In Situ CVD Coating for Fluidized Bed Reactor Integrity

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Solution Overview

Problem

Existing methods for coating thermally and chemically stressed components in fluidized bed reactors used for producing high-purity polycrystalline silicon granules are inefficient, often requiring bulk material application and shutdown for coating, which complicates the process and may lead to contamination or deformation.

Innovation Solution

An in-situ CVD method is used to coat reactor surfaces with Si and/or Si3N4 using a reactive gas mixture, allowing for coating during startup or restart, even when the reactor is bulk material-free, and enabling continuous operation without shutting down the reactor for repairs.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If a quartz reactor tube is used to ensure high purity and chemical stability, then product contamination is reduced, but the tube deforms at temperatures above 1150°C

Engineering Contradiction:
Improvechemical stabilityVSAvoidtube deformation
Core Design Contradiction:
ReliabilityVSShape

Solution Approach 1:

The patent applies a coating layer of silicon carbide (SiC) and/or silicon nitride (Si3N4) onto the quartz reactor tube surface. This composite structure combines the chemical stability and purity of quartz with the high-temperature mechanical strength of SiC/Si3N4, preventing tube deformation at temperatures above 1150°C while maintaining the underlying quartz tube's chemical resistance and product purity.

Inventive Principle:
Principle #40Composite materials

Solution Approach 2:

The patent changes the physical and chemical parameters of the reactor tube surface by depositing a coating layer with different thermal and mechanical properties. The SiC/Si3N4 coating has higher melting point and mechanical strength than quartz, allowing the system to operate at temperatures above 1150°C without deformation while the quartz substrate maintains chemical stability.

Inventive Principle:
Principle #35Parameter changes

2Ease of manufacture

If liquid polymer precursors are applied to coat reactor surfaces, then coating can be applied at room temperature, but the process requires bulk material application and shutdown

Engineering Contradiction:
Improvecoating applicationVSAvoidreactor shutdown time
Core Design Contradiction:
Ease of manufactureVSProductivity

Solution Approach 1:

The patent replaces the mechanical liquid polymer precursor application method with a gas-phase chemical vapor deposition (CVD) process. Instead of applying liquid coatings that require drying and curing, reactive gas mixtures are introduced into the reactor and decompose on the heated surface to form the coating, eliminating the need for bulk material handling and reactor shutdown.

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

Solution Approach 2:

The in-situ CVD coating process allows the reactor to remain in operation during coating application. The reactive gas mixture is introduced, the surface is heated to appropriate temperature, and the coating forms continuously without interrupting the overall production process, thereby maintaining productivity while achieving the coating benefit.

Inventive Principle:
Principle #20Continuity of useful action

3Productivity

If the reactor is operated continuously without shutdown for coating, then productivity is maintained, but existing coating methods cannot be applied

Engineering Contradiction:
Improvecontinuous operationVSAvoidcoating process feasibility
Core Design Contradiction:
ProductivityVSEase of manufacture

Solution Approach 1:

The patent replaces mechanical coating application methods (which require reactor shutdown, bulk material handling, and sequential processing) with a gas-phase CVD process. The reactive gas mixture can be introduced into the operating reactor, decomposed on the heated surface, and converted to coating material in-situ, enabling continuous operation while achieving effective coating.

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

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 provides a stable and efficient coating that maintains reactor integrity and product purity, allowing for continuous operation and repeated coating without shutdown, while improving the mechanical and chemical stability of reactor components.

Implementation Method 1

the Surfaces of the reactor which have a temperature of more than 600° C. and which come into contact with the reactive gas mixture are provided with an in-situ coating of Si and/or Si 3 N 4 using a CVD process

Methodology Applied
Scientific EffectChemical Vapour Deposition: Chemical Vapour Deposition

Implementation Method 2

By adding a reaction gas containing silicon, a pyrolysis reaction takes place on the hot particle surface. In the process, elementary silicon is deposited on the silicon particles

Methodology Applied
Scientific EffectPyrolysis: Pyrolysis

Data Source

PatentEP3420116B1Method for depositing an in situ coating onto thermally and chemically loaded components of a fluidized bed reactor for producing high-purity polysilicon
Publication Date: 2019.09.04 WACKER CHEMIE AG

AI summary

The invention relates to a method for coating thermally and chemically loaded components of a fluidized bed reactor for producing high-purity polysilicon granules, wherein the fluidized bed reactor, which is free or largely free of bulk material, is flushed with a reactive gas mixture at an average tubular wall temperature of 600°C to 1400°C over a time period of 1 h to 8 days and at a pressure of 1 to 15 bar absolute and the surfaces of the reactor that have a temperature of more than 600°C are thereby provided with an in situ coating of Si and/or SiC and/or Si3N4 by means of a CVD method.