Titanium Hydride Powder via Combined Hydrogen-Magnesium Reduction

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Solution Overview

Problem

Current methods for manufacturing titanium powders are costly, energy-intensive, and inefficient, with multi-stage processes that result in impurities and inferior mechanical properties, making them unsuitable for high-performance applications.

Innovation Solution

A combined hydrogen-magnesium reduction process for titanium chlorides, incorporating titanium hydride powder and metal halides, which reduces the need for hydro-metallurgical treatment and allows for the production of high-purity titanium hydride powders and alloys in a single cycle, utilizing vacuum distillation to remove magnesium and magnesium chloride efficiently.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If conventional multi-stage processes are used for manufacturing titanium powders, then production experience is gained, but production time and energy consumption increase significantly

Engineering Contradiction:
Improveproduction experienceVSAvoidproduction time
Core Design Contradiction:
ReliabilityVSLoss of time

Solution Approach 1:

The patent combines multiple conventional processing steps (reduction, hydrogenation, and vacuum separation) into a single integrated process. Titanium halide is reduced by magnesium in the presence of hydrogen atmosphere, directly producing titanium hydride powder without requiring separate hydrogenation and vacuum treatment steps, thereby significantly reducing production time while maintaining product quality

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The process maintains continuous useful action by conducting reduction and hydrogenation simultaneously in one operation. The hydrogen atmosphere is maintained throughout the reduction process, allowing continuous hydrogen uptake by the reduced titanium to form hydride, eliminating idle time between sequential operations

Inventive Principle:
Principle #20Continuity of useful action

2Reliability

If conventional multi-stage processes are used for manufacturing titanium powders, then production experience is gained, but energy consumption increases

Engineering Contradiction:
Improveproduction experienceVSAvoidenergy consumption
Core Design Contradiction:
ReliabilityVSUse of energy by moving object

Solution Approach 1:

The patent merges reduction and hydrogenation into one energy-efficient operation. The exothermic reduction reaction provides heat for the endothermic hydrogenation process, reducing external energy input requirements compared to separate staged operations

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The reduction reaction itself generates the conditions needed for hydrogenation. The heat from magnesium reduction of titanium halide maintains the temperature required for hydrogen dissolution and hydride formation, making the process self-sufficient regarding thermal energy

Inventive Principle:
Principle #25Self-service

3Ease of manufacture

If conventional processes are used for manufacturing titanium powders, then standard production methods are followed, but impurity content increases and mechanical properties deteriorate

Engineering Contradiction:
Improvestandard production methodsVSAvoidpurity and mechanical properties
Core Design Contradiction:
Ease of manufactureVSManufacturing precision

Solution Approach 1:

The patent uses hydrogen atmosphere as an inert (non-oxidizing) environment during reduction and hydrogenation. This prevents oxidation of titanium and magnesium, eliminating a major source of impurities while maintaining ease of manufacture through a straightforward atmospheric control approach

Inventive Principle:
Principle #39Inert atmosphere (Inert environment)

Solution Approach 2:

Hydrogen acts as an intermediary that serves dual functions: it prevents oxidation during reduction (protective atmosphere) and simultaneously reacts with reduced titanium to form hydride (reactive agent). This intermediary role eliminates the need for separate protective atmosphere steps while improving purity

Inventive Principle:
Principle #24Intermediary (Mediator)

4Ease of manufacture

If conventional processes are used for manufacturing titanium powders, then established procedures are followed, but the process requires hydro-metallurgical treatment

Engineering Contradiction:
Improveestablished proceduresVSAvoidprocess complexity
Core Design Contradiction:
Ease of manufactureVSDevice complexity

Solution Approach 1:

The patent extracts (removes) the hydro-metallurgical treatment step from the conventional process sequence. By directly producing titanium hydride powder through in-situ hydrogenation during reduction, the process eliminates the need for subsequent water-based purification and drying operations, simplifying the overall process while maintaining ease of manufacture

Inventive Principle:
Principle #2Taking out (Extraction)

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 significantly reduces production time and energy consumption, achieves high purity and mechanical strength, and enables the production of weldable titanium and titanium alloy components with properties comparable to those produced by conventional ingot metallurgy, while minimizing contaminant content and processing costs.

Implementation Method 1

manufacturing of hydrogenated titanium powders by the metallo-thermic reduction of titanium chlorides

Methodology Applied
Scientific EffectMetallo-thermic reduction: Redox Reactions

Implementation Method 2

supplying hydrogen onto the magnesium surface and in the body of the liquid magnesium at 750-850° C., followed by the dissolution of hydrogen into the liquid magnesium up to saturation

Methodology Applied
Scientific EffectDissolution: Solvation

Implementation Method 3

supplying liquid titanium tetrachloride TiCl4 into the retort filled with liquid magnesium to reduce titanium from the titanium tetrachloride

Methodology Applied
Scientific EffectReduction reaction: Redox Reactions

Implementation Method 4

dissolution of hydrogen in the reduced titanium metal to the end of the reduction reaction at 750-850° C.

Methodology Applied
Scientific EffectDissolution: Solvation

Implementation Method 5

vacuum separation of the subsequently obtained titanium hydride sponge block

Methodology Applied
Scientific EffectVacuum distillation: Vacuum Distillation

Implementation Method 6

vacuum separation (vacuum distillation) of hydrogenated porous titanium compound from magnesium and magnesium chlorides

Methodology Applied
Scientific EffectEvaporation: Evaporation

Implementation Method 7

Sintering is performed by the invented special cycle, allowing for the complete and near complete removal of atomic hydrogen from the sintered alloys

Methodology Applied
Scientific EffectDehydrogenation: Thermolysis

Data Source

PatentUS9067264B2Method of manufacturing pure titanium hydride powder and alloyed titanium hydride powders by combined hydrogen-magnesium reduction of metal halides
Publication Date: 2015.06.30 ADVANCE MATERIALS PRODUCTS INC

AI summary

The invention relates to energy-saving manufacturing of purified hydrogenated titanium powders or alloying titanium hydride powders, by metallo-thermic reduction of titanium chlorides, including their hydrogenation, vacuum separation of titanium hydride sponge block from magnesium and magnesium chlorides, followed by crushing, grinding, and sintering of said block without need for any hydro-metallurgical treatment of the produced powders. Methods disclosed contain embodiments of processes for manufacturing high purity high-purity powders and their use in manufacturing near-net shape titanium and titanium-alloy articles by sintering titanium hydride and alloyed titanium hydride powders produced from combined hydrogen-magnesium reduction of titanium chlorides, halides and hydrides of other metals. Additional titanium hydride powder introduced with titanium tetrachloride beneficially affects the kinetics of magnesium-thermic reduction due to formation of additionally-emitted atomic hydrogen, which helps to reduce presence of oxides, and so cleans inter-particle interfaces of the product and enhances diffusion between all components of the powder mixture.