and high stirring rate). Second, a preliminary explanation of the HT was suggested and the optimum HT conditions for obtaining ideal Gaussian PSD with chi-squared (χ2) < 3 were found to be 85 °C for 5 h. Third, using a central composite design, a quantitative MPS model, expressed in terms of the significant factors, was developed and experimentally verified to synthesize nearly monodispersed LDH nanoparticles with MPS ~200–500 nm.
机译:层状双氢氧化物(LDH)纳米粒子具有出色的阴离子插入性能,并且它们作为治疗性纳米载体的潜力很高。但是,对平均粒度(MPS)的控制和单分散粒度分布(PSD)的实现的了解仍然难以捉摸。在本文中,借助于在Cl -嵌入(Zn,Al)-LDH的模型系统上进行的实验统计设计,使用共沉淀方法随后进行水热处理(HT)来控制单晶纳米颗粒的合成)分三个步骤实现。首先,采用2 4-1 设计可以确定MPS的影响参数(即盐浓度,碳酸盐与铝的摩尔比,溶液添加速率以及盐浓度与搅拌速率之间的相互作用),以及PSD(即盐浓度和搅拌速度),以及导致单分散PSD的最佳共沉淀条件(即低盐浓度和高搅拌速度)。其次,提出了对HT的初步解释,并发现获得卡方(χ 2 )<3的理想高斯PSD的最佳HT条件为85°C 5 h。第三,使用中央复合设计,开发了定量MPS模型(以重要因素表示),并通过实验验证了MPS〜200–500 nm的近单分散LDH纳米颗粒的合成。

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