WCl6 Purification via Fluidized Bed Condensation

Resolve Bottlenecks,
Find Innovative Solutions
Generate Solutions

Solution Overview

Problem

Current methods for purifying tungsten hexachloride (WCl6) often result in a mixture of alpha and beta crystal forms, with sublimation producing mostly alpha form and mechanical harvesting leading to wide particle sizes and impurity contamination, making it unsuitable for semiconductor applications.

Innovation Solution

A system and method involving a boiler, condenser, and fluidizing gas to vaporize WCl6, followed by condensation in a fluidizing bed, which selectively produces at least 95% beta-form crystals with controlled particle size and low impurity levels, using a process that maintains temperatures between 100°C to 180°C and employs a carrier gas to separate impurities.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If sublimation is used for purification, then productivity is enhanced and operation temperature is reduced, but the product attaches to cold wall requiring additional labor and mechanical apparatus for harvesting, and produces wide particle size distribution

Engineering Contradiction:
Improvepurification speedVSAvoidharvesting difficulty
Core Design Contradiction:
ProductivityVSEase of operation

Solution Approach 1:

The patent replaces mechanical scraping apparatus with a fluidization-based harvesting system. The fluidizing gas fluidizes the condensed product particles, allowing them to be easily removed through gas flow without requiring mechanical scraping tools or additional labor-intensive processes.

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

Solution Approach 2:

The patent uses fluidizing gas flow to transport and remove the purified product particles from the condensation zone. The pneumatic fluidization system enables easy product recovery and control of particle size distribution through adjustment of gas flow parameters.

Inventive Principle:
Principle #29Pneumatics and hydraulics

2Productivity

If mechanical harvesting is used, then product can be collected, but particle size becomes wide and impurity contamination increases

Engineering Contradiction:
Improveproduct collection efficiencyVSAvoidparticle size control
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The patent replaces mechanical harvesting with a fluidization-based collection system. The fluidizing gas gently suspends and transports particles, avoiding the mechanical contact and scraping that cause particle size variation and impurity contamination associated with traditional mechanical harvesting methods.

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

3Productivity

If alpha-form WCl6 is produced, then sublimation is effective, but vaporization rate is inconsistent and shelf life is reduced

Engineering Contradiction:
Improvepurification efficiencyVSAvoidvaporization consistency
Core Design Contradiction:
ProductivityVSReliability

Solution Approach 1:

The patent changes the crystal form parameter from alpha-form to beta-form WCl6 through controlled condensation conditions. The beta-form crystals exhibit consistent vaporization rates and improved shelf life, resolving the reliability issues associated with alpha-form material while maintaining purification effectiveness.

Inventive Principle:
Principle #35Parameter changes

4Reliability

If high temperature processing is used, then decomposition is prevented, but corrosion hazards increase and special equipment is required

Engineering Contradiction:
Improvedecomposition preventionVSAvoidequipment requirements
Core Design Contradiction:
ReliabilityVSDevice complexity

Solution Approach 1:

The patent changes the processing temperature parameter to a lower range that is sufficient to prevent decomposition of WCl6 without requiring the high temperatures that cause corrosion. This reduces equipment complexity and eliminates the need for special corrosion-resistant materials while maintaining product integrity.

Inventive Principle:
Principle #35Parameter changes

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

The method achieves high purity WCl6 with greater than 95% beta-form crystals, suitable for semiconductor manufacturing, ensuring consistent vaporization rates and improved shelf life, while avoiding mechanical scraping and impurity contamination.

Implementation Method 1

the boiler is heated to one or more temperatures at or above the boiling point of WCl6 to cause at least a portion of the crude material to vaporize

Methodology Applied
Scientific EffectVaporization: Evaporation

Implementation Method 2

the condenser stream is maintained at one or more temperatures ranging from 100 to 180°C wherein at least a portion of the condenser stream condenses

Methodology Applied
Scientific EffectCondensation: Condensation

Implementation Method 3

the condenser comprises a fluidizing bed which selectively produces at least 95% beta-form crystals

Methodology Applied
Scientific EffectFluidization: Fluidisation

Data Source

PatentEP3081667B1A delivery system for depositing tungsten film or tungsten containing film and a process of preparing the delivery system
Publication Date: 2021.07.28 VERSUM MATERIALS US LLC
  • EP3081667B1 patent drawingFigure 1
  • EP3081667B1 patent drawingFigure 2
  • EP3081667B1 patent drawing

AI summary

Condensable metal halide materials, such as but not limited to tungsten chloride (WCl6), can be used deposit films metal or metal containing films in a chemical vapor deposition (CVD) or atomic layer deposition process. Described herein are high purity compositions comprising condensable materials and methods to purify condensable materials. In one aspect, there is provided a composition comprising: tungsten hexachloride which is substantially free of at least one impurity and wherein the tungsten hexachloride comprises at least 90%, preferably 95 % and more preferably 99 % by weight or greater of a β- WCl6 and 5% by weight or less of the α- WCl6 as measured by X-ray diffraction.