Nanodiamond Disaggregation Using Ozone and Alkaline Sonication

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Solution Overview

Problem

Nanodiamonds tend to aggregate strongly, forming clusters that are difficult to disaggregate using traditional methods, which often introduce contaminants and require expensive equipment, making it challenging to produce single-digit nanodiamonds suitable for biomedical applications.

Innovation Solution

A method involving ozone oxidation and horn sonication of nanodiamond clusters in an alkaline solvent at a pH of 8-11, followed by centrifugation, to break down aggregates into nanodiamond particles with a median size of less than 10 nanometers, without introducing contaminants or requiring costly equipment.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If traditional disaggregation methods (sonication, milling) are used to break down nanodiamond aggregates, then particle size is reduced, but metal contaminants are introduced and equipment cost increases

Engineering Contradiction:
Improveparticle sizeVSAvoidmetal contamination
Core Design Contradiction:
Manufacturing precisionVSObject-affected harmful factors

Solution Approach 1:

The patent uses a two-step process where ozone oxidation acts as an intermediary chemical treatment that modifies the nanodiamond surface and weakens aggregate bonds before mechanical disaggregation. This chemical pre-treatment reduces the force needed for mechanical breakdown, allowing gentler processing that avoids metal contamination from steel mill components while achieving the desired particle size reduction.

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The patent replaces traditional mechanical disaggregation methods (ball milling, attrition milling) with a chemical oxidation approach using ozone. The ozone oxidation process breaks down aggregate bonds through chemical reactions rather than mechanical force, eliminating the need for steel milling media and associated metal contamination risks while achieving effective particle size reduction.

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

2Productivity

If attrition milling with steel components is used to disaggregate nanodiamonds, then aggregates are broken down, but severe wear and corrosion occur and metal impurities contaminate the product

Engineering Contradiction:
Improvedisaggregation efficiencyVSAvoidmetal impurities
Core Design Contradiction:
ProductivityVSObject-generated harmful factors

Solution Approach 1:

Ozone oxidation serves as a chemical intermediary that pre-treats the nanodiamond aggregates, weakening the bonds between primary particles. This reduces the mechanical stress required for disaggregation, allowing the process to be completed with minimal mechanical action that doesn't require steel components, thereby maintaining productivity while eliminating metal impurity generation.

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The patent employs ozone, a strong oxidant, to chemically attack and weaken the bonds holding nanodiamond aggregates together. This oxidation process accelerates the disaggregation by chemically breaking down the aggregate structure, replacing the need for prolonged mechanical milling that would generate metal wear and impurities while maintaining high disaggregation efficiency.

Inventive Principle:
Principle #38Strong oxidants (Accelerated oxidation)

3Manufacturing precision

If pH is adjusted to 11 to obtain single-digit nanodiamonds after milling, then particle size is reduced below 10 nanometers, but an additional process step is required increasing cost and complexity

Engineering Contradiction:
Improveparticle sizeVSAvoidprocess complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent combines the oxidation and disaggregation steps into a single integrated process. The ozone oxidation simultaneously weakens aggregate bonds and facilitates particle separation, achieving both chemical modification and physical size reduction in one operation. This eliminates the need for separate pH adjustment steps required after mechanical milling, reducing process complexity while achieving single-digit nanodiamond production.

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The ozone oxidation process continuously acts on the nanodiamond aggregates throughout the treatment period, progressively weakening bonds and facilitating gradual disaggregation. This continuous chemical action replaces the discontinuous multi-step process of milling followed by pH adjustment, maintaining productive action throughout while eliminating unnecessary process steps and reducing overall complexity.

Inventive Principle:
Principle #20Continuity of useful 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

The method effectively produces high-purity, single-digit nanodiamonds suitable for biomedical applications, maintaining particle size stability and enabling redispersion from a dry state, thus overcoming the limitations of existing techniques.

Implementation Method 1

combining aggregated nanodiamond clusters in a liquid medium comprising a solvent, and ozone oxidized nanodiamond clusters

Methodology Applied
Scientific EffectOxidation: Oxidation

Implementation Method 2

sonicating the mixture for a time sufficient to produce nanodiamond particles having a median particle size less than the median particle size of the aggregated nanodiamond clusters

Methodology Applied
Scientific EffectUltrasonic cavitation: Acoustic Cavitation

Implementation Method 3

followed by centrifugation, to break down aggregates into nanodiamond particles

Methodology Applied
Scientific EffectCentrifugal separation: Centrifugal Separation

Data Source

PatentUS12509351B2Disaggregation of nanodiamond particles
Publication Date: 2025.12.30 DAICEL CORP
  • US12509351B2 patent drawing
  • US12509351B2 patent drawing
  • US12509351B2 patent drawing

AI summary

Methods for disaggregating nanodiamond clusters, for example, by using sonication to break apart nanodiamond aggregates in an aqueous slurry having an alkaline pH. Compositions, such as aqueous nanodiamond dispersions and dry particulate compositions can be produced using these methods.