EP2250126A2 - Tellurures de zinc dopés pour applications thermoélectriques - Google Patents

Tellurures de zinc dopés pour applications thermoélectriques

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Publication number
EP2250126A2
EP2250126A2 EP09708165A EP09708165A EP2250126A2 EP 2250126 A2 EP2250126 A2 EP 2250126A2 EP 09708165 A EP09708165 A EP 09708165A EP 09708165 A EP09708165 A EP 09708165A EP 2250126 A2 EP2250126 A2 EP 2250126A2
Authority
EP
European Patent Office
Prior art keywords
semiconductor material
temperature
generator
thermoelectric
elements
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP09708165A
Other languages
German (de)
English (en)
Inventor
Frank Haass
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
BASF SE
Original Assignee
BASF SE
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by BASF SE filed Critical BASF SE
Priority to EP09708165A priority Critical patent/EP2250126A2/fr
Publication of EP2250126A2 publication Critical patent/EP2250126A2/fr
Withdrawn legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00—Selenium; Tellurium; Compounds thereof
    • C01B19/002—Compounds containing, besides selenium or tellurium, more than one other element, with -O- and -OH not being considered as anions
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00—Selenium; Tellurium; Compounds thereof
    • C01B19/007—Tellurides or selenides of metals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
    • H01L23/38—Cooling arrangements using the Peltier effect
    • 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
    • H10N10/852—Thermoelectric active materials comprising inorganic compositions comprising tellurium, selenium or sulfur
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/0001—Technical content checked by a classifier
    • H01L2924/0002—Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency
    • Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines

