DE102012217588A1 - Manufacture of thermoelectric layer for thermal leg of thermoelectric generator, involves subjecting semiconductor material produced using aqueous solution comprising soluble polymer and soluble organic precursor, to sol-gel process - Google Patents

Manufacture of thermoelectric layer for thermal leg of thermoelectric generator, involves subjecting semiconductor material produced using aqueous solution comprising soluble polymer and soluble organic precursor, to sol-gel process Download PDF

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DE102012217588A1
DE102012217588A1 DE201210217588 DE102012217588A DE102012217588A1 DE 102012217588 A1 DE102012217588 A1 DE 102012217588A1 DE 201210217588 DE201210217588 DE 201210217588 DE 102012217588 A DE102012217588 A DE 102012217588A DE 102012217588 A1 DE102012217588 A1 DE 102012217588A1
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thermoelectric
sol
aqueous solution
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gel process
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Dr. Eder Florian
Bastian Plochmann
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Siemens AG
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
    • C04B35/457—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates based on tin oxides or stannates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/624—Sol-gel processing
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
    • H10N10/01—Manufacture or treatment
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
    • H10N10/80—Constructional details
    • H10N10/85—Thermoelectric active materials
    • H10N10/851—Thermoelectric active materials comprising inorganic compositions
    • H10N10/853—Thermoelectric active materials comprising inorganic compositions comprising arsenic, antimony or bismuth
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/90—Electrical properties
    • C04B2111/94—Electrically conducting materials
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3294—Antimony oxides, antimonates, antimonites or oxide forming salts thereof, indium antimonate

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

Manufacture of thermoelectric layer involves subjecting semiconductor material produced using aqueous solution comprising soluble polymer and soluble organic precursor, to sol-gel process and forming gel aggregate, then drying and heat-treating.

Description

Die Erfindung betrifft ein Verfahren zum Herstellen einer thermoelektrischen Schicht nach dem Oberbegriff von Patentanspruch 1. The invention relates to a method for producing a thermoelectric layer according to the preamble of patent claim 1.

Für Thermoelemente, thermoelektrische Generatoren oder dgl. müssen n- und p-halbleitende Schichten als Thermoschenkel angeordnet und in Reihe geschaltet werden. Wesentliche Materialparameter für die Thermoschenkel sind dabei die elektrische Leitfähigkeit σ, die thermische Leitfähigkeit λ und der Seebeckkoeffizient S. For thermocouples, thermoelectric generators or the like. N- and p-type semiconductive layers must be arranged as a thermo leg and connected in series. Essential material parameters for the thermo legs are the electrical conductivity σ, the thermal conductivity λ and the Seebeckkoeffizient S.

Die Gütezahl eines thermoelektrischen Generators ist definiert als ZT = S2σλ–1. Zur Optimierung der Thermoschenkel muss daher der Seebeckkoeffizient und die elektrische Leitfähigkeit maximiert und die thermische Leitfähigkeit minimiert werden. The figure of merit of a thermoelectric generator is defined as ZT = S 2 σλ -1 . To optimize the thermo leg, therefore, the Seebeckkoeffizient and the electrical conductivity must be maximized and the thermal conductivity to be minimized.

Nachteiligerweise sind elektrisch gut leitende Materialien in der Regel auch gute Wärmeleiter. Durch die hohe Wärmeleitfähigkeit wird Wärme schnell von der Heißseite zur Kaltseite eines thermoelektrischen Generators übertragen, so dass die Gesamttemperaturdifferenz über den thermoelektrischen Generator verringert wird und damit der Wirkungsgrad sinkt. Disadvantageously, electrically good conductive materials are usually also good heat conductors. Due to the high thermal conductivity heat is transferred quickly from the hot side to the cold side of a thermoelectric generator, so that the total temperature difference across the thermoelectric generator is reduced and thus the efficiency decreases.

Ein weitverbreiteter Ansatz ist die Verwendung von Materialien, bei denen an Partikel- und Korngrenzen Phononen, also Gitterschwingungen, durch die im Festkörper Wärme übertragen wird, gestreut werden, während Ladungsträger ungehindert fließen können. Zur Senkung der thermischen Leitfähigkeit müssen also Störstellen in Form von Korngrenzen, Partikelgrenzen oder Poren geschaffen werden, um die Phononenstreuung zu maximieren. A widespread approach is the use of materials in which at particle and grain boundaries are scattered phonons, ie lattice vibrations, through which heat is transferred in the solid state, while carriers can flow freely. To reduce the thermal conductivity so impurities in the form of grain boundaries, particle boundaries or pores must be created to maximize the phonon scattering.

