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Method For Monitoring A Process For Powder-Bed Based Additive Manufacturing Of A Component And Such A System

a technology of powder-bed based additive manufacturing and process monitoring, which is applied in the direction of electrolytic organic production, multiple component coatings, electrochemical coatings, etc., can solve the problems of inability to continuously produce renewable energy, inability to develop an electrochemical system with which cosub>2 /sub>could be reduced with long-term stability

Inactive Publication Date: 2018-08-16
SIEMENS ENERGY GLOBAL GMBH & CO KG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

The patent is about the need for cathodes that can effectively convert carbon dioxide to hydrocarbons. The invention aims to provide a new catalyst concept that does not require copper deposition and can be processed to create an electrode. Additionally, the patent aims to develop selective electro-catalysts that are stable over a long period of time and can be embedded into gas diffusion electrodes that can connect to electrical contacts.

Problems solved by technology

This process, which is divided up into many component steps over time and spatially at the molecular level, is reproducible on the industrial scale only with difficulty.
However, overproduction of renewable energies is not continuously available, but at present only at periods of strong insolation and / or wind.
In spite of many efforts, it has not been possible to date to develop an electrochemical system with which CO2 could be reduced with long-term stability and in an energetically favorable manner to competitive energy sources with sufficiently high current density and acceptable yield.
However, the prior art in this regard is not yet very developed.
However, in the case of electrodes produced in this way, the selectivity of the electrode can decrease with time, which can lead to an increase in hydrogen production.
In this context, said wet method 1. can have the disadvantages mentioned hereinafter, aside from the fact that examples of gas diffusion electrodes known from the literature contain the catalyst only as an additive and consist mainly of bound conductive charcoal (for high conversions the catalyst loading should be high):
The suspensions or pastes that are usually applied by spraying or bar coating generally have long drying times, which means that continuous production with relatively large electrode areas (of industrial relevance) is not economically possible.
Excessively rapid drying leads to cracking, called “mud cracking”, within the layers applied, which makes the electrode unusable.
This process is highly solvent- or boiling point-dependent and can lead to a high reject rate of the electrodes produced, since the evaporation cannot be assured in a homogeneous manner over the entire area.
A further central disadvantage is the use of surface-active substances (surfactants) or thickeners, plasticizers, which are used for stabilization of the particle suspensions since they cannot be removed without residue by the corresponding drying phases or the thermal crosslinking process.
The embedding process 2., wherein Nafion® (perfluorosulfonic acid, PFSA) is used as binder rather than PTFE, likewise has corresponding disadvantages, since a wet-chemical method using appropriate surfactants is being employed here too.
Nafion® itself is a hydrophilic ionomer having highly acidic R—HSO3 groups which can lead to unwanted acid corrosion or partial dissolution of the metal in the case of some catalysts.
The purely hydrophilic properties of Nafion® can likewise be disadvantageous, since Nafion®, owing to its hydrophilic properties, is unsuitable for formation of hydrophobic channels that are advantageous for gas transport within a gas diffusion electrode.
However, multilayer coating processes are not very attractive for economic reasons.
Nafion®-based coating processes can additionally lead to unwanted formation of hydrogen.
Owing to the low mechanical stability, the latter method is less suitable than the above-specified one-step process.
However, reproduction experiments which are cited hereinafter as comparative examples demonstrate that the static pressing method described does not lead to stable electrodes.
The added Vulkan XC 72 was likewise found to have an adverse effect, and so it was likewise not possible to obtain any hydrocarbons.
However, in-house preliminary tests have shown that this is not appropriate to the aim.

Method used

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  • Method For Monitoring A Process For Powder-Bed Based Additive Manufacturing Of A Component And Such A System
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Examples

Experimental program
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Effect test

examples

[0177]All experiments and also the comparative examples and examples were conducted at a room temperature of about 20° C.-25° C., unless stated otherwise.

[0178]The pressure in the comparative examples and examples was likewise not varied, but left at room pressure (about 1.013 bar).