Definitions

  • the present invention relates to semiconductor materials containing tin and usually tellurium and at least one or two further dopants, as well as these containing thermoelectric generators and Peltier arrangements.
  • Thermoelectric generators and Peltier devices as such have long been known, p-type and n-type doped semiconductors, heated on one side and cooled on the other, carry electrical charges through an external circuit, electrical work being done to a load in the circuit can be performed.
  • the achieved conversion efficiency of heat into electrical energy is thermodynamically limited by the Carnot efficiency.
  • an efficiency of (1000 - 400): 1000 60% is possible.
  • efficiencies below 10% are achieved.
  • Such a Peltier arrangement operates as a heat pump and is therefore suitable for cooling equipment parts, vehicles or buildings.
  • the heating via the Peltier principle is cheaper than a conventional heating, because more and more heat is transported than the supplied energy equivalent corresponds.
  • thermoelectric generators are used, for example, in space probes for generating direct currents, for the cathodic corrosion protection of pipelines, for the power supply of illuminated and radio buoys and for the operation of radios and television sets.
  • the advantages of the thermoelectric generators are in their utmost reliability. So they work regardless of atmospheric conditions such as humidity; there is no fault-susceptible mass transport, but only a charge transport. It can be used any fuel from hydrogen over natural gas, gasoline, kerosene, diesel fuel up to biologically produced fuels such as rapeseed oil methyl ester.
  • thermoelectric energy conversion adapts extremely flexibly to future needs, such as hydrogen economy or energy generation from regenerative energies.
  • thermoelectric generators At least in part even today, however, previous technologies only achieve efficiencies of well below 10%, so that still a large part of the energy is lost unused. When using waste heat, therefore, significantly higher efficiencies are sought.
  • Concentrators such as parabolic troughs can focus solar energy on thermoelectric generators, generating electrical energy.
  • thermoelectrically active materials are essentially evaluated on the basis of their efficiency. Characteristic of thermoelectric materials in this regard is the so-called Z factor (figure of merit):
  • thermoelectric materials which have the lowest possible thermal conductivity, the highest possible electrical conductivity and the largest possible Seebeck coefficient, so that the Z-factor as high as possible Takes value.
  • the product S 2 ⁇ is called the power factor and serves to compare the thermoelectric materials.
  • thermoelectric materials have maximum Z-T values of about 1 at an optimum temperature. Beyond this optimum temperature, Z-T values are often significantly lower than 1.
  • thermoelectrically active material which has the highest possible value for Z and a high temperature difference that can be achieved. From the point of view of solid-state physics many problems have to be overcome:
  • a high ⁇ requires a high electron mobility in the material, ie electrons (or holes in p-type materials) should not be strongly bound to the atomic hulls.
  • Materials with high electrical conductivity ⁇ usually have at the same time a high thermal conductivity (Wiedemann - Franz's Law), which means that Z can not be favorably influenced.
  • Currently used materials such as Bi 2 Te 3 are already compromises. Thus, the electrical conductivity is reduced by alloying less than the thermal conductivity. Therefore, it is preferable to use alloys such as (Bi 2 Te 3 ) 9o (Sb 2 Te 3 ) 5 (Sb 2 Se 3 ) 5 or Bi 12 Sb 23 Te 6 S, as described in US Pat. No. 5,448,109.
  • thermoelectric materials with high efficiency preferably further boundary conditions are to be met. Above all, they have to be sufficiently temperature-stable to be able to work under operating conditions for years without significant loss of efficiency. This requires a high temperature stable phase per se, a stable phase composition and a negligible diffusion of alloying components into the adjacent contact materials.
  • Doped lead tellurides for thermoelectric applications are described, for example, in WO 2007/104601. These are lead tellurides which, in addition to a large amount of lead, also contain one or two further dopants. The respective proportion of dopants, based on the formula (I) given in WO, is 1 ppm to 0.05.
  • Example 5 discloses Pbo, 987Ge o , oiSn o , oo3Tei, ooi- This material also contains the lowest lead content of the exemplary compounds. Thus, the materials have very high lead contents and, if any, only very low levels of tin.
  • WO 2007/104603 relates to lead germanium tellurides for thermoelectric applications. These are ternary compounds of lead, germanium and tellurium, which in turn contain very high levels of lead.
  • thermoelectrically active materials which have a high thermoelectric efficiency and show a suitable property profile for different fields of application.
  • a 1 ... A n are different from one another and are selected from the group of the elements Li, Na, K, Rb, Cs, Mg, Ca, Y, Ti, Zr, Hf, Nb, Ta, Cr, Mn, Fe, Cu, Ag, Au, Ga, In, Tl, Ge, Sb, Bi
  • X is F, Cl, Br or I
  • Zinntelluride having a tin content of more than 5 wt .-%, preferably of at least 10 wt .-%, in particular of at least 20 wt .-% have very good thermoelectric properties when added with at least one additional dopant are.
  • n indicates the number of chemical elements other than SnPb, and Te, Se, S and X are not considered.
  • the materials may be pure tellurides.
  • Tellurium may also be wholly or partly replaced by selenium, sulfur or, in minor amounts, halide.
  • Preference is 0 ⁇ p ⁇ 0.2, more preferably 0 ⁇ p ⁇ 0.05.
  • n is an integer of at least 1.
  • n has a value ⁇ 10, more preferably ⁇ 5.
  • n has the value 1 or 2.
  • the proportion of tin is according to the invention 0.05 ⁇ a ⁇ 1.
  • Each of the mutually different additional elements A 1 to A n is present in an amount of 1 ppm ⁇ x1 ... xn ⁇ 0.05.
  • the sum of x1... Xn is preferably 0.0005 to 0.1, particularly preferably 0.001 to 0.08.
  • the individual values are likewise preferably 0.0005 to 0.1, more preferably 0.001 to 0.08.
  • the dopants A 1 ... A n can be selected as desired from the group consisting of the elements Li, Na, K, Rb, Cs, Mg, Ca, Y, Ti, Zr, Hf, Nb, Ta, Cr, Mn, Fe, Cu, Ag, Au, Ga, In, Tl, Ge, Sb, Bi. Particularly preferred are A 1 ... A n selected from the group of the elements Li, Na, K, Mg, Ti, Zr, Hf, Nb, Ta, Mn, Ag, Ga, In, Ge. In particular, A 1 ... A n are different from one another and are selected from the group of the elements Ag, Mn, Na, Ti, Zr, Ge, Hf.
  • Seebeck coefficients were determined, for example, in the range from 70 to 202 ⁇ V / K for the p-type systems.
  • the electrical conductivity was, for example, in the range of 1000 to 5350 S / cm.
  • the exemplary power factors were 18 to 54 ⁇ W / K 2 cm.
  • the materials of the invention are generally prepared by reactive milling or, preferably, by fusing and reaction of mixtures of the respective constituent elements or their alloys.
  • a reaction time of the reactive grinding or, preferably, melting together of at least one hour has proven to be advantageous.
  • the melting together and reacting are preferably carried out for a period of at least 1 hour, more preferably at least 6 hours, especially at least 10 hours.
  • the melting process can be carried out with or without mixing of the starting mixture.
  • a rotary or tilt oven to ensure the homogeneity of the mixture.
  • the melting time is generally 2 to 50 hours, especially 30 to 50 hours.
  • Melting generally occurs at a temperature at which at least one component of the mixture has already melted.
  • the melting temperature is at least 800 ° C., preferably at least 950 ° C.
  • the melting temperature is in a temperature range from 800 to 1100 ° C., preferably 950 to 1050 ° C.
  • the material After cooling the molten mixture, it is advantageous, pern the material at a temperature of generally at least 100 0 C, preferably at least 200 0 C lower than the melting point of the resulting semiconductor material to TEM.
  • the temperature is 450 to 750 0 C, preferably 550 and 700 0 C.
