Grafting Polymers on Metal Oxide Surfaces via Silane Anchoring

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Solution Overview

Problem

Current methods for covalently attaching polymers to metal-based substrates, especially those with metal oxides, lack simplicity, efficiency, and versatility, and are not industrially applicable, limiting the ability to confer a wide range of modified properties such as anti-adhesive, cytotoxic, and biocompatible characteristics.

Innovation Solution

A two-step method involving the grafting of hetero-bifunctional anchoring molecules followed by a thiol-ene reaction with polymers, allowing for high-density, high-yielding immobilization of polymers onto metal oxide surfaces, including titanium-based substrates, using photo-initiated reactions to control linker length and surface density.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of manufacture

If simple adsorption methods are used to immobilize surface treatment molecules, then the process is simple, but the stability of immobilisation is low and molecules detach easily

Engineering Contradiction:
Improvesimplicity of immobilization processVSAvoidstability of polymer attachment
Core Design Contradiction:
Ease of manufactureVSReliability

Solution Approach 1:

The patent applies preliminary action by first creating a self-assembled monolayer of silane molecules on the metal oxide surface before introducing the polymer. This pre-prepared layer with exposed alkenyl groups provides stable covalent attachment points, eliminating the instability issue of simple adsorption while maintaining process simplicity.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent uses an intermediary approach by introducing a silane-based anchoring molecule layer as a mediator between the metal oxide surface and the polymer. This intermediary layer provides both stability through covalent bonding and versatility for different polymer types, resolving the contradiction between simple attachment and stable immobilization.

Inventive Principle:
Principle #24Intermediary (Mediator)

2Reliability

If aggressive chemical treatments are used to remove the passivating oxide layer, then covalent attachment to metal is achieved, but the process becomes complex and requires extensive cleaning procedures

Engineering Contradiction:
Improvecovalent attachment strengthVSAvoidcomplexity of surface treatment process
Core Design Contradiction:
ReliabilityVSDevice complexity

Solution Approach 1:

The patent converts the harmful effect of the stable passivating oxide layer into a benefit by designing silane molecules that specifically target and bind to oxide surface groups. Instead of removing the oxide layer, the method utilizes it as the anchoring point for polymer attachment, simplifying the process while maintaining covalent attachment strength.

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

Solution Approach 2:

The patent applies parameter changes by modifying the chemical nature of the surface treatment from aggressive oxide removal to gentle silane grafting on intact oxide surfaces. This parameter change in the treatment approach maintains covalent attachment capability while dramatically reducing process complexity and eliminating the need for extensive cleaning procedures.

Inventive Principle:
Principle #35Parameter changes

3Reliability

If hydroxylated surface oxide is used for polymer grafting, then direct covalent linkage is achieved, but the method is limited to specific hydrophobic siloxane polymers and excludes hydrophilic polymers

Engineering Contradiction:
Improvecovalent linkage capabilityVSAvoidrange of applicable polymer types
Core Design Contradiction:
ReliabilityVSAdaptability or versatility

Solution Approach 1:

The patent applies universality by designing the silane-based anchoring layer with exposed alkenyl groups that can undergo thiol-ene reactions with diverse polymer types. This universal attachment mechanism works with both hydrophobic and hydrophilic polymers, including those containing hydroxyl groups, thereby expanding adaptability while maintaining covalent linkage capability.

Inventive Principle:
Principle #6Universality (Multi-functionality)

Solution Approach 2:

The patent changes the chemical parameter of the surface functional groups from hydroxyl groups to exposed alkenyl groups on the silane layer. This parameter change enables versatile covalent attachment to various polymer types through thiol-ene chemistry, overcoming the limitation to only hydrophobic siloxane polymers while preserving direct covalent linkage.

Inventive Principle:
Principle #35Parameter changes

4Reliability

If in situ copolymerization is used to bind polymers to titanium dioxide, then covalent binding is achieved, but the method requires extensive adjustments and specialized techniques not available to general users

Engineering Contradiction:
Improvecovalent binding strengthVSAvoidease of implementation
Core Design Contradiction:
ReliabilityVSEase of manufacture

Solution Approach 1:

The patent applies segmentation by dividing the polymer attachment process into two independent steps: first forming a silane-based anchoring layer, then introducing the polymer. This segmentation simplifies the process compared to in situ copolymerization, making it easier to implement while maintaining covalent binding strength through the thiol-ene reaction mechanism.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The patent uses an intermediary silane layer with exposed alkenyl groups as a mediator between the titanium dioxide surface and the polymer. This intermediary approach replaces the complex in situ copolymerization process with simpler sequential steps, improving ease of implementation while preserving covalent binding through the thiol-ene reaction.

Inventive Principle:
Principle #24Intermediary (Mediator)

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 enables the efficient and versatile functionalization of metal substrates with polymers, achieving high surface density and long-lasting polymer layers, which can confer anti-adhesive, cytotoxic, and biocompatible properties, suitable for medical implants and other applications.

Implementation Method 1

exposing said substrate surface to a hetero-bifunctional anchoring molecule carrying at least a silane group

Methodology Applied
Scientific EffectSilane grafting: Chemical Bonding

Implementation Method 2

a second step of exposing the substrate surface to a polymer carrying at least three groups A2 capable of reacting with A1 in a thiol-ene reaction

Methodology Applied
Scientific EffectThiol-ene reaction: Photopolymerisation

Data Source

PatentEP2919920B1Method for grafting polymers on metallic substrates
Publication Date: 2020.07.08 CENT NAT DE LA RECH SCI (C N R S)
  • EP2919920B1 patent drawingFigure 1
  • EP2919920B1 patent drawingFigure 2
  • EP2919920B1 patent drawing

AI summary

The present invention relates to a method of conferring modified properties, e.g. modified physical and/or biochemical properties, to a metallic substrate surface, comprising at least two steps consisting in(i) a first step comprising at least exposing said substrate surface to a hetero-bifunctional anchoring molecule carrying at least a silane group and at least a A group,said A group being optionally introduced within said anchoring molecule via a preliminary functionalizing step, and (ii) a second step of exposing the substrate surface to a polymer carrying at least three groups A2 capable of reacting with A in a thiol-ene reaction,the number average molecular weight of said polymer being greater than 1 000 g/mol.