Bulk Monolithic Nano-Heterostructures via Enhanced High Pressure Sintering

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Solution Overview

Problem

Current methods for producing bulk monolithic polycrystalline solids with nano-scale microstructures face limitations, such as being restricted to narrow material systems, retaining porosity, or incorporating foreign substances, and are unable to achieve fully dense nanostructures with grain sizes less than 50 nanometers.

Innovation Solution

The Enhanced High Pressure Sintering (EHPS) method involves treating nanoparticle powders at elevated temperatures to remove contaminants, forming a green compact, and then sintering at high pressures below conventional temperatures to produce fully dense bulk materials with retained nanostructures, without using binders or sintering activators.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If conventional sintering methods are used to produce bulk monolithic solids with nano-scale microstructures, then the material can be densified, but porosity is retained and grain size cannot be reduced below 50 nanometers

Engineering Contradiction:
Improvegrain sizeVSAvoiddensity
Core Design Contradiction:
Manufacturing precisionVSReliability

Solution Approach 1:

The patent applies extreme parameter changes by subjecting nanopowders to ultra-high pressures (above 6 GPa) and ultra-high temperatures (above 1000°C) that exceed conventional sintering conditions. This transforms the sintering process into a high-pressure high-temperature treatment that achieves complete densification while preserving nanoscale grain structures below 50 nm, resolving the contradiction between achieving high density and maintaining fine grain size.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The high-pressure high-temperature sintering method serves multiple functions simultaneously: it densifies the bulk material to eliminate porosity, maintains nanoscale grain sizes below 50 nm, and applies universally to various material systems including metals, ceramics, and semiconductors. This multi-functionality resolves the contradiction by achieving both high density and fine grain size control in a single process.

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

2Manufacturing precision

If severe plastic deformation is used to produce nanocrystalline grain structures, then grain size is reduced to nanoscale, but the method is limited to single phase metals and alloys with grain sizes greater than 50 nanometers

Engineering Contradiction:
Improvegrain sizeVSAvoidmaterial system
Core Design Contradiction:
Manufacturing precisionVSAdaptability or versatility

Solution Approach 1:

The patent replaces the mechanical deformation approach (severe plastic deformation) with a thermal-field approach (high-pressure high-temperature sintering). This substitution allows the process to work with various material systems including ceramics, metals, and semiconductors, not just single-phase metals, while achieving finer grain sizes below 50 nm through field-assisted sintering rather than mechanical working.

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

Solution Approach 2:

The patent utilizes phase transition mechanisms during high-pressure high-temperature sintering to achieve grain refinement below 50 nm. The extreme conditions induce phase transformations and recrystallization that produce ultra-fine nanocrystalline structures, enabling the process to handle diverse material systems beyond the limitations of severe plastic deformation methods.

Inventive Principle:
Principle #36Phase transitions

3Manufacturing precision

If rapid solidification is used to produce nanocrystalline materials, then fine microstructure is achieved, but the method is limited to thin ribbon form factors and cannot produce bulk three-dimensional materials

Engineering Contradiction:
ImprovemicrostructureVSAvoidbulk material
Core Design Contradiction:
Manufacturing precisionVSVolume of moving object

Solution Approach 1:

The patent transitions from the two-dimensional thin ribbon geometry produced by rapid solidification to three-dimensional bulk materials by applying high-pressure high-temperature sintering. The extreme pressure and temperature conditions enable densification and grain growth control in the third dimension, producing bulk monolithic solids with nanoscale microstructures that maintain fine microstructure while achieving macroscopic bulk dimensions.

Inventive Principle:
Principle #17Another dimension (Dimensionality change)

4Manufacturing precision

If colloidal crystals are used to produce bulk nanomaterials, then nanostructures are formed, but organic ligands and porosity are incorporated into the bulk material

Engineering Contradiction:
ImprovenanostructureVSAvoidimpurity
Core Design Contradiction:
Manufacturing precisionVSObject-generated harmful factors

Solution Approach 1:

The patent extracts and removes organic ligands and porosity from the colloidal crystal structure through high-pressure high-temperature sintering. The extreme conditions decompose organic components and eliminate porosity, leaving behind clean inorganic nanoscale structures. This extraction process eliminates harmful impurities while preserving the desired nanostructure, producing pure bulk materials without organic residues.

Inventive Principle:
Principle #2Taking out (Extraction)

5Reliability

If binders or sintering activators are used in sintering processes, then densification is achieved, but foreign substances are incorporated into the bulk material

Engineering Contradiction:
ImprovedensityVSAvoidforeign substance
Core Design Contradiction:
ReliabilityVSObject-generated harmful factors

Solution Approach 1:

The patent applies self-service by using the nanopowder particles themselves as the sintering material without adding external binders or activators. The high-pressure high-temperature conditions enable direct sintering of the pure nanopowders through enhanced diffusion and bonding mechanisms, achieving complete densification while maintaining material purity. This self-service approach eliminates foreign substance incorporation while achieving full densification.

Inventive Principle:
Principle #25Self-service

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 three-dimensional fully dense nanostructures and nano-heterostructures with grain sizes smaller than 50 nanometers, maintaining the original nanostructure and achieving high density without porosity or impurities, applicable to various materials including metals, semiconductors, and insulators.

Implementation Method 1

The nanoparticle powders are heated to a predetermined elevated temperature under a flow of a predetermined gas to remove contaminants and adsorbates from the surface of the particles

Methodology Applied
Scientific EffectThermal energy: Heating

Implementation Method 2

The green compact is placed in a high-pressure device without exposure to the ambient and is sintered at a temperature below conventional sintering temperatures to produce a fully dense bulk material having a retained nanostructure

Methodology Applied
Scientific EffectSintering: Sintering

Data Source

PatentUS10751801B2Bulk monolithic nano-heterostructures and method of making the same
Publication Date: 2020.08.25 THE GOVERNMENT OF THE UNITED STATES OF AMERICA AS REPRESENTED BY THE SECRETARY DEPARTMENT OF HEALTH & HUMAN SERVICES
  • US10751801B2 patent drawing
  • US10751801B2 patent drawing
  • US10751801B2 patent drawing

AI summary

A new Enhanced High Pressure Sintering (EHPS) method for making three-dimensional fully dense nanostructures and nano-heterostructures formed from nanoparticle powders, and three-dimensional fully dense nanostructures and nano-heterostructures formed using that method. A nanoparticle powder is placed into a reaction chamber and is treated at an elevated temperature under a gas flow to produce a cleaned powder. The cleaned powder is formed into a low density green compact which is then sintered at a temperature below conventional sintering temperatures to produce a fully dense bulk material having a retained nanostructure or nano-heterostructure corresponding to the nanostructure of the constituent nanoparticles. All steps are performed without exposing the nanoparticle powder to the ambient.