  • the annealing is carried out for a period of preferably at least 1 hour, particularly preferably at least 2 hours, in particular at least 4 hours. Usually, the annealing time is 1 to 8 hours, preferably 6 to 8 hours. In one embodiment of the present invention, the annealing is performed at a temperature which is 100 to 500 ° C lower than the melting temperature of the resulting semiconductor material. A preferred temperature range is 150 to 350 0 C lower than the melting point of the resulting HaIb- conductor material.
  • thermoelectric materials according to the invention is generally carried out in an evacuated and sealed quartz tube. Mixing of the components involved can be ensured by using a rotatable and / or tiltable opening. After completion of the reaction, the furnace is cooled. Thereafter, the quartz tube is removed from the oven and the block-shaped semiconductor material is sliced. These disks are now cut into pieces of about 1 to 5 mm in length, from which thermoelectric modules can be produced.
  • a quartz tube it is also possible to use tubes or ampoules of other materials inert to the semiconductor material, for example of tantalum.
  • tubes other containers of suitable shape can be used.
  • Other materials such as graphite, may also be used as the container material, as long as they are inert to the semiconductor material.
  • a synthesis of the materials can also be carried out by melting / fusing in an induction furnace, for example in crucibles made of graphite.
  • the cooled material can be ground wet, dry or in another suitable manner at a suitable temperature, so that the semiconductor material according to the invention is obtained in customary particle sizes of less than 10 ⁇ m.
  • the milled material of the invention is then extruded hot or cold, or preferably hot or cold pressed into moldings having the desired shape.
  • the bulk density of the shaped parts pressed in this way should preferably be greater than 50%, particularly preferably greater than 80%, than the bulk density of the raw material in the unpressed state.
  • Compounds which improve the densification of the material according to the invention can be added in quantities of preferably 0.1 to 5% by volume, more preferably 0.2 to 2% by volume, based in each case on the powdered material according to the invention.
  • Additives which are added to the materials according to the invention should preferably be inert to the semiconductor material and preferably dissolve out of the material according to the invention during heating to temperatures below the sintering temperature of the materials according to the invention, if appropriate under inert conditions and / or vacuum. After pressing, the pressed parts are preferably placed in a sintering furnace in which they are heated to a temperature of preferably at most 20 0 C below the melting point.
  • the pressed parts are sintered at a temperature of generally at least 100 ° C., preferably at least 200 ° C., lower than the melting point of the resulting semiconductor material.
  • the sintering temperature is 350 to 750 0 C, preferably 600 to 700 0 C. It is also spark plasma sintering (SPS) or microwave sintering can be performed.
  • the sintering is carried out for a period of preferably at least 0.5 hours, particularly preferably at least 1 hour, in particular at least 2 hours. Usually, the sintering time is 0.5 to 5 hours, preferably 1 to 3 hours. In one embodiment of the present invention, the sintering is performed at a temperature which is 100 to 600 ° C lower than the melting temperature of the resulting semiconductor material. A preferred temperature range is 150 to 350 0 C lower than the melting point of the resulting semiconductor material.
  • the sintering is preferably carried out in a reducing atmosphere, for example under hydrogen, or in a protective gas atmosphere, for example of argon.
  • the pressed parts are preferably sintered to 95 to 100% of their theoretical bulk density.
  • the invention also relates to semiconductor materials obtainable or obtained by the processes according to the invention or prepared.
  • Another object of the present invention is the use of the above-described semiconductor material and the semiconductor material obtainable by the method described above as a thermoelectric generator or Peltier arrangement.
  • thermoelectric generators or Peltier arrangements which contain the semiconductor material described above and / or the semiconductor material obtainable by the method described above.
  • Another object of the present invention is a process for the production of thermoelectric generators or Peltier arrangements, in which series-connected thermoelectrically active building blocks (“legs”) are used with thin layers of the previously described thermoelectric materials.
  • thermoelectric generators or Peltier arrangements which are known per se to the person skilled in the art and are described, for example, in WO 98/44562, US Pat. No. 5,448,109, EP-A-1 102 334 or US Pat. No. 5,439,528.
  • the thermoelectric generators or Peltier arrangements according to the invention generally expand the available range of thermoelectric generators and Peltier arrangements. By varying the chemical composition of the thermoelectric generators or Peltier arrangements, it is possible to provide different systems which meet different requirements in a variety of applications. Thus, the thermoelectric generators or Peltier arrangements according to the invention expand the range of applications of these systems.
  • the present invention also relates to the use of a thermoelectric generator according to the invention or a Peltier arrangement according to the invention.
  • the present invention relates to a heat pump, a cooler, a refrigerator, a (laundry) dryer, a generator for converting thermal energy into electrical energy, or a generator for using heat sources, comprising at least one thermoelectric generator according to the invention or a Peltier invention Arrangement.
  • a heat pump a cooler, a refrigerator, a (laundry) dryer, a generator for converting thermal energy into electrical energy, or a generator for using heat sources, comprising at least one thermoelectric generator according to the invention or a Peltier invention Arrangement.
  • the synthesis of the materials of the following compositions always took place from the elements or the elemental tellurides.
  • the purity of the materials used was always ⁇ 99.99%.
  • the educts were each weighed in the appropriate stoichiometric ratio into a purified quartz ampoule having an inner diameter of 10 mm.
  • the sample amount was 20 g each.
  • the ampoule was evacuated and melted. Subsequently, the ampoule was heated in the oven with a maximum of 500 K h "1 to 1050 0 C and held at this temperature for 8 hours., While the contents of the ampoule was continuously mixed by tilting the furnace After the reaction time, the ampoule with a maximum of 100 K. h "1 was cooled in an upright furnace position to 600 0 C and the material was annealed at this temperature for 24 h. Thereafter, the material was cooled to room temperature.
  • the samples were always compact, glossy silver Reguli, which were taken from the ampoules and cut with a diamond wire saw in about 1, 5 mm thick slices. The electric conductivity and the Seebeck coefficient were measured on these disks.
  • the Seebeck coefficient was determined by placing the material to be tested between a hot and a cold contact, the hot contact having a temperature around 300 ° C and keeping the cold side at room temperature. The measured voltage at the respective temperature difference between hot and cold contact provided the respectively specified Seebeck coefficient.
  • the electrical conductivity was determined at room temperature by a four-point measurement.
  • the process is known to the person skilled in the art.
  • Table 1 below gives the Seebeck coefficients S, the electrical conductivity ⁇ and the resulting power factor S 2 ⁇ for different compositions.
  • FIG. 2 shows the corresponding results for different materials.
  • the respective Seebeck coefficient is plotted against the temperature.
  • the measurements confirm that materials with a very high lead content show a change from p-type to n-type with increasing temperature.
  • the systems do not meet the requirements in terms of temperature stability, and the Seebeck coefficient has, depending on the temperature, very low values.
  • p-L means p-line and n-L n-line.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Manufacturing & Machinery (AREA)
  • Powder Metallurgy (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

