Low-Temperature Compression for Porous Monolithic Materials

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Solution Overview

Problem

Existing methods for manufacturing porous monolithic materials, such as those based on hydroxyapatite and other minerals, often result in materials with degraded chemical structures and unsatisfactory mechanical properties due to high-temperature sintering processes, which also limit the incorporation of organic components and homogeneity.

Innovation Solution

A process involving the formation of a mixture with a solvent, typically water, followed by isostatic compression at low temperatures to form ice crystals, which acts as a template for consolidating the powder into a monolith without heat-induced structural changes, allowing for the incorporation of organic components and achieving high mechanical resistance and homogeneous porosity.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Strength

If high-temperature sintering is applied to manufacture porous monolithic materials from mineral powder, then the material achieves structural consolidation, but the chemical structure of the mineral raw material is modified (partial elimination of oxygen atoms and hydroxides), degrading biocompatibility

Engineering Contradiction:
Improvestructural consolidationVSAvoidchemical structure
Core Design Contradiction:
StrengthVSStability of the object's composition

Solution Approach 1:

The invention changes the temperature parameter from high-temperature sintering to low-temperature freezing, and changes the consolidation mechanism from thermal diffusion to ice crystal template formation. The mixture is frozen at low temperature to form ice crystals that template the porous structure, then lyophilized to remove ice, achieving consolidation without high-temperature exposure that would modify the chemical structure

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention utilizes the phase transition of water from liquid to solid (freezing) to create ice crystals that serve as a temporary template. The ice crystals form a structured framework during freezing, which is then preserved through lyophilization to create the final porous structure, avoiding the need for high-temperature sintering that would alter the mineral's chemical composition

Inventive Principle:
Principle #36Phase transitions

2Strength

If high-temperature sintering is applied to manufacture porous monolithic materials, then the material achieves structural consolidation, but organic raw materials cannot be incorporated before sintering as they would be decomposed by heat treatment

Engineering Contradiction:
Improvestructural consolidationVSAvoidincorporation of organic components
Core Design Contradiction:
StrengthVSAdaptability or versatility

Solution Approach 1:

The invention changes the processing temperature from high-temperature sintering to low-temperature freezing and lyophilization. This parameter change allows organic materials to be incorporated into the mixture before freezing, as the low temperatures preserve organic integrity while still enabling porous structure formation through ice crystal templating

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention performs preliminary mixing of organic materials with the mineral powder and solvent before freezing. This preliminary action allows organic components to be uniformly distributed in the mixture before the freezing process creates the porous structure, ensuring both structural consolidation and preservation of organic materials

Inventive Principle:
Principle #10Preliminary action

3Ease of manufacture

If conventional sintering or additive manufacturing with laser heating is applied, then porous monolithic materials are manufactured, but the localized heating equivalent to high-temperature heating degrades the material structure

Engineering Contradiction:
Improveporous structure formationVSAvoidchemical structure
Core Design Contradiction:
Ease of manufactureVSStability of the object's composition

Solution Approach 1:

The invention replaces thermal heating processes with a phase transition-based process. Instead of using laser heating or sintering to create pores, the invention uses freezing to form ice crystals as templates, then lyophilization to remove them. This phase transition approach achieves porous structure formation without thermal degradation of the material composition

Inventive Principle:
Principle #36Phase transitions

4Volume of stationary object

If water is frozen to form ice crystals as porogen, then porous structure is created, but the resulting material is very brittle and requires gelling agents that reduce mechanical strength

Engineering Contradiction:
ImproveporosityVSAvoidmechanical strength
Core Design Contradiction:
Volume of stationary objectVSStrength

Solution Approach 1:

The invention replaces the need for gelling agents with a mechanical consolidation process. After freezing creates the ice crystal template and porous structure, high pressure is applied to densify and consolidate the material, providing mechanical strength through compression rather than through chemical gelling that would compromise the porous structure

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

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 preserves the chemical structure and mechanical properties of the starting material, enabling the production of monolithic materials with enhanced mechanical strength and uniform porosity, while allowing for the incorporation of organic components, thus overcoming the limitations of previous methods.

Implementation Method 1

followed by isostatic compression at low temperatures to form ice crystals

Methodology Applied
Scientific EffectFreezing: Freezing

Implementation Method 2

isostatic compression at low temperatures to form ice crystals, which acts as a template for consolidating the powder into a monolith

Methodology Applied
Scientific EffectCompression: Compression

Data Source

PatentEP3325033B1Method for producing a porous monolithic material
Publication Date: 2022.01.12 CENT NAT DE LA RECH SCI (C N R S)
  • EP3325033B1 patent drawingFigure 1
  • EP3325033B1 patent drawingFigure 2
  • EP3325033B1 patent drawingFigure 3

AI summary

The invention relates to a method for producing a porous monolithic material from at least one powder, preferably mineral, said method comprising at least one step of low-temperature compression of a mixture based on powder and at least one solvent, preferably water. The materials produced by said method have improved mechanical properties compared to the prior art materials. The materials for medical application, such as hydroxyapatite, also have improved biocompatibility compared to the prior art materials. The invention also relates to the materials produced by said method.