Chlorine-Free Polysilane Synthesis for SiC Fibers

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Solution Overview

Problem

The production of chlorine-free and infusible polysilanes for silicon carbide fibers is hindered by complex synthesis processes, high chlorine content, and low yield, as well as the need for costly and non-reproducible thermal crosslinking methods, which affect the mechanical strength and stability of the fibers.

Innovation Solution

A process involving the disproportionation of methylchlorodisilane mixtures, followed by chlorine substitution with primary amines, and crosslinking using chain formers with nucleophilic groups, results in a chlorine-free polysilane with low chlorine content, high yield, and improved processing characteristics.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Stability of the object's composition

If thermal crosslinking is used to produce infusible polysilane, then the polysilane becomes infusible and suitable for fiber production, but the process becomes costly, non-reproducible, and yields low amounts of product

Engineering Contradiction:
Improveinfusibility of polysilaneVSAvoidyield of polysilane
Core Design Contradiction:
Stability of the object's compositionVSProductivity

Solution Approach 1:

The invention changes the chemical parameters of the oligosilane by introducing nitrogen-containing groups through reaction with amines or amides. This chemical modification enables crosslinking without requiring thermal treatment, thereby achieving infusibility while maintaining high yield and avoiding the drawbacks of thermal crosslinking such as cost, reproducibility issues, and product loss

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention uses amines or amides as intermediary substances to facilitate crosslinking. These nitrogen-containing compounds react with the oligosilane to form crosslinked structures, serving as a温和 mediator that achieves the desired infusibility without the harsh conditions of thermal crosslinking

Inventive Principle:
Principle #24Intermediary (Mediator)

2Stability of the object's composition

If thermal crosslinking is used to produce infusible polysilane, then the polysilane becomes infusible, but highly reactive cleavage products are formed that require complex removal procedures

Engineering Contradiction:
Improveinfusibility of polysilaneVSAvoidcomplexity of product purification
Core Design Contradiction:
Stability of the object's compositionVSDevice complexity

Solution Approach 1:

The invention converts the potentially harmful highly reactive cleavage products of thermal crosslinking into benign byproducts. By using amine or amide-mediated crosslinking, the reaction produces ammonia or amide molecules as byproducts, which are easily removed and do not require complex purification procedures

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

3Quantity of substance

If chlorine substitution is performed using conventional methods, then chlorine content is reduced, but the process requires multiple steps including thermal crosslinking and redissolution, reducing yield and increasing cost

Engineering Contradiction:
Improvechlorine content of polysilaneVSAvoidsimplicity of production process
Core Design Contradiction:
Quantity of substanceVSEase of manufacture

Solution Approach 1:

The invention merges the chlorine substitution step with the crosslinking step into a single integrated process. The amine or amide reagent simultaneously replaces chlorine atoms and forms crosslinked structures, eliminating the need for separate thermal crosslinking and redissolution steps, thereby simplifying the manufacturing process and increasing yield

Inventive Principle:
Principle #5Merging (Combining)

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 process produces polysilanes with less than 1% chlorine content, enabling the production of high-quality, infusible, and soluble fibers suitable for silicon carbide composites, offering cost-effectiveness, reproducibility, and improved mechanical properties.

Implementation Method 1

a disproportionation reaction of a methylchlorodisilane mixture to form a chlorine-containing oligosilane

Methodology Applied
Scientific EffectDisproportionation reaction: Chemical Bonding

Implementation Method 2

a substitution reaction of the chlorine atoms contained in the oligosilane by reaction with a primary amine

Methodology Applied
Scientific EffectNucleophilic substitution: Chemical Bonding

Implementation Method 3

a crosslinking reaction of the oligosilanes using a chain former to form polysilanes

Methodology Applied
Scientific EffectCrosslinking reaction: Chemical Bonding

Data Source

PatentEP2931789B1Method for the synthesis of a chlorine-free, pre-cermanic polymer for the production of ceramic molded bodies
Publication Date: 2019.03.27 BJS CERAMICS
  • EP2931789B1 patent drawingFigure 1

AI summary

A method for producing a polysilane includes a disproportionation reaction of a methylchlorodisilane mixture to form chlorine-containing oligosilane, a substitution reaction of the chlorine atoms contained in the oligosilane by the reaction with a primary amine and a cross-linking reaction of the oligosilanes using a chain former to form polysilanes. The obtained polysilanes are infusible and are very suitable for being spun to form green fibers and processed to form silicon carbide fibers and fiber composites. The method is characterized in that it can be carried out cost-effectively and quickly and with very high yields.