L'invention concerne un matériau semi-conducteur de type p ou n qui contient un composé de formule générale Sna Pb1-a-(x1+... +xn) A1x1...Anxn (Te1-p-q-r SepSqXr)1+z (I). Dans la formule (I), 0,05 < a < 1, n ≥ 1, n représentant le nombre d'éléments chimiques différents de Sn et Pb et, respectivement indépendamment, 1 ppm ≤ x1... xn ≤ 0,05, A1... An sont différents les uns des autres et sélectionnés dans le groupe des éléments Li, Na, K, Rb, Cs, Mg, Ca, Y, Ti, Zr, Hf, Nb, Ta, Cr, Mn, Fe, Cu, Ag, Au, Ga, In, Tl, Ge, Sb, Bi, X représente F, Cl, Br ou I, 0 ≤ p ≤ 1, 0 ≤ q ≤ 1, 0 ≤ r ≤ 0,01, - 0,01 ≤ z ≤ 0,01, à condition que p + q + r ≤ 1 et a + x1 +... + xn ≤ 1.
EP09708165A 2008-02-07 2009-02-05 Tellurures de zinc dopés pour applications thermoélectriques Withdrawn EP2250126A2 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP09708165A EP2250126A2 (fr) 2008-02-07 2009-02-05 Tellurures de zinc dopés pour applications thermoélectriques

