17 Citations (Scopus)

Abstract

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<sup>-</sup>-intercalated (Zn, Al)-LDH, controlled synthesis of single crystalline nanoparticles using the coprecipitation method followed by hydrothermal treatment (HT) was achieved in three steps. First, a 2<sup>4-1</sup> 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 (χ<sup>2</sup>)<3 were found to be 85°C for 5h. 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 ~200-500nm.

Original languageEnglish (US)
Pages (from-to)264-272
Number of pages9
JournalJournal of Colloid and Interface Science
Volume459
DOIs
StatePublished - Dec 1 2015

Fingerprint

Particle size analysis
Chlorides
Salts
Particle size
Nanoparticles
Coprecipitation
Carbonates
Aluminum
Design of experiments
Anions
Negative ions
Crystalline materials
hydroxide ion
Composite materials

Keywords

  • Controlled synthesis
  • Coprecipitation
  • Design of experiments
  • Layered double hydroxide nanoparticles

ASJC Scopus subject areas

  • Surfaces, Coatings and Films
  • Electronic, Optical and Magnetic Materials
  • Biomaterials
  • Colloid and Surface Chemistry

Cite this

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title = "Insights into the synthesis of layered double hydroxide (LDH) nanoparticles: Part 1. Optimization and controlled synthesis of chloride-intercalated LDH",
abstract = "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) was 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 5h. 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 ~200-500nm.",
keywords = "Controlled synthesis, Coprecipitation, Design of experiments, Layered double hydroxide nanoparticles",
author = "Xiaodi Sun and Erica Neuperger and Sandwip Dey",
year = "2015",
month = "12",
day = "1",
doi = "10.1016/j.jcis.2015.07.073",
language = "English (US)",
volume = "459",
pages = "264--272",
journal = "Journal of Colloid and Interface Science",
issn = "0021-9797",
publisher = "Academic Press Inc.",

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TY - JOUR

T1 - Insights into the synthesis of layered double hydroxide (LDH) nanoparticles

T2 - Part 1. Optimization and controlled synthesis of chloride-intercalated LDH

AU - Sun, Xiaodi

AU - Neuperger, Erica

AU - Dey, Sandwip

PY - 2015/12/1

Y1 - 2015/12/1

N2 - 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) was 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 5h. 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 ~200-500nm.

AB - 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) was 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 5h. 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 ~200-500nm.

KW - Controlled synthesis

KW - Coprecipitation

KW - Design of experiments

KW - Layered double hydroxide nanoparticles

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