Molybdenum Oxyhalide Precursor Synthesis via Eutectic Melt

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Solution Overview

Problem

There is a need for improved methods to prepare high-yield and high-purity molybdenum and tungsten oxyhalide precursors for vapor deposition, which are crucial for achieving high conformality and high deposition rates in semiconductor manufacturing, as existing sources like molybdenum pentachloride and MoO2Cl2 lack efficient preparation techniques.

Innovation Solution

A process involving the heating of molybdenum or tungsten trioxide in a solid state or melt-phase reaction with eutectic blends of alkaline and alkaline earth metal salts to produce highly pure crystalline oxyhalides such as MoO2Cl2 and WO2Cl2, facilitating their isolation and deposition.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If conventional sources like molybdenum pentachloride or MoO2Cl2 are used for vapor deposition, then deposition can proceed, but the preparation yield and purity are insufficient for high-volume manufacturing requirements

Engineering Contradiction:
Improvepurity of oxyhalide precursorVSAvoidpreparation yield and efficiency
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The invention changes the preparation parameters by using melt-phase reaction conditions with eutectic blends of alkaline and alkaline earth metal halides, heating to specific temperature ranges (200-900°C) to achieve both high yield and high purity oxyhalide precursors that conventional methods cannot simultaneously provide

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention introduces eutectic blends of alkaline and alkaline earth metal halides as intermediary reaction media that facilitate the conversion of Group VI metal trioxides to oxyhalides, enabling high-yield and high-purity preparation that neither conventional direct chlorination nor simple heating can achieve alone

Inventive Principle:
Principle #24Intermediary (Mediator)

2Manufacturing precision

If high conformality and high deposition rates are required for semiconductor manufacturing, then improved source reagents are needed, but existing preparation methods lack efficiency

Engineering Contradiction:
Improveconformality of deposited filmVSAvoidtime for precursor preparation
Core Design Contradiction:
Manufacturing precisionVSLoss of time

Solution Approach 1:

The invention performs preliminary action by preparing high-purity crystalline oxyhalide precursors in advance using the efficient melt-phase method with eutectic blends, which can then be stored and used repeatedly in vapor deposition processes, reducing preparation time for each deposition run while ensuring consistent film conformality

Inventive Principle:
Principle #10Preliminary action

3Productivity

If molybdenum or tungsten trioxide is heated in solid state, then reaction can proceed, but the yield and purity are insufficient compared to melt-phase reactions

Engineering Contradiction:
Improveyield of oxyhalideVSAvoidreaction temperature
Core Design Contradiction:
ProductivityVSTemperature

Solution Approach 1:

The invention exploits phase transitions by melting the eutectic blend of alkaline and alkaline earth metal halides to create a liquid reaction medium, which dramatically enhances the yield of oxyhalide products compared to solid-state reactions, while the eutectic composition allows melting at lower temperatures than individual components

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 method enables the production of highly pure crystalline oxyhalides, enhancing the deposition of Group VI metal films on microelectronic devices with improved conformality and deposition rates, suitable for high-volume manufacturing.

Implementation Method 1

a molybdenum or tungsten trioxide is heated in either a solid state medium or in a melt-phase reaction comprising a eutectic blend comprising one or more alkaline and/or alkaline earth metal salts

Methodology Applied
Scientific EffectMelt-phase reaction:

Implementation Method 2

a melt-phase reaction comprising a eutectic blend comprising one or more alkaline and/or alkaline earth metal salts

Methodology Applied
Scientific EffectEutectic blend:

Implementation Method 3

The molybdenum or tungsten oxyhalide thus formed may be isolated as a vapor and crystallized

Methodology Applied
Scientific EffectVaporization: Evaporation

Implementation Method 4

The molybdenum or tungsten oxyhalide thus formed may be isolated as a vapor and crystallized to provide highly pure crystalline oxyhalides

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Data Source

PatentUS20240140819A1Oxhalide precursors
Publication Date: 2024.05.02 ENTEGRIS INC
  • US20240140819A1 patent drawing
  • US20240140819A1 patent drawing
  • US20240140819A1 patent drawing

AI summary

The invention provides a process for preparing molybdenum and tungsten oxyhalide compounds which are useful in the deposition of molybdenum and tungsten containing films on various surfaces of microelectronic devices. In the process of the invention, a molybdenum or tungsten trioxide is heated in either a solid state medium or in a melt-phase reaction comprising a eutectic blend comprising alkaline and/or alkaline earth metal salts. The molybdenum or tungsten oxyhalides thus formed may be isolated as a vapor and crystallized to provide highly pure precursor compounds such as MoO2Cl2.