Sealed Sample Transfer for Low-Dew-Point Thermal Analysis
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Solution Overview
Problem
Existing thermal analysis methods face challenges in maintaining a controlled atmosphere with low dew points and preventing sample exposure during transfer and analysis, particularly for battery materials, due to issues with seal integrity, pressure differences, and the need for larger gloveboxes, which increase costs and prolong setup times.
Innovation Solution
A thermal analysis system with a sample preparation means that includes a walled space, a pass box, a transfer mechanism, and a sealing mechanism to maintain a controlled atmosphere, allowing sample transfer and analysis while preserving the sample's integrity and enabling low dew point conditions.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Ease of operation
If the sample vessel is sealed using indium or gallium within a glovebox and then extracted for analysis, then the sample can be transferred to the heating analysis device, but the seal may break during heating analysis due to melting of the sealing material, and atmospheric exposure may occur during transfer
Solution Approach 1:
A transfer chamber is introduced as an intermediary space between the glovebox and the heating analysis device. The transfer chamber allows the sealed sample vessel to be transferred without direct exposure to the atmosphere, maintaining seal integrity while enabling sample transfer operations.
Solution Approach 2:
The sample vessel is nested within the transfer chamber, which itself is nested within the heating analysis device. This nested structure allows the sample vessel to be transferred through the transfer chamber without breaking the seal, while the transfer chamber remains sealed to prevent atmospheric exposure.
2Temperature
If the heating analysis device is installed in a dedicated glovebox, then the dew point can be controlled, but the heat from the heating furnace elevates the dew point within the glovebox, making it difficult to sustain dew point below -80°C
Solution Approach 1:
The system is segmented into separate functional zones: the glovebox for sample preparation, the transfer chamber for sealed transfer, and the heating analysis device for thermal analysis. This segmentation allows the heating furnace to operate independently without elevating the dew point in the glovebox, as the transfer chamber acts as a thermal and atmospheric barrier.
Solution Approach 2:
The heating furnace is extracted from the glovebox environment and placed in a separate heating analysis device. This extraction removes the source of heat that was elevating the dew point in the glovebox, allowing the glovebox to maintain dew point below -80°C while the heating device performs thermal analysis at elevated temperatures.
3Productivity
If the sample vessel is extracted from the glovebox for analysis, then the analysis can be conducted in a heating analysis device, but there is possibility of lids blowing off due to pressure difference when connecting vacuum line to sealed sample vessel
Solution Approach 1:
The transfer chamber serves as an intermediary that equalizes pressure between the glovebox and the heating analysis device before sample vessel opening. This pressure equalization prevents lids from blowing off when vacuum lines are connected, while still allowing efficient analysis to proceed.
4Ease of manufacture
If indium or gallium is used for sealing the sample vessel, then the sample vessel can be sealed within a glovebox, but these materials react with halogens such as chlorine or bromine, affecting thermal analysis results of battery materials containing halogens
Solution Approach 1:
The sample vessel with its seal is designed as a disposable component that is sealed in the glovebox, transferred sealed to the heating device, and then opened only after the analysis is complete. This eliminates the need for the sealing material to withstand chemical reactions during analysis, as the seal is only required during transfer, not during the heating analysis phase.
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
Enables easy and efficient thermal analysis with reduced atmospheric exposure, maintaining low dew points and ensuring accurate results by preventing sample contamination, thus addressing the limitations of existing methods.
Implementation Method 1
a heating means heating said heating tube and surrounding said heating tube on the outer side thereof
Implementation Method 2
said thermal analysis means comprising: said heating tube housing the sample holder from said sample preparation means, and a pump means drawing a vacuum within said heating tube
Implementation Method 3
a gas supply means in order to sustain the dew point at a specific temperature while the pressure in said heating tube is returned to atmospheric pressure
Data Source
AI summary
To provide a thermal analysis system and a thermal analysis method capable of easily performing thermal analysis while suppressing atmospheric exposure associated with sample movement. A thermal analysis system according to the present disclosure includes a sample preparing unit and a thermal analyzing unit. The sample preparing unit includes a wall portion forming an internal space, a gate portion capable of opening and closing an opening of the wall portion, and a sample holding member including a sample holder and temperature sensors. The thermal analyzer includes a moving mechanism for moving a sample holder into a thermal analysis part, a sealing mechanism for sealing the sample holder from an internal space of a sample preparation part, and a coupling mechanism for connecting a heating tube of the thermal analysis part to a gate part in a state of sealing the heating tube from the outside. A heating tube for housing a sample holder from a sample preparing part and a heating part for heating the heating tube are provided.