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP08151149 2008-02-07
EP09708165A EP2250126A2 (fr) 2008-02-07 2009-02-05 Tellurures de zinc dopés pour applications thermoélectriques
PCT/EP2009/051298 WO2009098248A2 (fr) 2008-02-07 2009-02-05 Tellurures de zinc dopés pour applications thermoélectriques

Publications (1)

Publication Number Publication Date
EP2250126A2 true EP2250126A2 (fr) 2010-11-17

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP09708165A Withdrawn EP2250126A2 (fr) 2008-02-07 2009-02-05 Tellurures de zinc dopés pour applications thermoélectriques

Country Status (9)

Country Link
US (1) US8772622B2 (fr)
EP (1) EP2250126A2 (fr)
JP (1) JP5468554B2 (fr)
KR (1) KR20110004362A (fr)
CN (1) CN101965313A (fr)
CA (1) CA2715040A1 (fr)
RU (1) RU2010137002A (fr)
TW (1) TW200950165A (fr)
WO (1) WO2009098248A2 (fr)

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KR102001062B1 (ko) 2012-01-16 2019-10-01 삼성전자주식회사 나노복합체형 열전재료, 이를 포함하는 열전모듈과 열전장치
KR101442018B1 (ko) * 2013-04-10 2014-09-24 국방과학연구소 알칼리 및 알칼리 토금속이 첨가된 화합물 및 이 화합물을 합성하여 제조되는 열전재료
KR101760834B1 (ko) 2015-10-07 2017-08-01 서울대학교산학협력단 칼코겐화합물 열전소재 및 이를 포함하는 열전소자
WO2020116388A1 (fr) * 2018-12-04 2020-06-11 住友化学株式会社 Composé, et matériau de conversion thermoélectrique
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CN111517292A (zh) * 2020-04-30 2020-08-11 西华大学 一种碲化锡基热电材料及其制备方法
TWI792310B (zh) * 2021-05-13 2023-02-11 國立中興大學 高效能熱電材料

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CN101965313A (zh) 2011-02-02
KR20110004362A (ko) 2011-01-13
US8772622B2 (en) 2014-07-08
TW200950165A (en) 2009-12-01
RU2010137002A (ru) 2012-03-20
JP2011514666A (ja) 2011-05-06
WO2009098248A2 (fr) 2009-08-13
JP5468554B2 (ja) 2014-04-09
CA2715040A1 (fr) 2009-08-13
US20110012069A1 (en) 2011-01-20
WO2009098248A3 (fr) 2010-02-25

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