Vanadium Phosphate-Carbon Composite Synthesis via Hydrothermal Process

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Solution Overview

Problem

Current methods for preparing vanadium phosphate-carbon composite materials are complex, costly, and often involve the release of harmful gases like ammonia, which complicates industrialization and affects electrochemical performance.

Innovation Solution

A process involving the mixing of a vanadium precursor with H3PO4, a compound containing carboxylic acid functions, and a polysaccharide compound in an aqueous solvent, followed by heating to form a solid residue and then calcining at high temperatures to produce a vanadium phosphate-carbon composite material, avoiding harmful gas release and optimizing electrochemical performance.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If traditional sol-gel process with multiple steps is used, then vanadium phosphate-carbon composite material can be obtained, but the process becomes complex and time-consuming

Engineering Contradiction:
Improveelectrochemical performanceVSAvoidprocess complexity
Core Design Contradiction:
ReliabilityVSDevice complexity

Solution Approach 1:

The patent combines multiple process steps (sol-gel formation, carbon coating, and vanadium phosphate synthesis) into a single integrated hydrothermal reaction step. By mixing vanadium precursor, phosphate source, and carbon source together in one pot and performing hydrothermal treatment, the method eliminates intermediate steps such as separate gel formation, drying, and carbon coating operations, thereby simplifying the overall process while maintaining electrochemical performance

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The patent performs preliminary mixing of all reactants (vanadium precursor, phosphate source, carbon source, and water) in specific stoichiometric ratios before the hydrothermal reaction. This preliminary preparation ensures that all components are properly distributed and positioned for simultaneous reaction during hydrothermal treatment, avoiding the need for subsequent mixing or addition steps

Inventive Principle:
Principle #10Preliminary action

2Reliability

If NH4H2PO4 is used as phosphate source, then vanadium phosphate can be formed, but ammonia is released making industrialization difficult

Engineering Contradiction:
Improveelectrochemical performanceVSAvoidammonia release
Core Design Contradiction:
ReliabilityVSObject-generated harmful factors

Solution Approach 1:

The patent changes the chemical parameter of the phosphate source from ammonium phosphate (NH4H2PO4) to alternative phosphate sources such as phosphoric acid (H3PO4) or metal phosphates. This parameter change eliminates the release of harmful ammonia gas during the reaction while still providing the necessary phosphate ions for vanadium phosphate formation, thereby improving environmental compatibility for industrialization

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent converts the potentially harmful ammonia release into a beneficial outcome by selecting phosphate sources that do not generate harmful gases. The reaction conditions are optimized to ensure complete reaction without side products, transforming a harmful process into a clean, environmentally friendly synthesis method suitable for industrial application

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

3Manufacturing precision

If intimate comminution of vanadium phosphate precursor and glucose is performed, then homogeneous carbon coating is obtained, but the process becomes more complex and expensive

Engineering Contradiction:
Improvecarbon coating homogeneityVSAvoidprocess complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent performs preliminary mixing of the carbon source (glucose or other carbohydrates) with the vanadium phosphate precursor and phosphate source in the aqueous solution before hydrothermal treatment. This preliminary distribution ensures uniform carbon source availability throughout the reaction mixture, leading to homogeneous carbon coating formation during the hydrothermal reaction without requiring subsequent comminution or mixing steps

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent uses water as an intermediary medium to dissolve and distribute the carbon source (glucose) uniformly throughout the reaction mixture before hydrothermal treatment. This aqueous medium acts as a carrier that ensures homogeneous distribution of carbon precursor around vanadium phosphate nuclei, facilitating uniform carbon coating formation during the reaction without mechanical comminution

Inventive Principle:
Principle #24Intermediary (Mediator)

4Reliability

If multiple heating steps are used, then complete reaction and carbonization are achieved, but the process time increases

Engineering Contradiction:
Improvereaction completenessVSAvoidprocess duration
Core Design Contradiction:
ReliabilityVSLoss of time

Solution Approach 1:

The patent merges the heating step for chemical reaction and the heating step for carbonization into a single hydrothermal treatment step. By performing both functions simultaneously at elevated temperature and pressure in an autoclave, the method eliminates the need for separate heating stages, thereby reducing total process time while ensuring complete reaction and adequate carbon coating formation

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The patent utilizes phase transition of water to supercritical or near-supercritical conditions during hydrothermal treatment. This phase transition enables the system to achieve high temperature and pressure conditions that promote complete reaction and carbonization in a single step, eliminating the need for multiple heating stages required in conventional atmospheric pressure methods

Inventive Principle:
Principle #36Phase transitions

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 simplifies the production of vanadium phosphate-carbon composite materials, enhances electrochemical performance, and avoids the use of harmful gases, leading to improved stability and efficiency in lithium-ion or sodium-ion batteries.

Implementation Method 1

heating the mixture of step i) to a temperature of about 35° C. to 100° C., to form a solid residue

Methodology Applied
Scientific EffectEvaporation: Evaporation

Implementation Method 2

heating the solid residue to a temperature above about 850° C.

Methodology Applied
Scientific EffectHeating: Heating

Data Source

PatentUS11569497B2Liquid process for preparing a vanadium phosphate-carbon composite material
Publication Date: 2023.01.31 CENT NAT DE LA RECH SCI (C N R S)
  • US11569497B2 patent drawing
  • US11569497B2 patent drawing
  • US11569497B2 patent drawing

AI summary

The invention relates to a process for the preparation of a vanadium-carbon phosphate composite material, a vanadium-carbon phosphate composite material obtained according to the process, and to the uses of the composite material, especially as a precursor for the synthesis of electrochemically-active materials, electrode or active anode material.