Hierzu ist es bekannt, poröse thermoelektrische Schichten aus partikulären Ausgangsmaterialien zu fertigen, die durch Einbettung in eine stabile Matrix, z.B. durch Polymerverguss, oder durch Sintern zur endgültigen Schicht verarbeitet werden. Bei Einbettung in eine Matrix muss das Matrixmaterial elektrisch isolierend sein, so dass die thermoelektrischen Partikel nicht kurzgeschlossen werden. For this purpose, it is known to fabricate porous thermoelectric layers of particulate starting materials which are embedded by embedding in a stable matrix, e.g. by polymer casting, or by sintering to the final layer. When embedded in a matrix, the matrix material must be electrically insulating, so that the thermoelectric particles are not short-circuited.

Ein weiteres bekanntes Verfahren ist das elektrochemische Ätzen, durch welches nicht-poröse thermoelektrische Schichten mit Poren versehen werden können. Another known method is the electrochemical etching, through which non-porous thermoelectric layers can be provided with pores.

Alle bekannten Ansätze leiden jedoch unter dem Problem, dass keine mikroskopisch homogenen Schichten erzeugt werden können. Hieraus resultieren neben dem Herstellungsaufwand für die Strukturierung der Schichten noch Probleme wie schlechte mechanische Eigenschaften, insbesondere eine schlechte Biegebelastbarkeit, und verschlechterte elektrische Eigenschaften durch nicht ausreichende elektrische Kontaktierung der thermoelektrischen Partikel untereinander. However, all known approaches suffer from the problem that no microscopically homogeneous layers can be produced. This results in addition to the production costs for the structuring of the layers still problems such as poor mechanical properties, in particular a poor flexural strength, and deteriorated electrical properties due to insufficient electrical contact of the thermoelectric particles with each other.

Es ist daher Aufgabe der vorliegenden Erfindung, ein Verfahren nach dem Oberbegriff von Patentanspruch 1 bereitzustellen, mit dem einfach, kostengünstig und prozesssicher thermoelektrische Schichten mit guten elektrischen, thermischen und mechanischen Eigenschaften erhalten werden können. It is therefore an object of the present invention to provide a method according to the preamble of claim 1, with the simple, inexpensive and reliable thermoelectric layers can be obtained with good electrical, thermal and mechanical properties.

Diese Aufgabe wird durch ein Verfahren mit den Merkmalen des Patentanspruchs 1 gelöst. This object is achieved by a method having the features of patent claim 1.

Bei einem solchen Verfahren zum Herstellen einer thermoelektrischen Schicht wird ein halbleitendes Material durch einen Sol-Gel-Prozess aus zumindest einem löslichen organischen Vorläuferstoff erzeugt, welcher in Lösung unter Ausbildung eines Gels aggregiert und anschließend getrocknet und getempert wird. In such a method for producing a thermoelectric layer, a semiconductive material is produced by a sol-gel process of at least one soluble organic precursor substance, which is aggregated in solution to form a gel and then dried and annealed.

Erfindungsgemäß ist dabei vorgesehen, dass der wässrigen Lösung ein lösliches Polymer zugesetzt werden. According to the invention, it is provided that a soluble polymer is added to the aqueous solution.

Durch den an sich bekannten Sol-Gel-Prozess können thermoelektrische Schichten hergestellt werden, die eine Porenstruktur aufweisen. Diese ist üblicherweise jedoch schwer zu kontrollieren. Die erfindungsgemäße Zugabe des Polymers ermöglicht es jedoch, durch die Wahl der Ausgangsstoffe und des Verhältnisses zwischen Polymer und Vorläuferstoffen, Porengröße, Porenanteil und Porenverteilung genau zu kontrollieren. Das Polymer wirkt dabei als Templat, welches die entstehende Mikrostruktur der Schicht bestimmt. By the known sol-gel process thermoelectric layers can be produced, which have a pore structure. However, this is usually difficult to control. The addition of the polymer according to the invention, however, makes it possible to precisely control the pore size, pore content and pore distribution through the choice of starting materials and the ratio between polymer and precursor materials. The polymer acts as a template, which determines the resulting microstructure of the layer.

