KR20160139535A - Thermoelectric material containing higher manganese silicides, and preparation method thereof - Google Patents
Thermoelectric material containing higher manganese silicides, and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a thermoelectric material containing a high manganese silicide compound and a method of manufacturing the same. The thermoelectric material according to the present invention includes a high manganese silicide compound having a composition of MnSi 2 .1-x (0 ? X ? 0.2) and has excellent thermoelectric performance. Therefore, the thermoelectric material used in a cooling system of LED, water purifier, It can be usefully used in devices.
Description
The present invention relates to a thermoelectric material containing a high manganese silicide-based compound and having a thin film form, and a method for producing the same.
Manganese silicide, but the behavior, such as a metal in the composition MnSi, Mn 4 Si 7 (MnSi 1.75 ), Mn 11 Si 19 (MnSi 1 .72), Mn 15 Si 26 (MnSi 1 .73), Mn 27 Si 47 ( MnSi 1 .74), such as MnSi 1.72 ~ 1.75 in the composition range show the behavior of the p-type semiconductor having a 0.4 ~ 0.7 eV narrow bandgap energy. These manganese silicide having MnSi 1 .72 ~ 1.75 and a composition is referred to as manganese silicide (HMS, higher manganese silicides). The high-manganese silicide is rich in resources, is low in cost, is environmentally friendly, has excellent mechanical stability, and has high oxidation resistance at high temperatures, and researches on thermoelectric materials applied thereto have been actively conducted.
As an example thereof,
However, since the above technologies are difficult to produce thermoelectric materials having a complicated manufacturing process and thin film form, or even when a thin film material can be manufactured, high manganese silicide is used as a raw material for this purpose. It is difficult to produce a thin film having an exact composition ratio due to a difference in vapor pressure between raw materials at the time of vapor deposition.
Accordingly, there is a desperate need to develop a thin film type high manganese silicide thermoelectric material which is excellent in thermal conductivity, and is superior in cooling efficiency by a simple process.
It is an object of the present invention to provide a thin film type high manganese silicide type thermoelectric material which not only has excellent thermoelectric performance, but also has a better cooling efficiency by a simple process.
Another object of the present invention is to provide a method of manufacturing the thermoelectric material.
It is still another object of the present invention to provide a thermoelectric element including the thermoelectric material.
In order to achieve the above object,
The present invention, in one embodiment,
A compound represented by the following general formula (1)
There is provided a thermoelectric material having a thin film form of a polycrystalline structure in which crystals of the compound are regularly arranged:
[Chemical Formula 1]
MnSi 2 .1-x (0≤x≤0.2) .
In addition, the present invention, in one embodiment,
Manganese (Mn) is vapor-deposited on a substrate containing silicon (Si) to deposit on silicon (Si)
A compound represented by the following general formula (1)
And forming a thin film of polycrystalline structure in which crystals of the compound are regularly arranged.
[Chemical Formula 1]
MnSi 2 .1-x (0≤x≤0.2) .
Further, the present invention, in one embodiment,
A compound represented by the following general formula (1)
A thermoelectric material having a thin film form of a polycrystalline structure in which crystals of the compound are regularly arranged; And
There is provided a thermoelectric device further comprising a substrate containing silicon (Si) on one surface of a thin film thermoelectric material:
[Chemical Formula 1]
MnSi 2 .1-x (0≤x≤0.2) .
The thermoelectric material according to the present invention includes a high manganese silicide-based compound having a composition of MnSi 2 .1-x (0 ? X ? 0.2) and is excellent in thermoelectric performance. Therefore, the thermoelectric material used in a cooling system of LED, water purifier, . ≪ / RTI >
1 is a graph showing an X-ray diffraction measurement result of a thermoelectric material according to an embodiment of the present invention.
FIG. 2 is a graph illustrating the energy dispersive spectroscopy (EDS) of a 7 zone (3 zones and 3 zones) selected to measure energy dispersive spectroscopy (EDS) using a high-angle annular dark-field imaging (HAADF) 4 points).
3 is an image of a thermoelectric material according to an embodiment of the present invention using a high-resolution transmission electron microscope (HRTEM) in one embodiment.
FIG. 4 is a graph showing an electrical resistivity according to temperature of a thermoelectric material according to an embodiment of the present invention.
FIG. 5 is a graph showing Seebeck coefficients according to temperature of a thermoelectric material according to an embodiment of the present invention.
While the invention is susceptible to various modifications and alternative forms, specific embodiments thereof are shown by way of example in the drawings and will herein be described in detail.
It is to be understood, however, that the invention is not to be limited to the specific embodiments, but includes all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
In the present invention, the terms "comprising" or "having ", and the like, specify that the presence of a feature, a number, a step, an operation, an element, a component, But do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, or combinations thereof.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory and are intended to provide further explanation of the invention as claimed.
Hereinafter, the present invention will be described in detail with reference to the drawings, and the same or corresponding components are denoted by the same reference numerals regardless of the reference numerals, and a duplicate description thereof will be omitted.
