Fluorinated Graphene Two-Step Synthesis High Fluorine Content

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Solution Overview

Problem

Existing methods for preparing fluorinated graphene result in low fluorine content, which limits its application in fields like surface treatment and lubrication.

Innovation Solution

A two-step fluorination process involving a first fluorinating agent, such as fluorine gas, followed by a second fluorinating agent like gas-phase fluoride, under inert gas protection, to achieve a high fluorine content of 50%-80% in the graphene, ensuring intact sheets without defects.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of manufacture

If a single-step fluorination process is used, then the preparation process is simple, but the fluorine content is low

Engineering Contradiction:
Improvepreparation process simplicityVSAvoidfluorine content
Core Design Contradiction:
Ease of manufactureVSQuantity of substance

Solution Approach 1:

The fluorination process is divided into two distinct steps: first fluorination using fluorine gas to introduce fluorine atoms and form C-F bonds, followed by second fluorination using gas-phase fluoride to further increase fluorine content. This segmentation allows each step to optimize for its specific function, achieving high overall fluorine content while maintaining process clarity and controllability.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The first fluorination step acts as a preliminary action that prepares the graphene structure by introducing initial fluorine atoms and creating reactive sites. This preliminary fluorination enables the second fluorination step to proceed more effectively, as the pre-modified structure is more receptive to further fluorine incorporation, ultimately achieving high fluorine content.

Inventive Principle:
Principle #10Preliminary action

2Quantity of substance

If high fluorine content is achieved through extended reaction time, then fluorine content increases, but production efficiency decreases

Engineering Contradiction:
Improvefluorine contentVSAvoidproduction efficiency
Core Design Contradiction:
Quantity of substanceVSProductivity

Solution Approach 1:

The invention changes multiple parameters systematically: using different fluorinating agents (fluorine gas then gas-phase fluoride), different temperature ranges (150-550°C then 150-400°C), and different time periods (2-20 h then 2-10 h) for each fluorination step. This parameter optimization allows achieving high fluorine content (50%-80%) while controlling reaction intensity and duration to maintain production efficiency.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The two fluorination steps are designed to be continuous and complementary, with the second step building upon the first. This continuous action ensures that fluorine incorporation proceeds efficiently through both stages without interruption, maximizing fluorine content achievement while minimizing total processing time and maintaining high productivity.

Inventive Principle:
Principle #20Continuity of useful action

3Ease of manufacture

If fluorine gas is used as the only fluorinating agent, then the process is simple, but the fluorine content cannot reach theoretical level

Engineering Contradiction:
Improveprocess simplicityVSAvoidfluorine content precision
Core Design Contradiction:
Ease of manufactureVSManufacturing precision

Solution Approach 1:

Gas-phase fluoride acts as an intermediary fluorinating agent that bridges the gap between simple fluorine gas treatment and high fluorine content achievement. The gas-phase fluoride provides additional fluorine atoms through a different reaction mechanism, complementing the first fluorination step and enabling the structure to reach near-theoretical fluorine content while keeping the overall process relatively simple.

Inventive Principle:
Principle #24Intermediary (Mediator)

Data Source

PatentUS10850986B2Fluorinated graphene and preparation method thereof
Publication Date: 2020.12.01 HUNAN YUANCHANG NEW MATERIAL TECHNOLOGY CO LTD
  • US10850986B2 patent drawing

AI summary

The present invention relates to a preparation method of fluorinated graphene. The method for preparing fluorinated graphene, including the following steps: S1), under the protection of inert gas, the graphene undergoes a fluorination reaction with a first fluorinating agent, the reaction temperature is 150-550° C., the reaction time is 2-20 h, and a fluorinated graphene crude product is obtained. The graphene is graphene powder, or a graphene film; the first fluorinating agent includes fluorine gas; S2), under the protection of inert gas, the fluorinated graphene crude product undergoes a fluorination reaction with a second fluorinating agent, the reaction temperature is 150-400° C., the reaction time is 2-10 h, and a fluorinated graphene is obtained. The second fluorinating agent is gas-phase fluoride. By using the method, fluorinated graphene having a high fluorine content can be prepared, the fluorine content is close to the theoretical level, and the defect density is low.