Cryogenic Milling Vessel Segmentation for Reactive Samples

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Solution Overview

Problem

Existing laboratory mills for reactive samples face inefficiencies in milling at low temperatures under inert atmospheres, often requiring expensive equipment for continuous cooling and inconvenient handling of cooling mediums, which increases costs and exposure to atmospheric air.

Innovation Solution

A cryogenic milling vessel with a separable cylindrical milling compartment surrounded by a cryostatic unit, allowing partial filling with cooling medium and adjustable dimensions to fit standard laboratory mills, ensuring efficient and safe milling under inert conditions without additional equipment.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Temperature

If continuous cooling channels are used in the milling vessel, then low temperature milling efficiency is improved, but device cost and complexity increase

Engineering Contradiction:

Improvemilling temperatureVSAvoidcooling system complexity

Core Design Contradiction:

TemperatureVSDevice complexity

Solution Approach 1:

The milling vessel is divided into two functional parts: an inner milling compartment for sample processing and an outer cryostatic unit for cooling. This segmentation allows the cooling function to be provided by a simple external jacket filled with cooling medium, eliminating the need for complex internal cooling channels while maintaining effective low-temperature milling

Inventive Principle:

Principle #1Segmentation

Solution Approach 2:

A cooling medium (such as liquid nitrogen) is introduced as an intermediary substance between the milling compartment and the external environment. The cooling medium absorbs heat from the milling process through the cooling jacket, enabling continuous low-temperature milling without direct mechanical cooling components inside the vessel

Inventive Principle:

Principle #24Intermediary (Mediator)

2Reliability

If the milling vessel is immersed in liquid nitrogen for cooling, then inert atmosphere is maintained, but operational convenience deteriorates

Engineering Contradiction:

Improveinert atmosphere maintenanceVSAvoidcooling operation convenience

Core Design Contradiction:

ReliabilityVSEase of operation

Solution Approach 1:

The milling compartment is pre-cooled and sealed under inert atmosphere before the milling process begins. The cryostatic unit with cooling medium is prepared in advance, allowing the system to maintain inert conditions throughout operation without requiring repeated opening and immersion in liquid nitrogen

Inventive Principle:

Principle #10Preliminary action

Solution Approach 2:

The sealed milling compartment maintains its own inert atmosphere independently once prepared. The cooling system operates autonomously through the cooling jacket without requiring manual intervention to immerse the vessel in liquid nitrogen during operation, making the system self-sufficient for maintaining both temperature and atmosphere

Inventive Principle:

Principle #25Self-service

3Adaptability or versatility

If standard laboratory mill vessels are used, then equipment compatibility is maintained, but cryogenic cooling capability is lost

Engineering Contradiction:

Improveequipment compatibilityVSAvoidcooling capability

Core Design Contradiction:

Adaptability or versatilityVSTemperature

Solution Approach 1:

The invention merges two separate functions into one integrated system: the inner milling compartment maintains compatibility with standard laboratory mill vessels for equipment adaptability, while the outer cryostatic unit adds cryogenic cooling capability. This combination allows the system to work with existing mill equipment while providing enhanced low-temperature functionality

Inventive Principle:

Principle #5Merging (Combining)

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, fast, and cost-effective milling of reactive samples at low temperatures while maintaining an inert atmosphere, reducing exposure to atmospheric air and moisture, and allowing the use of existing equipment by adjusting the vessel's dimensions to fit within a glovebox.

Implementation Method 1

the milling compartment being surrounded by a cooling space being adapted to be filled with a cooling medium

Methodology Applied

Scientific EffectThermal conduction: Conduction (thermal)

Implementation Method 2

allowing at least partial filling with a cooling medium

Methodology Applied

Scientific EffectPhase change: Phase Change

Data Source

PatentEP3310486B1Cryogenic disc or ball milling vessel to a laboratory mill for milling reactive samples

Publication Date: 2022.05.25 UNIWERSYTET WARSZAWSKI

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Figure 2~3
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AI summary

The invention refers a cryogenic disc or ball milling vessel to a laboratory mill for milling reactive samples, comprising a cylindrical milling compartment, in which there are located grinding members like disc, rings or balls, closed at the top with a tight lid. The cryogenic milling vessel according to the invention comprises a cryostatic unit forming a cooling coating surrounding the milling compartment (1), in which milling compartment there are located grinding members in form of disc, rings or balls, the cryostatic unit (8) being at least partially filled with a cooling medium, preferably liquid nitrogen. The Cryogenic milling vessel according to the present invention allows for easy, fast, cheap and safe milling, comminuting or homogenizing a sample at low temperature ensuring no contact of the sample with atmospheric air and moisture.