LIBS System for Molten Metal Analysis

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Solution Overview

Problem

Current methods for chemical analysis of liquid metals, such as spark atomic emission spectroscopy on solid samples, are prone to errors due to temperature variations, cooling rates, and contamination, and lack real-time and in-situ monitoring capabilities, especially in the challenging environment of primary aluminum smelters.

Innovation Solution

A LIBS system that monitors the temperature of molten metal samples during cooling and initiates measurements when pre-selected criteria are met, using passive cooling to maintain consistent sample temperatures and avoid active heating, allowing for accurate and rapid chemical analysis in a portable, battery-powered configuration.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If spark atomic emission spectroscopy is used on solid samples, then chemical composition analysis can be performed, but measurement precision deteriorates due to temperature variations and cooling rates

Engineering Contradiction:
Improvechemical composition analysis accuracyVSAvoidsample temperature consistency
Core Design Contradiction:
Measurement precisionVSStability of the object's composition

Solution Approach 1:

The invention changes the physical state parameter of the sample from solid to liquid, and controls the temperature parameter to be above the melting point but below a specified threshold. This parameter change allows LIBS measurements to be performed on molten metal with consistent temperature, eliminating the temperature variation and cooling rate issues that affect spark OES on solid samples.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention performs preliminary heating of the crucible to a temperature above the melting point of the metal sample before introducing the sample. This preliminary action ensures the sample remains in a liquid state during measurement, maintaining temperature consistency and preventing the composition changes that occur during solidification.

Inventive Principle:
Principle #10Preliminary action

2Measurement precision

If active heating is used to maintain sample temperature, then measurement precision improves, but device complexity and energy consumption increase

Engineering Contradiction:
Improvetemperature control accuracyVSAvoidheating system complexity
Core Design Contradiction:
Measurement precisionVSDevice complexity

Solution Approach 1:

The invention uses the exothermic reaction between the molten metal sample and the preheated crucible to maintain the sample temperature. The crucible itself serves as the heat source, eliminating the need for external active heating systems. The chemical energy stored in the crucible-sample interaction automatically maintains the required temperature range.

Inventive Principle:
Principle #25Self-service

Solution Approach 2:

The invention converts the potentially harmful rapid cooling of molten metal into a beneficial self-heating mechanism. The exothermic reaction between the metal and crucible generates heat that counteracts cooling, transforming the cooling problem into a self-regulating temperature maintenance system.

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

3Measurement precision

If LIBS measurement is performed on molten metal samples, then measurement precision improves, but reliability deteriorates due to temperature control difficulties

Engineering Contradiction:
Improvechemical analysis accuracyVSAvoidmeasurement consistency
Core Design Contradiction:
Measurement precisionVSReliability

Solution Approach 1:

The invention implements a feedback control system that monitors the temperature of the crucible and molten metal sample, and adjusts the measurement timing and crucible preheating level accordingly. The system waits for the sample temperature to fall within the specified range (above melting point but below threshold) before initiating LIBS measurement, ensuring consistent measurement conditions.

Inventive Principle:
Principle #23Feedback

Solution Approach 2:

The invention introduces dynamic temperature monitoring and adaptive measurement timing. Instead of using a fixed measurement protocol, the system dynamically adjusts based on the actual temperature state of the sample, initiating measurements only when temperature criteria are met, thereby ensuring reliability across varying initial conditions.

Inventive Principle:
Principle #15Dynamics

4Device complexity

If sample cooling is allowed to occur naturally, then device complexity reduces, but measurement precision deteriorates due to temperature variations

Engineering Contradiction:
Improvecooling system simplicityVSAvoidtemperature stability
Core Design Contradiction:
Device complexityVSMeasurement precision

Solution Approach 1:

The invention performs preliminary preheating of the crucible to a controlled temperature range before introducing the molten metal sample. This preliminary action establishes a thermal environment that slows the cooling rate of the sample, maintaining it in a liquid state at a suitable temperature for LIBS measurement without requiring active cooling systems.

Inventive Principle:
Principle #10Preliminary 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 approach reduces measurement errors by ensuring consistent sample temperatures and facilitates rapid, accurate chemical analysis of molten metals, enabling immediate correlation with reduction cells and efficient sampling from multiple sources.

Implementation Method 1

laser-induced breakdown spectroscopy (LIBS) on a molten sample

Methodology Applied
Scientific EffectLaser-induced breakdown spectroscopy: Laser Ablation

Implementation Method 2

spark atomic emission spectroscopy (also known as spark optical emission spectroscopy or spark-OES)

Methodology Applied
Scientific EffectAtomic emission spectroscopy: Luminescence

Implementation Method 3

monitoring a temperature of the molten sample during cooling of the molten sample

Methodology Applied
Scientific EffectTemperature sensing: Thermocouple

Data Source

PatentUS20240426759A1System and method for performing laser-induced breakdown spectroscopy measurements on molten metal samples
Publication Date: 2024.12.26 DTE EHF
  • US20240426759A1 patent drawing
  • US20240426759A1 patent drawing
  • US20240426759A1 patent drawing

AI summary

LIBS measurement systems are disclosed that are configured to monitor the temperature of a molten metal sample during cooling of the molten metal sample in a crucible, and to initiate a LIBS measurement after the temperature of the molten metal sample satisfies measurement temperature criteria. The system may also monitor the temperature of an empty crucible to assist in ensuring that the crucible temperature is (i) sufficiently high to ensure that after the molten metal sample is delivered to the crucible and cools to satisfy the measurement temperature criteria, a sufficiently low cooling rate of the molten metal sample occurs during the LIBS measurement, and (ii) optionally sufficiently low to avoid an unnecessarily long cooling time of the molten metal sample prior to satisfying the measurement temperature criteria and initiation of the LIBS measurement. The LIBS measurement system may be mobile and battery-powered, and may include an integrated calibration station.