Semiconductor Nanocrystal Synthesis via Staged Temperature Control

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Solution Overview

Problem

Current methods for preparing semiconductor nanocrystals, particularly those involving Group IIIA and Group VA elements, face challenges in achieving precise control over particle size and wavelength characteristics with narrow size distributions, and often require complex reaction conditions and purities of precursors.

Innovation Solution

A method involving heating a mixture of carboxylic acid and solvents, followed by the controlled addition of Group IIIA and Group VA element precursors and amines at specific temperatures, under oxygen-free conditions, to form semiconductor nanocrystal seed particles of predetermined size and wavelength, allowing for tuning of reaction conditions to achieve desired properties.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If conventional methods are used to prepare semiconductor nanocrystals, then synthesis can be achieved, but precise control over particle size and wavelength characteristics with narrow size distributions is difficult

Engineering Contradiction:
Improveparticle size controlVSAvoidreaction conditions complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent applies parameter changes by systematically varying reaction temperature, precursor ratios, and ligand concentrations to achieve precise control over nanocrystal size and wavelength characteristics. The method establishes specific temperature ranges (e.g., 25-150°C for mixing, 150-300°C for heating) and precursor ratios (e.g., Group IIIA:Group VA = 1:1 to 2:1) that directly influence particle size distribution and optical properties, resolving the contradiction between manufacturing precision and process complexity.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent employs preliminary action by pre-mixing precursors and ligands at controlled temperatures before initiating the main reaction. The method requires pre-heating the reaction mixture to specific temperatures, pre-mixing precursors in predetermined ratios, and preparing the reaction environment (inert atmosphere) before adding materials. This preliminary preparation enables precise size control while making the overall process more systematic and manageable.

Inventive Principle:
Principle #10Preliminary action

2Manufacturing precision

If high purity precursors are used, then nanocrystal quality is improved, but the synthesis process becomes more complex and costly

Engineering Contradiction:
Improvenanocrystal qualityVSAvoidsynthesis process simplicity
Core Design Contradiction:
Manufacturing precisionVSEase of manufacture

Solution Approach 1:

The patent applies this principle by using ligands and precursors that can be readily disposed of or regenerated after the reaction. The method employs excess ligands (e.g., carboxylic acids, phosphonic acids) that serve multiple functions: they control nanocrystal growth, passivate surfaces, and can be removed or replaced in subsequent simple steps. This approach maintains high nanocrystal quality while simplifying the overall manufacturing process by reducing the need for extremely high purity precursors.

Inventive Principle:
Principle #27Cheap short-living objects (Disposable)

Solution Approach 2:

The patent uses ligands as intermediaries between precursors and the final nanocrystal product. These ligands (carboxylic acids, phosphonic acids, amines) mediate the reaction by controlling precursor decomposition, regulating growth rates, and stabilizing nanocrystal surfaces. The ligands enable the use of more tolerant, less expensive precursors while still achieving high-quality nanocrystals with controlled size and narrow size distributions.

Inventive Principle:
Principle #24Intermediary (Mediator)

3Manufacturing precision

If reaction temperature is increased to improve nanocrystal formation, then particle size control is enhanced, but energy consumption increases

Engineering Contradiction:
Improvesize distribution controlVSAvoidenergy consumption
Core Design Contradiction:
Manufacturing precisionVSUse of energy by moving object

Solution Approach 1:

The patent applies periodic action by using staged temperature profiles with distinct phases: an initial mixing phase at lower temperatures (25-150°C) to prepare precursors and ligands, followed by a controlled heating phase (150-300°C) for nanocrystal formation, and potentially a cooling or maintenance phase. This periodic temperature control achieves precise size distribution while minimizing total energy consumption by avoiding continuously high temperatures and optimizing the duration at each temperature stage.

Inventive Principle:
Principle #19Periodic action

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 semiconductor nanocrystals with precise control over particle size and wavelength, improving their size distribution and optical properties, and allows for the use of impure precursors, simplifying the synthesis process while maintaining high quality.

Implementation Method 1

heating the reaction mixture to a third temperature sufficient to form semiconductor nanocrystal seed particles

Methodology Applied
Scientific EffectNucleation: Nucleation

Implementation Method 2

heating the reaction mixture to a third temperature for a third period of time sufficient to form semiconductor nanocrystal seed particles of predetermined size

Methodology Applied
Scientific EffectCrystal growth: Crystallisation

Data Source

PatentUS9748096B2Methods of preparation of semiconductor nanocrystals group IIIA and group VA elements
Publication Date: 2017.08.29 SAMSUNG ELECTRONICS CO LTD
  • US9748096B2 patent drawing
  • US9748096B2 patent drawing
  • US9748096B2 patent drawing

AI summary

A method for preparing semiconductor nanocrystals is disclosed. The method includes adding one or more cation precursors and one or more anion precursors in a reaction mixture including a solvent in a reaction vessel, maintaining the reaction mixture at a first temperature and for a first time period sufficient to produce semiconductor nanocrystal seed particles of the cation and the anion, and maintaining the reaction mixture at a second temperature that is higher than the first temperature for a second time period sufficient to enlarge the semiconductor nanocrystal seed particles to produce semiconductor nanocrystals from the cation and the anion.