Lithium Titanium Phosphate NASICON Production via Slurry Spray Drying
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Solution Overview
Problem
Existing methods for producing lithium titanium phosphate face challenges in achieving industrially advantageous processes for homogeneously mixing titanium and phosphorus sources and obtaining a single-phase product, with complications in solid-phase methods and vitrification processes.
Innovation Solution
A method involving the preparation of a raw material slurry with titanium dioxide, phosphoric acid, and a surfactant, followed by heat treatment, spray drying with a lithium source, and subsequent firing to produce a single-phase lithium titanium phosphate with a NASICON structure, utilizing divalent or trivalent metal elements like Al and pentavalent elements like Zr to enhance lithium ion conductivity.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Ease of manufacture
If solid-phase reaction method is used to produce lithium titanium phosphate, then the process is simple, but it is difficult to achieve homogeneous mixing of titanium source and phosphorus source
Solution Approach 1:
The invention changes the physical state of raw materials from solid to liquid/solution form, enabling homogeneous mixing at the molecular level. Titanium source, phosphorus source, and lithium source are dissolved in a solvent to create a uniform slurry, which resolves the mixing homogeneity issue while maintaining process simplicity through spray drying technology.
Solution Approach 2:
The invention introduces a solvent as an intermediary medium to facilitate homogeneous mixing of raw materials. The solvent allows titanium source, phosphorus source, and lithium source to be uniformly distributed in solution form, and subsequent spray drying removes the solvent to leave uniformly distributed solid precursors for reaction.
2Manufacturing precision
If vitrification method is used to produce lithium titanium phosphate, then homogeneous mixing can be achieved, but the process becomes complicated
Solution Approach 1:
The invention extracts the homogeneous mixing step from the complex vitrification process by using solution chemistry. Raw materials are mixed homogeneously in solution form, then the solvent is removed through spray drying, leaving uniformly distributed solid precursors that can be directly fired to produce single-phase lithium titanium phosphate, eliminating the need for complex vitrification steps.
Solution Approach 2:
The invention replaces the mechanical mixing and multiple thermal processing steps of vitrification with a chemical solution-based mixing approach followed by spray drying. This substitution achieves homogeneous distribution more efficiently and simplifies the overall process while maintaining manufacturing precision.
3Productivity
If spray drying is performed without heat treatment, then deposition inside spray dryer occurs, but heat treatment alone does not sufficiently suppress deposition
Solution Approach 1:
The invention performs preliminary heat treatment of the slurry before spray drying to modify the properties of the slurry in advance. This pre-treatment, combined with surfactant addition, prepares the slurry for optimal spray drying performance by reducing deposition tendencies and improving atomization characteristics, thereby enhancing productivity while minimizing harmful deposition.
Solution Approach 2:
The invention introduces a surfactant as an intermediary substance that mediates between the slurry and the spray drying process. The surfactant reduces surface tension and prevents deposition inside the spray dryer, enabling efficient spray drying without the harmful deposition effects that would otherwise occur.
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 production of X-ray diffractometrically single-phase lithium titanium phosphate, improving lithium ion conductivity and simplifying the industrial process by reducing deposition issues during spray drying and enhancing reactivity of the reaction precursor.
Implementation Method 1
by heat treating a mixed slurry (1) containing titanium dioxide, phosphoric acid and a surfactant, due to the synergetic effect of an effect by the heat treatment and an effect of the surfactant added, the mixed slurry turns to a lithium-containing heat-treated slurry (3) suppressed in deposition inside a spray dryer
Implementation Method 2
a second step of heat treating the raw material mixed slurry (1) to obtain a raw material heat-treated slurry (2)
Implementation Method 3
a fourth step of subjecting the lithium-containing raw material heat-treated slurry (3) to a spray drying treatment to obtain a reaction precursor
Implementation Method 4
by firing the reaction precursor, an x-ray diffractometrically single-phase lithium titanium phosphate is easily obtained
Implementation Method 5
a fifth step of firing the reaction precursor
Data Source
AI summary
An X-ray diffractometrically single-phase lithium titanium phosphate can be obtained by an industrially advantageous method. Provided is a method for producing the lithium titanium phosphate having a NASICON structure represented by the following general formula (1): Li1+xMx(Ti1−yAy)2−x(PO4)3 (1), and provided is a method comprising a first step of preparing a raw material mixed slurry (1) comprising, at least, titanium dioxide, phosphoric acid and a surfactant, a second step of heat treating the raw material mixed slurry (1) to obtain a raw material heat-treated slurry (2), a third step of mixing the raw material heat-treated slurry (2) with a lithium source to obtain a lithium-containing raw material heat-treated slurry (3), a fourth step of subjecting the lithium-containing raw material heat-treated slurry (3) to a spray drying treatment to obtain a reaction precursor containing, at least, Ti, P and Li, and a fifth step of firing the reaction precursor.