Cryogenic Sample Bonding via Localized Melting and Freezing

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Solution Overview

Problem

Existing methods for attaching cryogenic samples to manipulators result in contamination and unreliable bonds due to frozen gases and volatile products at cryogenic temperatures, which interfere with the formation of a stable bond between the sample and the manipulator.

Innovation Solution

The method involves heating the part of the sample in contact with the manipulator to cause a phase change, followed by freezing to form a bond, which can be achieved through thermal conductivity or localized heating using a focused beam of light or energetic particles, ensuring a stable attachment without contamination.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If IBID is used to attach the sample to the manipulator at cryogenic temperatures, then the sample can be attached to the manipulator, but the gasses used for IBID are frozen all over the sample resulting in contamination and unreliable bonds

Engineering Contradiction:
Improvebond reliabilityVSAvoidsample contamination
Core Design Contradiction:
ReliabilityVSObject-affected harmful factors

Solution Approach 1:

The patent changes the temperature parameter locally by heating the manipulator tip above the freezing point of the sample material, allowing the sample to be attached in a melted state and then frozen to the manipulator, avoiding the harmful effects of frozen gases that occur at cryogenic temperatures

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent utilizes phase transitions of the sample material by heating it to melt and then freezing it to the manipulator, creating a reliable bond without the contamination problems associated with IBID at cryogenic temperatures

Inventive Principle:
Principle #36Phase transitions

2Reliability

If IBID is used to attach the sample to the manipulator, then the sample can be attached to the manipulator, but the volatile products formed during dissociation do not leave the surface at cryogenic temperatures disturbing the bond formation

Engineering Contradiction:
Improvebond reliabilityVSAvoidvolatile gas interference
Core Design Contradiction:
ReliabilityVSObject-generated harmful factors

Solution Approach 1:

The patent changes the temperature parameter by heating the manipulator tip above the freezing point of the sample material, allowing volatile products to escape as gas rather than remaining frozen on the surface, thus eliminating interference with bond formation

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

Instead of attaching the sample at cryogenic temperatures as in conventional IBID, the patent inverts the approach by heating the manipulator tip to attach the sample in a melted state, then freezing it to create the bond, thereby avoiding the harmful effects of frozen volatile products

Inventive Principle:
Principle #13The other way round (Inversion)

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 allows for reliable and contamination-free attachment of cryogenic samples to manipulators, ensuring a strong bond that prevents sample damage during further analysis, particularly in electron microscopy applications.

Implementation Method 1

the sample is attached to the manipulator by heating at least the part of the sample in contact with the manipulator, thereby causing a phase change of part of the sample material

Methodology Applied
Scientific EffectHeating: Heating

Implementation Method 2

subsequent freezing said part of the sample in contact with the manipulator to the manipulator, thereby forming a bond between the sample and the manipulator

Methodology Applied
Scientific EffectFreezing: Freezing

Implementation Method 3

The cooling down may be the result of the thermal conductivity to a part of the manipulator that is kept at a cryogenic temperature

Methodology Applied
Scientific EffectThermal conductivity: Conduction (thermal)

Data Source

PatentUS7845245B2Method for attaching a sample to a manipulator by melting and then freezing part of said sample
Publication Date: 2010.12.07 FEI CO
  • US7845245B2 patent drawing
  • US7845245B2 patent drawing
  • US7845245B2 patent drawing

AI summary

The invention relates to the extraction of a frozen hydrated sample for TEM (Transmission Electron Microscope) inspection, such as a vitrified biological sample, from a substrate and the attaching of said sample to a manipulator. Such a hydrated sample should be held at a cryogenic temperature to avoid ice formation. By melting or sublimating a part of the sample material outside the area to be studied in the TEM and freezing the material to the manipulator (10), a bond is formed between sample (1) and manipulator. This makes it possible to transport the sample from the substrate to e.g. a TEM grid.In a preferred embodiment a part (2) of the manipulator (10) is held at a cryogenic temperature, and the melting or sublimation is caused by heating the tip (3) of the manipulator by electric heating of the tip and then cooling the tip of the manipulator to a cryogenic temperature, thereby freezing the sample (1) to the manipulator.