Transition Metal Sulfide ALD for Uniform Ultra-Thin Heterostructures

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Solution Overview

Problem

Existing deposition methods for transition metal sulfides face challenges in achieving uniform, ultra-thin, and continuous layers with controlled crystalline quality, particularly in high form factor architectures, and struggle to form heterostructures or alloys effectively.

Innovation Solution

A vapor deposition process using atomic layer deposition (ALD) cycles with specific precursors at low temperatures (20-250°C) followed by sulfurization and annealing steps, allowing for the formation of amorphous layers that are subsequently crystallized, ensuring uniformity and controlled composition of transition metal sulfides and alloys.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If chemical vapor deposition (CVD) is used to deposit TMD layers, then crystalline quality can be achieved, but control of nucleation and uniformity is difficult, and deposition on high form factor architectures is not possible

Engineering Contradiction:
Improveuniformity of deposited layerVSAvoiddifficulty of implementing CVD on complex architectures
Core Design Contradiction:
Manufacturing precisionVSEase of manufacture

Solution Approach 1:

The CVD process is segmented into multiple sequential deposition steps with different precursor combinations and temperature conditions. This allows independent optimization of nucleation control, uniformity, and crystalline quality for each layer, resolving the contradiction between achieving uniform deposits and maintaining ease of manufacture on complex architectures

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The patent employs dynamic parameter changes during deposition, including temperature modulation and precursor flow rate adjustments, to achieve both uniform nucleation control and adaptability to high form factor architectures while maintaining crystalline quality

Inventive Principle:
Principle #35Parameter changes

2Manufacturing precision

If atomic layer deposition (ALD) is used to deposit ultra-thin TMD layers, then uniform growth can be achieved, but the material must be deposited amorphously requiring post-deposition crystallization annealing

Engineering Contradiction:
Improveuniformity of ultra-thin layersVSAvoidneed for additional crystallization annealing step
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent merges the deposition and crystallization functions into a single integrated process step by using CVD with controlled nucleation, eliminating the need for separate annealing equipment and process steps while maintaining uniform ultra-thin layer deposition

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The deposition process maintains continuous useful action by achieving direct crystalline growth without amorphous intermediate state, eliminating the interruption caused by post-deposition annealing and reducing overall process complexity

Inventive Principle:
Principle #20Continuity of useful action

3Manufacturing precision

If CVD deposition conditions are optimized for crystalline phase formation, then crystal quality is achieved, but deposition of group 5 metals as dopant or heterostructures is difficult

Engineering Contradiction:
Improvecrystalline phase qualityVSAvoiddifficulty of depositing heterostructures and alloys
Core Design Contradiction:
Manufacturing precisionVSAdaptability or versatility

Solution Approach 1:

The patent employs dynamic control of deposition parameters including temperature, pressure, and precursor ratios during the deposition process, allowing transition between different crystalline phases and composition control to achieve both high crystal quality and versatile heterostructure/alloy deposition

Inventive Principle:
Principle #15Dynamics

Solution Approach 2:

The deposition process uses periodic alternation between different precursor introductions and temperature cycles to control nucleation and growth of different materials, enabling precise control of heterostructure formation while maintaining crystalline quality

Inventive Principle:
Principle #19Periodic action

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 process achieves ultra-thin, smooth, and continuous layers with low roughness, enabling the formation of heterostructures and alloys with precise control over composition and orientation, suitable for complex architectures and microelectronic devices.

Implementation Method 1

a process of vapor deposition of a sulfide layer of a transition metal or one of its alloys, the process comprising a step of deposition of atomic layers

Methodology Applied
Scientific EffectAtomic layer deposition: Chemical Vapour Deposition

Implementation Method 2

the deposited layer being crystallized by the substrate being placed in a furnace at a temperature between 400°C and 1150°C

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Implementation Method 3

the deposited layer being crystallized by the substrate being placed in a furnace at a temperature between 400°C and 1150°C

Methodology Applied
Scientific EffectThermal heating: Heating

Data Source

PatentEP4600402A1Process for depositing a thin layer of sulfide from an alloy of transition metal groups 5 and 6, or from one of its heterostructures
Publication Date: 2025.08.13 COMMISSARIAT A LENERGIE ATOMIQUE ET AUX ENERGIES ALTERNATIVES
  • EP4600402A1 patent drawingFigure 1~2
  • EP4600402A1 patent drawing
  • EP4600402A1 patent drawing

AI summary

The present description relates to a process for vapor deposition of a sulfide layer of a transition metal by ALD according to the following cycle: - exposing a substrate to a precursor of the transition metal, whereby an intermediate layer is formed, - purging the reactor, - exposing the intermediate layer to a sulfur precursor, - purging the reactor, the substrate being at a temperature between 20°C and 250°C during the cycle, The cycle can be repeated several times with the same precursors or with different precursors, the precursor of the transition metal being chosen from molybdenum oxyhalides, tungsten oxyhalides, vanadium halides, niobium halides and tantalum halides.