Metal Phosphate Nanoparticle Synthesis via Supercritical Solvothermal Process

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Solution Overview

Problem

Current methods for synthesizing zinc phosphate nanoparticles lack control over characteristics such as size, crystallinity, and surface functionalization, which are crucial for effective anticorrosion and other applications, and existing solvothermal methods are not compatible with simultaneous surface grafting of organic molecules.

Innovation Solution

A solvothermal method using a continuous flow process at pressures above 5 MPa and temperatures between 100°C to 350°C, allowing for the synthesis of metal phosphate nanoparticles with precise control over composition, phase, hydration state, size, and surface functionalization with organic ligands.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If conventional synthesis methods are used to prepare zinc phosphate nanoparticles, then the synthesis process is simple, but the control over characteristics such as size, crystallinity, and surface functionalization is poor

Engineering Contradiction:
Improvecontrol over size, crystallinity, and surface functionalizationVSAvoidsynthesis process complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent applies parameter changes by systematically varying synthesis conditions including pH (3-6), temperature (100-350°C), pressure (5-30 MPa), reaction time (1-24 hours), and precursor concentrations to achieve precise control over nanoparticle size (10-100 nm), crystallinity (hopeite phase), and surface functionalization. This resolves the contradiction by demonstrating that controlled parameter variation enables high manufacturing precision without requiring complex additional equipment.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent employs preliminary action through surface functionalization during the synthesis process itself, where organic ligands (carboxylic acids, phosphonic acids, silanes) are introduced in the reaction medium before nanoparticle formation. This allows simultaneous control of size, crystallinity, and surface properties in a single step, achieving high manufacturing precision without complex multi-step processes.

Inventive Principle:
Principle #10Preliminary action

2Manufacturing precision

If solvothermal methods are used for synthesis, then control over nanoparticle characteristics is improved, but simultaneous surface grafting of organic molecules is not compatible

Engineering Contradiction:
Improvecontrol over size and crystallinityVSAvoidsurface functionalization capability
Core Design Contradiction:
Manufacturing precisionVSAdaptability or versatility

Solution Approach 1:

The patent merges nanoparticle synthesis and surface functionalization into a single integrated solvothermal process. Organic ligands are introduced in the reaction medium before nanoparticle formation, allowing simultaneous crystallization of the hopeite phase and grafting of surface functional groups. This resolves the contradiction by combining two previously separate operations into one versatile process that achieves both precise control over size/crystallinity and surface functionalization.

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The patent creates a universal solvothermal method that can simultaneously produce nanoparticles with controlled size, crystallinity, and surface functionalization using various organic ligands (carboxylic acids, phosphonic acids, silanes, amines). The method is adaptable to different metal phosphates and functionalization requirements, resolving the contradiction by demonstrating multi-functionality in a single process.

Inventive Principle:
Principle #6Universality (Multi-functionality)

3Reliability

If nanoparticles are used for anticorrosion treatment, then penetration into micro-cracks is improved, but control over nanoparticle characteristics is insufficient

Engineering Contradiction:
Improveanticorrosion effectivenessVSAvoidcontrol over size and crystallinity
Core Design Contradiction:
ReliabilityVSManufacturing precision

Solution Approach 1:

The patent applies parameter changes by optimizing synthesis conditions (pH 3-6, temperature 100-350°C, pressure 5-30 MPa, reaction time 1-24 hours) to produce nanoparticles with specific size (10-100 nm) and crystallinity (hopeite phase) that enable penetration into micro-cracks while maintaining anticorrosion effectiveness. This resolves the contradiction by demonstrating that controlled parameter variation produces nanoparticles with both the required physical characteristics and functional performance.

Inventive Principle:
Principle #35Parameter changes

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

This method enables the production of nanoparticles with high purity and controlled characteristics, facilitating their use in industrial-scale applications with enhanced stability and performance in anticorrosion and other fields.

Implementation Method 1

a reaction medium comprising at least: a metal reactant, a phosphate precursor and a solvent, is submitted to a solvothermal treatment at a pressure superior to 5 MPa, and at a temperature of from 100 to 350°C

Methodology Applied
Scientific EffectSolvothermal synthesis: Supercritical Fluid

Implementation Method 2

solvothermal treatment at a pressure superior to 5 MPa, and at a temperature of from 100 to 350°C

Methodology Applied
Scientific EffectSupercritical fluid transition: Supercritical Fluid

Data Source

PatentUS11492259B2Method for manufacturing metal phosphate nanoparticles by sub-and supercritical solvothermal synthesis and nanoparticles obtained by this method
Publication Date: 2022.11.08 CENT NAT DE LA RECH SCI (C N R S)
  • US11492259B2 patent drawing
  • US11492259B2 patent drawing
  • US11492259B2 patent drawing

AI summary

A method for manufacturing metal phosphate hydrate nanoparticles wherein metal reactants are selected from metal precursors of transition metals,phosphate precursors are selected from: Trisodium phosphate Na3PO4, disodium phosphate Na2HPO4, phosphoric acid H3PO4 and hypophosphoric acid H4P2O6, wherein said method comprises the following step of a reaction medium comprising at least a metal reactant, a phosphate precursor and a solvent, is submitted to a solvothermal treatment at a pressure superior to 50 MPa, and at a temperature of from 100 to 350° C.