Vorzugsweise weist das Polymer eine Zersetzungstemperatur unterhalb einer Zersetzungstemperatur des halbleitenden Materials auf. Dies ermöglicht es, das Polymer nach dem Trocknen des im Verlauf der Herstellung der Schicht entstehenden Gels durch eine schonende Wärmebehandlung zu entfernen, ohne dass die Zusammensetzung oder Struktur der Schicht beeinträchtigt wird. Preferably, the polymer has a decomposition temperature below a decomposition temperature of the semiconducting material. This makes it possible to remove the polymer by gentle heat treatment after drying the gel formed in the course of the production of the layer, without affecting the composition or structure of the layer.

Durch eine solche Wärmebehandlung wird das Polymer vorzugsweise zersetzt und/oder verdampft. Idealerweise sollten dabei die Zersetzungsprodukte kein signifikant großes Volumen einnehmen, um eine Zerstörung der Porenstruktur zu vermeiden. By such a heat treatment, the polymer is preferably decomposed and / or evaporated. Ideally, the decomposition products should not occupy a significantly large volume in order to avoid destruction of the pore structure.

Es ist ferner zweckmäßig, das Polymer in Form von Nanopartikeln zuzugegeben, so dass definierte Porenstrukturen im Nanometerbereich gebildet werden. It is also expedient to add the polymer in the form of nanoparticles so that defined pore structures in the nanometer range are formed.

Im Folgenden werden die Erfindung und ihre Ausführungsformen anhand der Zeichnung näher erläutert. Es zeigen: In the following the invention and its embodiments will be explained in more detail with reference to the drawing. Show it:

1 Eine schematische Darstellung der Verfahrensschritte bei einem Sol-Gel-Prozess; und 1 A schematic representation of the process steps in a sol-gel process; and

2 eine Mikrophotographie eines Schnitts durch eine mit einem Ausführungsbeispiel eines erfindungsgemäßen Verfahrens hergestellte Schicht. 2 a photomicrograph of a section through a layer produced with an embodiment of a method according to the invention.

Um eine halbleitende Schicht 10 für einen Thermoschenkel eines thermoelektrischen Generators herzustellen, werden zunächst Vorläuferprodukte für das Halbleitermaterial in Lösung 12 bereitgestellt. To a semiconducting layer 10 For producing a thermo leg of a thermoelectric generator, first precursor products for the semiconductor material in solution 12 provided.

Ein Beispiel für einen geeigneten Halbleiter ist antimondotiertes Zinnoxid. Als Edukte dienen hierbei tertiäres Zinnbutoxid in wasserfreiem Ethanol und Acetylaceton, sowie Antimon(III)ethoxid in wasserfreiem Ethanol. Die beiden Sole werden gemischt. Es kommt dabei zur Hydrolyse und Kondensation der Alkoholate, wobei sich zunächst Aggregationskeime 14 und schließlich ein Netzwerk 16 der Kondensationsprodukte ausbildet. Das so entstandene Gel wird getrocknet und anschließend getempert. An example of a suitable semiconductor is antimony doped tin oxide. The educts used in this case are tertiary tin butoxide in anhydrous ethanol and acetylacetone, and also antimony (III) ethoxide in anhydrous ethanol. The two brine are mixed. It comes thereby to the hydrolysis and condensation of the alcoholates, whereby first aggregation germs 14 and finally a network 16 forms the condensation products. The resulting gel is dried and then tempered.

Ein so gefertigter Halbleiter ist porös, weist jedoch eine schlecht definierte Porenstruktur auf. Um Porengröße und -verteilung kontrolliert einzustellen, werden dem Ausgangssol Nanopartikel aus einem wasserlöslichen Polymer zugesetzt. Hierfür können beispielsweise Polyethylenglykol, Polypropylenglykol, Copolymere der vorgenannten, Polyvinylpyrrolidon, substituierte und unsubstituierte Polyether und Polyester Verwendung finden. A semiconductor produced in this way is porous, but has a poorly defined pore structure. In order to control the pore size and distribution, nanoparticles of a water-soluble polymer are added to the starting sol. For example, polyethylene glycol, polypropylene glycol, copolymers of the aforementioned, polyvinylpyrrolidone, substituted and unsubstituted polyethers and polyesters can be used for this purpose.

