Optical ZnS Material Preparation via Elemental Sulfur CVD

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Solution Overview

Problem

Existing methods for preparing CVDZnS materials result in high emissivity due to hydrogen-zinc complexes and excessive internal impurities, limiting their application to temperatures below 200°C due to reduced transmittance and increased radiation.

Innovation Solution

A chemical vapor deposition method involving controlled heating and inert gas management to maintain a saturated sulfur vapor pressure of 0.8 to 1.8 KPa, avoiding the formation of hydrogen-zinc complexes by not decomposing H2S, thereby reducing emissivity and enhancing transmittance across a broader temperature range.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of manufacture

If H2S gas is used as raw material for CVDZnS preparation, then the deposition process can proceed, but hydrogen-zinc complexes form causing high scattering and reduced transmittance

Engineering Contradiction:
Improvedeposition processVSAvoidtransmittance
Core Design Contradiction:
Ease of manufactureVSManufacturing precision

Solution Approach 1:

The patent extracts and removes the harmful hydrogen component from the traditional H2S raw material system. By replacing H2S with elemental sulfur (S8) as the raw material, the decomposition reaction that produces hydrogen ions is eliminated, thereby preventing the formation of hydrogen-zinc complexes that cause scattering and reduce transmittance.

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The patent changes the chemical composition parameter of the raw material from hydrogen-containing (H2S) to hydrogen-free (elemental sulfur). This fundamental parameter change alters the reaction pathway, preventing hydrogen ion generation and subsequent complex formation with zinc vapor, thus improving optical transmittance.

Inventive Principle:
Principle #35Parameter changes

2Quantity of substance

If H2S decomposition occurs during reaction, then sulfur is supplied for ZnS formation, but excessive internal impurities increase long-wave band emissivity to 0.3 or more

Engineering Contradiction:
Improvesulfur supplyVSAvoidemissivity
Core Design Contradiction:
Quantity of substanceVSObject-generated harmful factors

Solution Approach 1:

The patent converts the traditional approach of using H2S (which decomposes to provide sulfur but creates harmful hydrogen impurities) into using elemental sulfur directly. This eliminates the harmful decomposition byproduct (hydrogen) while still achieving complete sulfur supply for ZnS formation, thereby reducing emissivity from 0.3 to below 0.1.

Inventive Principle:
Principle #22Blessing in disguise (Convert harm into benefit)

Solution Approach 2:

The patent changes the raw material parameter from hydrogen sulfide to elemental sulfur, fundamentally altering the chemical reaction pathway. This parameter change eliminates hydrogen ion generation during sulfur supply, preventing the formation of internal impurities that would increase emissivity, thus achieving low-emissivity ZnS material.

Inventive Principle:
Principle #35Parameter changes

3Productivity

If traditional CVDZnS is prepared with H2S, then material can be produced, but application temperature is limited to about 200°C due to high emissivity

Engineering Contradiction:
Improvematerial productionVSAvoidapplication temperature
Core Design Contradiction:
ProductivityVSTemperature

Solution Approach 1:

The patent extracts the limiting factor (hydrogen content from H2S decomposition) that restricts application temperature. By using elemental sulfur instead of H2S, the harmful hydrogen-zinc complexes are eliminated, reducing emissivity and enabling the material to maintain low emissivity at higher temperatures up to 400°C or above.

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The patent changes the raw material composition parameter to eliminate hydrogen, fundamentally improving the material's high-temperature performance. This parameter change reduces long-wave band emissivity, allowing the ZnS material to be used at temperatures of 400°C and above, expanding the application temperature range from 200°C to 400°C or higher.

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 produces CVDZnS with emissivity reduced to 0.01 to 0.1 at 200°C to 400°C, maintaining high transmittance, allowing the material to be used at higher temperatures with improved optical quality and extended application.

Implementation Method 1

heating the first crucible, the second crucible and a deposition chamber... after the zinc and the sulfur are melted, flowing the carrier gases containing zinc vapor and sulfur vapor

Methodology Applied
Scientific EffectVaporization: Evaporation

Implementation Method 2

flowing the carrier gases containing zinc vapor and sulfur vapor respectively into the deposition chamber through pipelines to deposit ZnS on a deposition substrate

Methodology Applied
Scientific EffectChemical vapor deposition: Chemical Vapour Deposition

Data Source

PatentUS11746438B2Method for preparing an optical ZnS material from zinc and sulfur raw material sources by using a feeding device to replenish the sulfur raw material source
Publication Date: 2023.09.05 SINOMA SYNTHETIC CRYSTALS CO LTD
  • US11746438B2 patent drawing
  • US11746438B2 patent drawing

AI summary

The present invention provides an optical ZnS material and a preparation method thereof, wherein the preparation method comprises: charging zinc and sulfur into a first crucible and a feeding device of a chemical vapor deposition furnace, respectively; heating the first crucible, the second crucible and a deposition chamber, and charging sulfur into the second crucible through the feeding device; introducing an inert carrier gas into the first crucible, and introducing an inert carrier gas and hydrogen into the second crucible, flowing the carrier gas containing zinc vapor and sulfur vapor respectively into the deposition chamber through pipelines to deposit ZnS, and supplying the second crucible with sulfur regularly and quantitatively through the feeding device during the deposition process to maintain a saturated vapor pressure of sulfur in a range of 0.8 to 1.8 KPa. The preparation method of the present invention does not generate H2S; thus it can avoid the formation of hydrogen-zinc complexes by H ions produced from the decomposition of H2S and Zn vapor, which would otherwise affect the transmittance and emissivity of ZnS material.