Mesoporous Carbon via Nanocrystalline Cellulose Templating

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Solution Overview

Problem

Conventional microporous carbons have limitations such as broad pore-size distributions, slow mass transport, low conductivity, and structural collapse during high-temperature treatments, which hinder their effectiveness in applications like adsorption of large molecules and energy storage devices.

Innovation Solution

A process involving the carbonization of nanocrystalline cellulose (NCC) in an inorganic matrix followed by removal of the matrix to produce mesoporous carbon with a chiral nematic organization, offering a simpler and more efficient method for synthesizing mesoporous carbon materials with higher surface areas and novel properties.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of manufacture

If conventional microporous carbons are used, then they are widely available and low cost, but they have broad pore-size distributions and slow mass transport

Engineering Contradiction:
Improveavailability and costVSAvoidpore-size distribution
Core Design Contradiction:
Ease of manufactureVSManufacturing precision

Solution Approach 1:

The patent uses a silica template as an intermediary structure during synthesis. The silica template provides a predefined porous structure that guides the formation of carbon pores, ensuring uniform pore sizes. After carbonization, the silica template is removed, leaving behind carbon with narrow pore-size distribution. This intermediary approach resolves the contradiction by enabling precise pore control during manufacturing while maintaining cost-effectiveness through the use of simple templating materials.

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The patent controls pore-size distribution by adjusting synthesis parameters such as silica template pore size, carbonization temperature, and precursor composition. By changing these parameters, the final carbon material achieves narrow pore-size distribution tailored for specific applications, while the overall manufacturing process remains simple and cost-effective.

Inventive Principle:
Principle #35Parameter changes

2Ease of manufacture

If conventional microporous carbons are used, then they are low cost, but they have slow mass transport of molecules

Engineering Contradiction:
ImprovecostVSAvoidmass transport
Core Design Contradiction:
Ease of manufactureVSSpeed

Solution Approach 1:

The patent optimizes mass transport by controlling pore size and connectivity through template selection and carbonization parameters. The resulting mesoporous carbon materials have larger, more uniform pores that facilitate faster molecular diffusion while maintaining cost-effective manufacturing through simple templating approaches.

Inventive Principle:
Principle #35Parameter changes

3Ease of manufacture

If conventional microporous carbons are used, then they are widely available, but they have low conductivity due to functionalization during activation

Engineering Contradiction:
ImproveavailabilityVSAvoidconductivity
Core Design Contradiction:
Ease of manufactureVSReliability

Solution Approach 1:

Instead of activating carbon to create pores (which introduces functional groups that reduce conductivity), the patent inverts the approach by using a template to define pores during carbonization. This avoids activation treatment entirely, preserving the intrinsic high conductivity of carbon while still achieving the desired porous structure for molecular transport.

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

4Ease of manufacture

If conventional microporous carbons are used, then they are low cost, but they collapse during high-temperature treatments

Engineering Contradiction:
ImprovecostVSAvoidstructural stability
Core Design Contradiction:
Ease of manufactureVSStability of the object's composition

Solution Approach 1:

The patent performs preliminary carbonization of the carbon precursor in the presence of the silica template before template removal. This preliminary carbonization creates a stable carbon framework that maintains the porous structure even after template removal and subsequent high-temperature treatments. The pre-formed carbon structure prevents collapse that would otherwise occur in conventional approaches.

Inventive Principle:
Principle #10Preliminary action

5Manufacturing precision

If template-synthesis using liquid crystalline templates is used, then materials with well-defined porous structures are obtained, but the process involves high number of steps and difficulty in fully loading the mesoporous host

Engineering Contradiction:
Improveporous structure definitionVSAvoidnumber of steps
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent merges the template formation and carbon precursor loading into a single impregnation step. The carbon precursor is loaded onto the silica template during the same process used to form the liquid crystalline structure, eliminating the need for separate loading steps. This streamlined approach maintains well-defined porous structures while significantly reducing process complexity.

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The patent performs preliminary carbon precursor impregnation onto the silica template before liquid crystalline phase formation. This ensures complete and uniform loading of the template with carbon precursor in advance, eliminating the need for repeated loading steps and simplifying the overall synthesis process while maintaining precise porous structure definition.

Inventive Principle:
Principle #10Preliminary action

6Manufacturing precision

If hard-templating of carbon is used, then mesoporous carbon materials are produced, but it involves multiple loading steps and difficulty in fully loading the mesoporous host

Engineering Contradiction:
Improvemesoporous structureVSAvoidloading efficiency
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The patent performs preliminary and complete carbon precursor impregnation onto the silica template before liquid crystalline phase formation and carbonization. This single preliminary loading step achieves complete saturation of the template, eliminating the need for multiple repeated loading steps and significantly improving productivity while maintaining precise mesoporous structure.

Inventive Principle:
Principle #10Preliminary 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 resulting mesoporous carbon materials exhibit higher surface areas and retention of chiral nematic structure, enhancing their suitability for applications in catalyst supports, supercapacitors, batteries, and adsorbents, while avoiding the drawbacks of traditional methods.

Implementation Method 1

The chiral nematic (or cholesteric) liquid crystalline phase, where mesogens organize into a helical assembly

Methodology Applied
Scientific EffectSelf-assembly: Self-Assembly

Implementation Method 2

liquid crystal templating has become a very important method to developing periodic materials with organization in the 1-100 nm dimension range

Methodology Applied
Scientific EffectLiquid crystals: Liquid Crystals

Implementation Method 3

the silica host is removed with a procedure known to dissolve silica, often using aqueous or alcoholic hydroxide salts (e.g., NaOH, KOH, NH4OH) or hydrogen fluoride (HF)

Methodology Applied
Scientific EffectChemical dissolution:

Implementation Method 4

carbonising nanocrystalline cellulose (NCC) in an inorganic matrix

Methodology Applied
Scientific EffectPyrolysis: Pyrolysis

Data Source

PatentUS10023466B2Chiral or achiral, mesoporous carbon
Publication Date: 2018.07.17 FPINNOVATIONS INC
  • US10023466B2 patent drawing
  • US10023466B2 patent drawing
  • US10023466B2 patent drawing

AI summary

A composition and a method for producing mesoporous carbon materials with a chiral or achiral organization. In the method, a polymerizable inorganic monomer is reacted in the presence of nanocrystalline cellulose to give a material of inorganic solid with cellulose nanocrystallites organized in a chiral nematic organization. The cellulose can be carbonized through thermal treatment under inert atmosphere (e.g., nitrogen or argon) and the silica may subsequently be removed using aqueous solutions of sodium hydroxide (NaOH) or hydrogen fluoride (HF) to give the stable mesoporous carbon materials that retain the chiral nematic structure of the cellulose. These materials may be obtained as free-standing films with very high surface area. Through control of the reaction conditions the pore-size distribution may be varied from predominantly microporous to predominantly mesoporous materials. These are the first materials to use cellulose as both the structural template and carbon source for a mesoporous carbon material. These are also the first carbon materials to combine mesoporosity with long-range chiral ordering. Possible applications for these materials include: charge storage devices (e.g. supercapacitors and anodes for Li-ion batteries), adsorbents, gas purifiers, light-weight nanocomposite materials, catalyst supports (e.g., for chiral transformations), gas storage, and as a hard-template to generate other materials, preferably with chiral structures.