3D Printed Ceramic NMR Flow Cell for High Pressure

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Solution Overview

Problem

Commercial flow cells for low-field NMR spectrometers, particularly in the chemical and pharmaceutical industries, face safety concerns due to movable seals which are potentially unsafe in terms of explosion protection and require extensive safety and leak detection measures, and lack pressure stability.

Innovation Solution

A cylindrical flow cell with a ceramic base body and opposing capillary receptacles, featuring soldered and welded connections for infallible explosion protection, capable of withstanding high pressures, and incorporating a static mixer for efficient mixing of reactants, fabricated using 3D printing to eliminate dead volumes and ensure laminar flow.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of operation

If movable seals are used in commercial flow cells, then ease of connection is improved, but explosion safety and pressure stability deteriorate

Engineering Contradiction:
Improveease of connectionVSAvoidexplosion safety
Core Design Contradiction:
Ease of operationVSReliability

Solution Approach 1:

The invention removes the movable seal component entirely from the flow cell design. Instead of using movable seals for connection, the flow cell employs fixed, infallible connections made of chemically inert material that are permanently bonded to the process piping through welding or other permanent joining methods, thereby eliminating the safety risks associated with movable seals while maintaining connection functionality.

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The flow cell is divided into distinct functional components: a chemically inert body (made of PTFE, PFA, or PVDF), separate connection elements (infallible connections), and a housing. This segmentation allows each component to be optimized for its specific function - the body for chemical resistance, the connections for safety and pressure stability - while being assembled into a complete system that achieves both ease of connection and explosion safety.

Inventive Principle:
Principle #1Segmentation

2Ease of operation

If movable seals are used in commercial flow cells, then ease of connection is improved, but pressure stability deteriorates

Engineering Contradiction:
Improveease of connectionVSAvoidpressure stability
Core Design Contradiction:
Ease of operationVSStress or pressure

Solution Approach 1:

The invention removes the movable seal component entirely from the flow cell design. Instead of using movable seals for connection, the flow cell employs fixed, infallible connections made of chemically inert material that are permanently bonded to the process piping through welding or other permanent joining methods, thereby eliminating the safety risks associated with movable seals while maintaining connection functionality.

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The flow cell is divided into distinct functional components: a chemically inert body (made of PTFE, PFA, or PVDF), separate connection elements (infallible connections), and a housing. This segmentation allows each component to be optimized for its specific function - the body for chemical resistance, the connections for safety and pressure stability - while being assembled into a complete system that achieves both ease of connection and explosion safety.

Inventive Principle:
Principle #1Segmentation

3Measurement precision

If wall thickness is reduced in central area, then NMR signal quality is improved, but mechanical strength deteriorates

Engineering Contradiction:
Improvesignal qualityVSAvoidmechanical strength
Core Design Contradiction:
Measurement precisionVSStrength

Solution Approach 1:

The flow cell wall thickness is not uniform but varies locally to optimize different functions. In the central measurement area, the wall thickness is minimized (0.5-2 mm) to maximize electromagnetic wave transmission and improve NMR signal quality. In the connection areas and structural supports, the wall thickness is increased to provide the necessary mechanical strength and pressure resistance. This local variation in wall thickness allows the design to simultaneously achieve both optimal signal quality and adequate mechanical strength.

Inventive Principle:
Principle #3Local quality

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

The solution provides a pressure-stable, safe, and efficient flow cell for high-pressure applications, enabling direct measurement of samples without depressurization, reducing noise in NMR spectrometers, and facilitating online monitoring of chemical reactions with improved signal quality and reduced reaction time.

Implementation Method 1

the circular cylindrical base body of the flow cell is manufactured by 3D printing from a ceramic slurry comprising ZrO2 and subsequent sintering

Methodology Applied
Scientific EffectSintering: Sintering

Implementation Method 2

an inner diameter of the receptacles and an outer diameter of the sleeves are adapted to form a solder gap for a solder connection between the ceramic base body and each of the sleeves

Methodology Applied
Scientific EffectSoldering: Soldering

Implementation Method 3

each capillary is connected to the sleeve via a welded connection

Methodology Applied
Scientific EffectWelding: Welding

Data Source

PatentEP3679384B1Pressure-resistant, 3D printed nmr flow cell
Publication Date: 2023.05.31 ALUMINA SYST GMBH
  • EP3679384B1 patent drawingFigure 1A~1C
  • EP3679384B1 patent drawingFigure 2A~2B
  • EP3679384B1 patent drawingFigure 3

AI summary

A flow cell (100, 200) for nuclear magnetic resonance spectrometry (NMR), having: a circular-cylindrical main body (101) comprising a ceramic material; and two receiving portions, each for receiving a capillary (103), lying opposite one another along a central axis of symmetry of the circular-cylindrical main body (101), each capillary (103) being infallibly bonded, in terms of protection in explosive atmospheres, to the circular-cylindrical main body (101).