Mesoporous Carbon via Spinodal Decomposition

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Solution Overview

Problem

Traditional methods for synthesizing mesoporous carbon, such as hard- and soft-templating, are costly and hazardous, and lack a facile route for mesopore development, making them unsuitable for industrial-scale viability.

Innovation Solution

A surfactant-free method involving in-situ polymerization of phloroglucinol-formaldehyde resins with polyethylene glycol (PEG) under reflux in acidic ethanol, utilizing spinodal decomposition to create mesoporous carbons, which are less costly and can be derived from renewable resources.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If hard-templating or soft-templating methods are used to synthesize mesoporous carbon, then well-defined mesopore size distributions and morphologies are achieved, but the process becomes costly and hazardous

Engineering Contradiction:
Improvemesopore size distributionVSAvoidmanufacturing cost
Core Design Contradiction:
Manufacturing precisionVSEase of manufacture

Solution Approach 1:

The invention extracts and eliminates the expensive and hazardous templating agents (silica templates requiring HF/NaOH etching, or costly block copolymers) from the synthesis process. Instead, it uses a simplified carbonization approach where the template structure is directly incorporated into the carbon matrix through controlled decomposition, achieving mesoporous structures without traditional templating steps.

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The patent employs inexpensive, easily decomposable organic templates (such as sugars or simple polymers) that serve their structuring function during synthesis and then completely decompose during carbonization, leaving no residual template material. These disposable templates are much cheaper than silica or block copolymers and require no hazardous removal steps.

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

2Manufacturing precision

If traditional templating methods are used, then controlled porosity is achieved, but hazardous chemicals and complex synthesis are required

Engineering Contradiction:
Improveporosity controlVSAvoidhazardous chemicals
Core Design Contradiction:
Manufacturing precisionVSObject-affected harmful factors

Solution Approach 1:

The invention converts the typically harmful high-temperature carbonization process, which would normally destroy delicate template structures, into a beneficial step. The controlled decomposition of organic templates during carbonization directly creates the desired mesoporous structure in the carbon product, turning a destructive process into a constructive one that eliminates hazardous chemicals.

Inventive Principle:
Principle #22Blessing in disguise (Convert harm into benefit)

Solution Approach 2:

The patent changes the key parameter of template stability by using organic materials with controlled decomposition temperatures that match the carbonization process. This allows the template to remain intact during synthesis but decompose completely during carbonization, achieving porosity control without hazardous chemicals.

Inventive Principle:
Principle #35Parameter changes

3Manufacturing precision

If block copolymer templating agents are used, then mesoporous structures are formed, but synthetic intensity and cost increase

Engineering Contradiction:
Improvemesopore morphologyVSAvoidsynthesis complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The invention segments the synthesis process into two independent stages: (1) forming the carbon matrix with embedded organic template structures, and (2) decomposing the template during carbonization. This segmentation eliminates the need for complex block copolymer self-assembly while achieving similar mesoporous morphologies through simpler, separate steps.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

Instead of using complex block copolymers to template the carbon structure and then removing them, the invention inverts the approach by using simple organic templates that are intentionally designed to decompose and become part of the carbonization process, creating porosity through their controlled destruction rather than their presence.

Inventive Principle:
Principle #13The other way round (Inversion)

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 produces mesoporous carbons with improved physical resilience, thermal stability, and controlled porosity, reducing costs and environmental hazards while maintaining high surface area and porosity, making it suitable for industrial applications.

Implementation Method 1

in-situ polymerization of phloroglucinol-formaldehyde (PF) resins

Methodology Applied
Scientific EffectPolymerization:

Implementation Method 2

synthesizes mesoporous carbons through spinodal decomposition

Methodology Applied
Scientific EffectSpinodal decomposition:

Implementation Method 3

under reflux in acidic ethanol

Methodology Applied
Scientific EffectReflux:

Data Source

PatentUS10017391B2Direct polymer templating synthesis of mesoporous carbon
Publication Date: 2018.07.10 UT BATTELLE LLC
  • US10017391B2 patent drawing
  • US10017391B2 patent drawing
  • US10017391B2 patent drawing

AI summary

The invention is directed to a method for fabricating a mesoporous carbon composite material. The method comprises providing a precursor composition and subjecting the precursor material to a curing step followed by carbonization step. The precursor composition comprises (i) a templating component comprised of a linear homopolymer material, (ii) a phenolic compound or material, (iii) a crosslinkable aldehyde component, and (iv) an acid catalyst.