MOF Crystallite Shape Control via Non-Coordination Buffering

Resolve Bottlenecks,
Find Innovative Solutions
Generate Solutions

Solution Overview

Problem

Conventional synthetic schemes for metal-organic frameworks (MOFs) often result in anisotropic crystallites with extended rod-like structures, limiting gas diffusion due to inaccessible external surfaces, and struggle to control crystallite size and shape, which is crucial for adsorbent performance in applications like CO2 capture from flue gas.

Innovation Solution

The use of non-coordinating anions and controlled pH during synthesis, along with the choice of buffers and surface functionalization, allows for precise control of crystallite dimensions and shape, enabling the formation of low aspect ratio MOFs with improved dispersity and accessibility for gas diffusion.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Shape

If conventional synthetic schemes are used for MOFs, then crystalline product is obtained, but crystallites form extended rod-like structures with limited gas diffusion

Engineering Contradiction:
Improvecrystallite shapeVSAvoidgas diffusion accessibility
Core Design Contradiction:
ShapeVSEase of operation

Solution Approach 1:

The patent changes chemical parameters during synthesis, specifically using modulators with different coordinating strengths (e.g., monocarboxylic acids vs. dicarboxylic acids) and adjusting pH levels to control crystallite morphology. These parameter changes transform the crystal growth from anisotropic rod-like structures to more isotropic shapes with improved surface accessibility for gas diffusion.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent introduces modulator molecules as intermediaries during synthesis that temporarily bind to crystal surfaces and direct growth patterns. These modulators act as mediators between the MOF precursors and the final crystal structure, controlling aspect ratio and morphology to prevent excessive rod-like elongation while maintaining crystallinity.

Inventive Principle:
Principle #24Intermediary (Mediator)

2Manufacturing precision

If conventional synthetic schemes are used for MOFs, then crystalline product is obtained, but crystallite size and shape control is difficult

Engineering Contradiction:
Improvecrystallite size and shape controlVSAvoidsynthesis process complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent systematically varies synthesis parameters including modulator concentration, pH level, temperature, and reaction time to achieve precise control over crystallite size and shape. By establishing parameter ranges and their effects on morphology, the patent enables predictable control without requiring complex equipment or procedures.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent applies different modulators to specific crystal facets or growth directions, creating local variations in growth rates that result in controlled overall morphology. This local quality approach allows precise shape control by targeting specific crystallographic planes with appropriate modulators.

Inventive Principle:
Principle #3Local quality

3Stability of the object's composition

If high aspect ratio crystallites are formed, then material phase stability is achieved, but external surface accessibility for adsorption is reduced

Engineering Contradiction:
Improvematerial phase stabilityVSAvoidexternal surface area
Core Design Contradiction:
Stability of the object's compositionVSArea of stationary object

Solution Approach 1:

The patent adjusts synthesis parameters such as modulator type, concentration, and pH to control the aspect ratio of crystallites. By optimizing these parameters, the patent achieves a balance where crystallites maintain phase stability while developing more compact shapes with increased external surface area for adsorption applications.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent controls the degree of asymmetry in crystallite shapes to optimize both stability and surface area. Rather than forming highly asymmetric rod-like structures, the patent promotes more symmetric or equiaxed shapes that provide comparable stability with superior surface accessibility for gas adsorption.

Inventive Principle:
Principle #4Asymmetry

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 approach leads to MOFs with enhanced adsorption capabilities and catalytic performance by optimizing crystallite size and shape, specifically improving CO2 capture efficiency and stability under humid conditions, addressing the challenges of existing MOF synthesis methods.

Implementation Method 1

the reacting is in the presence of a buffer devoid of metal coordinating functionality, thereby controlling an amount of crystal growth of the metal-organic framework along one or more crystallographic directions

Methodology Applied
Scientific EffectpH control:

Implementation Method 2

Each polytopic organic linker in the plurality of polytopic organic linkers is connected to two or more metal cations in the plurality of metal cations

Methodology Applied
Scientific EffectCoordination bonding: Chemical Bonding

Data Source

PatentEP3856748B1Metal-organic framework phase and crystallite shape control
Publication Date: 2024.03.06 EXXONMOBIL TECHNOLOGY & ENGINEERING CO
  • EP3856748B1 patent drawingFigure 1
  • EP3856748B1 patent drawingFigure 2
  • EP3856748B1 patent drawingFigure 3

AI summary

Methods of synthesizing crystalline metal-organic frameworks (MOFs) comprising polytopic organic linkers and cations, where each linker is connected to two or more cations, are provided. In the disclosed methods, the linkers are reacted with a compound of formula M n X m , where M is cationic Be, Mg, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Zr, Nb, Mo, Ru, Rh, Pd, Cd, or Hf, X is anionic, n and m are integers. The reacting is buffered by a buffer devoid of metal coordinating functionality when the pKa of the anion is below a threshold related to the lowest pKa of the linker. The reacting is optionally not buffered when the pKa of the anion is at or above this threshold. The disclosed methods lead to product phase MOF in which crystal growth is controlled leading to control over molecular diffusion.