Die Nanopartikel verteilen sich gleichmäßig im entstehenden Gel und unterstützen die Bildung einer definierten Mikrostruktur, wie in den Mikrophotographien in 2 zu erkennen. The nanoparticles are evenly distributed in the resulting gel and assist in the formation of a defined microstructure, as in the microphotographs in 2 to recognize.

Beim Tempern des getrockneten Gels zersetzen sich die zugegebenen Polymere, so dass sich die eigentlichen Poren 18 in der Schicht 10 ausbilden können. Die entstehenden Zersetzungsprodukte können durch das Porennetzwerk abdiffundieren, so dass die gewünschte poröse Schicht mit guter elektrischer und geringer thermischer Leitfähigkeit entsteht. Auf diese Weise können halbleitende Schichten mit einer Dicke von wenigen Nanometern bis zu einigen Mikrometern erzeugt werden. Upon annealing the dried gel, the added polymers decompose, leaving the actual pores 18 in the layer 10 can train. The resulting decomposition products can diffuse through the pore network, so that the desired porous layer with good electrical and low thermal conductivity is formed. In this way, semiconducting layers with a thickness of a few nanometers to a few micrometers can be produced.

Claims (4)

Verfahren zum Herstellen einer thermoelektrischen Schicht (10), bei welchem ein halbleitendes Material durch einen Sol-Gel-Prozess aus zumindest einem löslichen organischen Vorläuferstoff erzeugt wird, welcher in Lösung unter Ausbildung eines Gels aggregiert und anschließend getrocknet und getempert wird, dadurch gekennzeichnet, dass der wässrigen Lösung ein lösliches Polymer zugesetzt wird. Method for producing a thermoelectric layer ( 10 ), in which a semiconductive material is produced by a sol-gel process from at least one soluble organic precursor, which is aggregated in solution to form a gel and then dried and annealed, characterized in that a soluble polymer is added to the aqueous solution , Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass das Polymer eine Zersetzungstemperatur unterhalb einer Zersetzungstemperatur des halbleitenden Materials aufweist. A method according to claim 1, characterized in that the polymer has a decomposition temperature below a decomposition temperature of the semiconducting material. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass das Polymer in einem anschließenden Wärmebehandlungsschritt zersetzt und/oder verdampft wird. A method according to claim 1 or 2, characterized in that the polymer is decomposed and / or evaporated in a subsequent heat treatment step. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass das Polymer in Form von Nanopartikeln zugegeben wird. Method according to one of claims 1 to 3, characterized in that the polymer is added in the form of nanoparticles.
DE201210217588 2012-09-27 2012-09-27 Manufacture of thermoelectric layer for thermal leg of thermoelectric generator, involves subjecting semiconductor material produced using aqueous solution comprising soluble polymer and soluble organic precursor, to sol-gel process Withdrawn DE102012217588A1 (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3257088A4 (en) * 2015-02-13 2019-01-16 Pen, The Practical method of producing an aerogel composite continuous thin film thermoelectric semiconductor material

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102005063038A1 (en) * 2005-12-29 2007-07-05 Basf Ag Nano wires or nano tubes manufacturing method for e.g. air conditioning system, involves providing melted mass or solution, which contains thermo electric active material or precursor compounds of thermo electric active materials
US20090185942A1 (en) * 2007-12-04 2009-07-23 National Institute Of Aerospace Associates Fabrication of advanced thermoelectric materials by hierarchical nanovoid generation
US20110006249A1 (en) * 2009-07-10 2011-01-13 Lidong Chen Thermoelectric composite material and method of producing the same

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102005063038A1 (en) * 2005-12-29 2007-07-05 Basf Ag Nano wires or nano tubes manufacturing method for e.g. air conditioning system, involves providing melted mass or solution, which contains thermo electric active material or precursor compounds of thermo electric active materials
US20090185942A1 (en) * 2007-12-04 2009-07-23 National Institute Of Aerospace Associates Fabrication of advanced thermoelectric materials by hierarchical nanovoid generation
US20110006249A1 (en) * 2009-07-10 2011-01-13 Lidong Chen Thermoelectric composite material and method of producing the same

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3257088A4 (en) * 2015-02-13 2019-01-16 Pen, The Practical method of producing an aerogel composite continuous thin film thermoelectric semiconductor material

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