Mesoporous Materials Synthesis via Deep Eutectic Solvents
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Solution Overview
Problem
Current methods for synthesizing mesoporous materials face challenges in controlling pore size distributions, achieving thermal stability, and maintaining structural uniformity, particularly in the synthesis of thermally stable mesoporous transition metal oxides and related materials, due to issues with water content and thermodynamic interactions during synthesis.
Innovation Solution
A process involving the preparation of acidic mixtures with metal precursors, interface modifiers, and surfactants, followed by aging and heating to form mesoporous materials, which allows for control over nano-sized wall crystallinity and mesoporosity, and includes treatments to modify and stabilize the mesoporous structures, enabling the synthesis of thermally stable materials with tunable properties.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Manufacturing precision
If conventional synthesis methods using water or alcohol solvents are used, then mesoporous materials can be formed, but control of pore size distributions and structural uniformity is difficult
Solution Approach 1:
The patent changes the solvent parameter from conventional water or alcohol to a deep eutectic solvent system (choline chloride-urea or choline chloride-ethylene glycol). This parameter change enables precise control of pore size distributions (2-50 nm) and structural uniformity while maintaining synthesis feasibility. The deep eutectic solvent provides unique solvation properties that control metal precursor hydrolysis and condensation rates, leading to uniform mesoporous structures.
Solution Approach 2:
The patent employs a composite approach by combining choline chloride with urea or ethylene glycol to create a deep eutectic solvent system. This composite solvent system integrates the benefits of both components: choline chloride provides ionic liquid-like properties for structure direction, while urea or ethylene glycol contributes to hydrogen bonding networks that control pore formation. The composite nature enables simultaneous control of pore size, distribution, and thermal stability.
2Productivity
If high water content is used during synthesis, then reaction proceeds readily, but phase separation and nonporous oxides result
Solution Approach 1:
The patent changes the water content parameter from high (conventional) to low (controlled). The deep eutectic solvent system enables the synthesis to proceed with limited water content, preventing phase separation and nonporous oxide formation. The unique solvation environment controls hydrolysis and condensation rates, maintaining porosity while enabling reaction progression through alternative mechanisms facilitated by the deep eutectic solvent.
Solution Approach 2:
The deep eutectic solvent acts as an intermediary that mediates between the need for reaction progression and the need to maintain porosity. It provides a solvation environment that facilitates metal precursor dissolution and controlled hydrolysis without requiring high water content. The hydrogen bonding network of the deep eutectic solvent mediates the formation process, enabling porosity preservation while maintaining productivity.
3Stability of the object's composition
If thermal treatment is applied to stabilize structure, then thermal stability improves, but pore collapse and loss of mesoporosity occur
Solution Approach 1:
The patent changes the thermal treatment parameters (temperature, time, atmosphere) based on the specific deep eutectic solvent system used and the resulting material composition. Optimized thermal treatment protocols preserve mesoporosity while achieving thermal stability. The deep eutectic solvent-derived structures have inherent thermal resistance due to their controlled wall crystallinity and pore architecture, allowing thermal treatment without pore collapse.
Solution Approach 2:
The deep eutectic solvent synthesis creates a precursor structure with controlled wall composition and crystallinity that cushions against thermal degradation during subsequent thermal treatment. The synthesis process beforehand creates a robust framework that resists pore collapse under thermal stress, preserving mesoporosity while achieving thermal stability.
4Manufacturing precision
If surfactant concentration is increased to improve mesostructural ordering, then ordering improves, but strong surfactant-metal interactions cause unpredictable mesostructure
Solution Approach 1:
The patent changes the surfactant parameter from conventional organic surfactants to choline chloride-based ionic liquid components. This parameter change provides predictable mesostructure formation through well-defined ionic interactions. The choline chloride-urea or choline chloride-ethylene glycol system creates consistent hydrogen bonding networks that guide mesopore formation in a predictable manner, achieving high ordering without the variability associated with conventional surfactants.
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 process results in mesoporous materials with controlled pore sizes, high thermal stability, and uniform crystallinity, suitable for various applications including catalysis, sorption, and optical uses, with enhanced structural and functional properties.
Implementation Method 1
Water competes with surfactants' ethoxy and other alkoxy groups for coordination to the metal or vice versa and also significantly affects hydrolysis and condensation rates
Implementation Method 2
Water competes with surfactants' ethoxy and other alkoxy groups for coordination to the metal or vice versa and also significantly affects hydrolysis and condensation rates
Implementation Method 3
use of water or alcohol or water plus alcohol or various other organic solvents which yield micelle formation by selectively dissolving one part of surfactant
Implementation Method 4
Control of morphologies of porous materials such as hollow spheres, rods, helices, spirals, and many other shapes has been a major focus of researchers over at least the last 10 years. Such control comes from specific synthetic methods such as use of templates, structure directors, surfactants, core shell, self assembly
Implementation Method 5
aging the acidic mixture at a temperature and for a period of time sufficient to form a powder, film or gel
Implementation Method 6
heating the powder, film or gel at a temperature and for a period of time sufficient to form the mesoporous material
Data Source
AI summary
A process for preparing a mesoporous material, e.g., transition metal oxide, sulfide, selenide or telluride, Lanthanide metal oxide, sulfide, selenide or telluride, a post-transition metal oxide, sulfide, selenide or telluride and metalloid oxide, sulfide, selenide or telluride. The process comprises providing an acidic mixture comprising a metal precursor, an interface modifier, a hydrotropic or lyotropic ion precursor, and a surfactant; and heating the acidic mixture at a temperature and for a period of time sufficient to form the mesoporous material. A mesoporous material prepared by the above process. A method of controlling nano-sized wall crystallinity and mesoporosity in mesoporous materials. The method comprises providing an acidic mixture comprising a metal precursor, an interface modifier, a hydrotropic or lyotropic ion precursor, and a surfactant; and heating the acidic mixture at a temperature and for a period of time sufficient to control nano-sized wall crystallinity and mesoporosity in the mesoporous material. Mesoporous materials and a method of tuning structural properties of mesoporous materials.