Indium Phosphide Synthesis via Liquid Phosphorus Injection

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Solution Overview

Problem

Current methods for synthesizing indium phosphide (InP) polycrystalline materials, such as the horizontal Bridgman method and phosphorus injection synthesis, face challenges including long synthesis times, contamination, high costs, and inefficiencies due to the two-step process, which affect the quality and purity of the material.

Innovation Solution

A process involving the liquefaction of phosphorus vapor to facilitate an instantaneous reaction with liquid indium, using a system comprising a quartz phosphorus bubble, condenser, phosphorus source furnace, and low-temperature inert gas delivery, ensuring high-purity and efficient synthesis of InP polycrystalline material for subsequent monocrystal growth.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If horizontal Bridgman method or horizontal gradient solidification method is used to synthesize InP polycrystalline materials, then the synthesis can be performed with conventional equipment, but the synthesis time becomes very long (about 24 hours for 1.5 Kg) and the synthesis capacity is limited

Engineering Contradiction:
Improvesynthesis capacityVSAvoidsynthesis time
Core Design Contradiction:
ProductivityVSLoss of time

Solution Approach 1:

The patent changes the physical state of phosphorus from solid to liquid, and introduces it in a controlled manner to the indium melt. This parameter change enables rapid synthesis (completing in minutes rather than hours) while achieving large-scale production (kilogram to tens of kilogram level) without the time and capacity limitations of conventional slow-heating methods.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent uses liquid phosphorus injection technology where liquid phosphorus is injected into the indium melt under controlled pressure and flow conditions. This hydraulic approach enables precise control of the reaction rate and synthesis capacity, allowing rapid large-scale synthesis without the time constraints of solid-state diffusion methods.

Inventive Principle:
Principle #29Pneumatics and hydraulics

2Productivity

If phosphorus vapor is injected into indium melt using pressure difference, then the synthesis can proceed, but bubble burst occurs and phosphorus vapor is not fully absorbed, affecting synthesis effect and causing volatilization to furnace body

Engineering Contradiction:
Improvesynthesis efficiencyVSAvoidsynthesis stability
Core Design Contradiction:
ProductivityVSReliability

Solution Approach 1:

The patent changes the state of phosphorus from vapor to liquid before injection. Liquid phosphorus is injected directly into the indium melt, eliminating the bubble formation and pressure control issues associated with vapor injection. This ensures complete absorption of phosphorus by the melt and prevents volatilization to the furnace body, improving both reliability and efficiency.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent introduces an inert gas (argon or nitrogen) as an intermediary carrier to transport liquid phosphorus to the indium melt. This intermediary approach allows controlled delivery of phosphorus without direct pressure differential injection, preventing bubble burst and ensuring stable, complete absorption while maintaining high synthesis efficiency.

Inventive Principle:
Principle #24Intermediary (Mediator)

3Manufacturing precision

If two-step process (synthesis in synthesis furnace then monocrystal growth in high-pressure monocrystal furnace) is used, then InP polycrystalline material can be prepared and subsequently grown into monocrystals, but the process complexity increases and contamination risk increases

Engineering Contradiction:
Improvematerial purityVSAvoidprocess steps
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent combines the synthesis and monocrystal growth processes into a single high-pressure monocrystal furnace system. Liquid phosphorus is injected directly into the indium melt within the same furnace where monocrystal growth occurs, eliminating the need for separate synthesis and growth furnaces. This integration reduces contamination risk between steps and simplifies the overall process while maintaining high material purity.

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The patent enables continuous synthesis and crystal growth in one uninterrupted process. The liquid phosphorus is injected into the indium melt, InP forms in-situ, and monocrystals grow continuously from the InP-rich melt without removing the material from the furnace. This continuous process eliminates contamination risks associated with intermediate handling and transfers between different furnaces.

Inventive Principle:
Principle #20Continuity of useful 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

This method enables high-efficiency, high-purity synthesis of InP with precise proportioning, reducing contamination and costs, and allowing for continuous crystal growth with improved integrity and thermal stability of the resulting monocrystals.

Implementation Method 1

vaporizing the phosphorus in the quartz phosphorus bubble by heating the phosphorus source furnace

Methodology Applied
Scientific EffectVaporization: Evaporation

Implementation Method 2

condensing the vaporized phosphorus vapor into liquid white phosphorus through the condenser

Methodology Applied
Scientific EffectCondensation: Condensation

Implementation Method 3

flowing the liquid white phosphorus into the indium melt to react and synthesize a proportioned indium phosphide

Methodology Applied
Scientific EffectChemical reaction: Chemical Bonding

Data Source

PatentUS12116690B2Process for synthesizing indium phosphide by liquid phosphorus injection method
Publication Date: 2024.10.15 THE 13TH RES INST OF CHINA ELECTRONICS TECH GRP CORP
  • US12116690B2 patent drawing

AI summary

The present invention relates to a process for synthesizing indium phosphide by liquid phosphorus injection method, which belongs to the field of semiconductor technology. The method comprises: converting gaseous phosphorus into liquid phosphorus through a condenser, injecting the liquid phosphorus into an indium melt while preventing phosphorus vaporization by randomly delivering a low temperature inert gas, and causing an instantaneous reaction between the liquid phosphorus and the liquid indium melt, so that an indium phosphide melt can be synthesized at a relatively low temperature, with advantages of high efficiency, high purity, precise proportioning, large capacity, aiding in the growth of a phosphorus-rich indium phosphide polycrystal and facilitating the growth of an indium phosphide monocrystal. The method includes the steps of indium cleaning, phosphorus charging, furnace loading, communication of condenser, synthesis, preparation of crystals, etc.