[0179]The further detailed data are reported for their respective comparative examples or examples.

reference example 1

Production of a Mixed Metal Oxide Catalyst by Coprecipitation:

[0207]Illustrative Method for Cu / Al2O3

[0208]An appropriate hydrotalcite precursor of the composition [Cu0.6Al0.4(OH)2](CO3)0.4.mH2O (unknown water content for the freshly precipitated hydrotalcite) is prepared by a coprecipitation. Simultaneously added are a 0.41 M metal salt solution (A) composed of Cu(NO3)2.3H2O (0.246 mol) and Al(NO3)3.9H2O (0.164 M) and a hydroxide / carbonate solution (B) composed of 0.3 M NaOH (12 g), 0.045 M (NH4)2CO3 (4.32 g), such that the pH is between pH 8 and 8.5.

[0209]The addition rate of the metal salt solution was chosen as 120 mL / h. Oswalt ripening was effected for 30 min. Thereafter, the solids were filtered off and washed to neutrality. Thereafter, the precursor was dried at 80° C. for 12 h, pulverized and calcined. The calcination step is effected in a tubular furnace having a temperature ramp of β=2 K / min up to 300° C. with isothermal conditions for 4 h in an argon / oxygen mixture: 20% b...

example 1

Production of a 2-Layer Electrode

[0216]Copper powder with a particle diameter of 100-200 μm and PTFE TF 1750 Dyneon were mixed in an IKA A10 knife mill for 6 min (grinding for 15 sec, wait for 30 sec). The powder layer was then sieved off and graded by means of a template of thickness 0.5 mm to form a base layer. This was followed by extrusion with a 2-roll calender with a roll separation of 0.5 mm. Thereafter, a catalyst layer was applied by sieving application, for example in each case analogously to comparative examples 6 to 8, through a 0.2 mm frame, and extrusion was again effected with a 2-roll calender with a roll separation of 0.35 mm. The result was a highly porous base layer with a porosity of >70%, good mechanical stability and very good conductivity at 5 mohm / cm. It was possible to use catalysts with a copper content of 40% by weight.

[0217]Preferably, the catalysts had a purity above the commercially available materials or quality standards, as in the example as well. Th...

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Abstract

A gas diffusion electrode and electrolysis cells containing gas diffusion electrodes are provided. The gas diffusion electrodes include a copper-containing carrier, and first and second layers. The first layer comprising at least copper and at least one binder having hydrophilic and hydrophobic pores. The second layer comprising copper and at least one binder. The second layer present atop the carrier and the first layer atop the second layer, wherein the content of binder in the first layer is less than the binder in the second layer.

Description

CROSS-REFERENCE TO RELATED APPLICATIONS[0001]This application is a U.S. National Stage Application of International Application No. PCT / EP2016 / 067165 filed Jul. 19, 2016, which designates the United States of America, and claims priority to DE Application No. 10 2015 215 309.6 filed Aug. 11, 2015, the contents of which are hereby incorporated by reference in their entirety.FIELD OF INVENTION[0002]The present invention relates to a gas diffusion electrode preferably comprising a copper-containing carrier and a first layer comprising at least copper and at least one binder and a second layer. The (first) layer comprises hydrophilic and hydrophobic pores and / or channels. The second layer comprising copper and at least one binder, wherein the second layer is present atop the carrier and the first layer atop the second layer, wherein the content of binder in the first layer is less than in the second layer. The present invention also relates to a process for producing a gas diffusion ele...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): C25B11/04C25B11/03C25B3/04C25B3/25
CPCC25B11/0489C25B11/0405C25B11/035C25B11/0415C25B3/04C25B3/25C25B11/057C25B11/095C25B11/031C25B11/051
Inventor KRAUSE, RALFMALTENBERGER, ANNARELLER, CHRISTIANSCHMID, BERNHARDSCHMID, GUNTER
Owner SIEMENS ENERGY GLOBAL GMBH & CO KG