TEM Vacuum Transfer Assembly for Ice-Free Cryosample Handling

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Solution Overview

Problem

Current cryotransfer systems in microscopy are expensive, user-unfriendly, and prone to specimen degradation due to ice formation, with limited capability for in-situ experiments and poor vacuum maintenance, especially when handling air-sensitive samples and large samples.

Innovation Solution

A redesigned vacuum transfer assembly with a sample holder stage and vacuum housing that allows for controlled, vacuum-sealed transfer of samples, maintaining ultra-high vacuum conditions and enabling in-situ experiments at low temperatures, featuring a wider sample rod for better cooling and additional stimuli application, and an integrated α-tilt system within the holder.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If a complete cryotransfer system with integrated TEM and permanently fitted sample holder is used, then cryotransfer capability is achieved, but the system becomes expensive and lacks versatility for in-situ experiments

Engineering Contradiction:
Improvecryotransfer capabilityVSAvoidin-situ experiment capability
Core Design Contradiction:
ReliabilityVSAdaptability or versatility

Solution Approach 1:

The system is divided into separate functional modules: a removable sample holder that can be transferred between different microscopes, a vacuum housing that maintains ultra-high vacuum, and a coupling unit that enables versatile connections. This segmentation allows the same sample holder to be used for cryotransfer in TEM and for in-situ experiments in other microscopes, achieving both reliability and versatility without requiring a permanently integrated expensive system.

Inventive Principle:
Principle #1Segmentation

2Weight of moving object

If a small valve is used in the Dewar to keep holder weight acceptable, then weight is reduced, but vacuum pumping speed becomes limited

Engineering Contradiction:
Improveholder weightVSAvoidvacuum pumping speed
Core Design Contradiction:
Weight of moving objectVSProductivity

Solution Approach 1:

Instead of increasing valve size in the traditional vertical direction which would increase weight, the system adds a second valve at a different location (another dimension in the holder structure). This allows dual-path vacuum pumping capability without significantly increasing the weight of individual components, thereby achieving high pumping speed while maintaining acceptable holder weight.

Inventive Principle:
Principle #17Another dimension (Dimensionality change)

3Object-affected harmful factors

If a sliding mechanism with airtight seal is used to push sample into sealed space, then sample protection is achieved, but the sealed area becomes small and cannot accommodate sensors

Engineering Contradiction:
Improvesample protection from airVSAvoidsealed area
Core Design Contradiction:
Object-affected harmful factorsVSArea of stationary object

Solution Approach 1:

The sealed space is segmented into multiple zones with multiple airtight seals at different locations. This creates several smaller sealed compartments rather than one large sealed area, allowing sensors and other components to be placed in specific zones while maintaining protection for the sample in other zones. The coupling unit further segments the connection interface to accommodate various sensor types.

Inventive Principle:
Principle #1Segmentation

4Ease of operation

If the sample holder is transferred through air to allow insertion into TEM, then accessibility is improved, but vacuum conditions deteriorate and ice formation occurs on sample

Engineering Contradiction:
Improvesample holder insertionVSAvoidvacuum condition and sample integrity
Core Design Contradiction:
Ease of operationVSReliability

Solution Approach 1:

The sample holder is pre-cooled to cryogenic temperatures before transfer, and the vacuum housing is pre-evacuated to ultra-high vacuum conditions. During transfer through air, the sample remains protected inside the pre-cooled holder with minimal exposure. The rapid insertion into the pre-prepared vacuum environment minimizes ice formation and maintains sample integrity, achieving both ease of operation and reliability.

Inventive Principle:
Principle #10Preliminary action

5Temperature

If a wider sample rod is used for better cooling and additional stimuli application, then cooling capability and experimental capability are improved, but the holder diameter increases affecting vacuum maintenance

Engineering Contradiction:
Improvecooling capabilityVSAvoidvacuum maintenance
Core Design Contradiction:
TemperatureVSReliability

Solution Approach 1:

The holder structure is segmented into the sample rod and the outer housing. The sample rod can be optimized for cooling capability with appropriate diameter, while the outer housing provides the vacuum seal. This segmentation allows the sample rod to be wider for better cooling and stimuli application without proportionally increasing the overall holder diameter, thereby maintaining better vacuum conditions.

Inventive Principle:
Principle #1Segmentation

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

Facilitates easy cryotransfer of cryosamples without ice formation, maintains ultra-high vacuum in the TEM, and allows for longer experimental durations with improved mechanical stability and resolution, enabling larger sample handling and additional experimental capabilities.

Implementation Method 1

maintaining ultra-high vacuum conditions

Methodology Applied
Scientific EffectVacuum: Vacuum

Implementation Method 2

a cooling rod inside the holder, which transports 'coldness' to the tip of the rod

Methodology Applied
Scientific EffectThermal conduction: Conduction (thermal)

Data Source

PatentUS11994663B2Vacuum transfer assembly
Publication Date: 2024.05.28 HENNYZ BV
  • US11994663B2 patent drawing
  • US11994663B2 patent drawing
  • US11994663B2 patent drawing

AI summary

The present invention is in the field of a vacuum transfer assembly, such as for cryotransfer, and specifically a TEM vacuum transfer assembly, which can be used in microscopy, a sample holder, a vacuum housing, a sample holder stage and a sample holder coupling unit for use in the assembly, and a microscope comprising said assembly as well as a method of vacuum transfer into a microscope.