In the present specification, the term "polycrystal" means an irregularly aggregated form of single crystals having a certain crystal orientation, and may include some single crystals. In the case of the thermoelectric material according to the present invention, single crystals having a certain directionality and arranged may have a structure gathered along the lattice direction of the silicon wafer.
The present invention relates to a thermoelectric material containing a high manganese silicide compound represented by the general formula (1) and a method for producing the same.
The manganese silicide is rich in resources, low in cost, eco-friendly, excellent in mechanical stability, and has high oxidation resistance at high temperature, so that research on thermoelectric materials produced using the manganese silicide has been actively conducted. However, the technologies developed so far are difficult to manufacture thermoelectric materials having a complex manufacturing process and thin films, and even if thin films can be formed, high-manganese silicide must be used as a raw material for this purpose. Therefore, manganese and silicon are used as raw materials It is difficult to produce a thin film having an exact composition ratio due to a difference in vapor pressure between raw materials at the time of vapor deposition.
Accordingly, the present invention proposes a MnSi 2 .1-x (0≤x≤0.2) and having a composition of manganese silicide based compound in the form of a thin film thermoelectric material containing, and methods for their preparation.
Hereinafter, the present invention will be described in detail.
The present invention, in one embodiment,
A thermoelectric material comprising a compound represented by the following formula (1):
[Chemical Formula 1]
MnSi 2 .1-x (0≤x≤0.2) .
The thermoelectric material according to the present invention may include a high-manganese silicide-based compound which is low in raw material cost, is environmentally friendly, and excellent in mechanical stability. More specifically include compounds represented by the compound having MnSi 2.1-x (0≤x≤0.2) composition, for example, MnSi 2, such as Mn 2 Si 4, Mn 3 Si 6 to about a fraction of more than 95% of the thermal conductive material to, and may include some of the high manganese silicide-based compounds MnSi 1 .72-1.75 composition exhibit the same behavior of the behavior, such as a metal look manganese silicide (MnSi) and the p-type semiconductor.
In one embodiment, X-ray diffraction and energy dispersive spectroscopy were measured to confirm the crystal structure and compound composition of the thermoelectric material. As a result, the lattice constant of the thermoelectric material was found to be a = 0.5518 nm and c = 1.7445 nm. It was also found that the content ratio (Mn / Si) of manganese (Mn) and silicon (Si) contained in the thermoelectric material was 1: 1.91 to 2.09, and the average was 1: 2.00.
From these results and the thermoelectric material is having MnSi 1 .72 ~ 1.75 and manganese silicide based compound composition and structure are similar to MnSi 1 .72 ~ 1.75 The composition is not MnSi 2 .1-x (0≤x≤0.2) composition Containing manganese silicide compound (see Experimental Example 1).
Further, the thermoelectric material according to the present invention may have a thin film form of polycrystalline structure in which crystals of the compound represented by the formula (1) are uniformly arranged.
In order to confirm the structure of the thermoelectric material according to the present invention, a high resolution transmission electron microscope (HRTEM) photograph of the thermoelectric material was performed. As a result, it was confirmed that the thermoelectric material had a thin film shape formed on a silicon (Si) wafer having a Miller index of [1,1,1]. Also, it was confirmed that the thin film had uniformly sized crystals having a certain directionality and arrangement, and the directionality thereof progressed along the lattice directionality of the silicon wafer.
From these results, it can be seen that the thermoelectric material according to the present invention is a thin film of polycrystalline structure in which crystals of the compound represented by the formula (1) are uniformly arranged.
Further, the thermoelectric material according to the present invention can exhibit excellent thermoelectric performance by including a compound represented by
As an example, the thermoelectric material may have an average output factor (S 2 σ) of 1.00 × 10 -4 W / k 2 · m or more. Specifically, the average output factor (S 2 σ) is 2.00 × 10 -4 W / k 2 · m or more; 3.00 × 10 -4 W / k 2 · m or more; 4.00 × 10 -4 W / k 2 · m or more; Or 5.0 × 10 -4 W / k 2 · m or more.
Further, the figure of merit (ZT) of the thermoelectric material may be 0.4 or more. Specifically, the thermoelectric material has a figure of merit (ZT) of 0.45 or more; 0.46 or more; 0.47 or more; .0.48 or higher; 0.49 or more; Or 0.5 or more.
Generally, the thermoelectric performance of a thermoelectric material is determined by a figure of merit (ZT, T is an absolute temperature) derived by the following equation (1), and the larger the value, the better the performance:
[Equation 1]
As shown in Equation (1), the figure of merit (ZT) of the thermoelectric material depends on the Seebeck coefficient S, the electric resistivity ?, And the thermal conductivity ? The Seebeck coefficient and the electrical conductivity depend on the concentration and scattering of the carrier, ie the carrier. That is, a material having a good thermoelectric performance exhibits a large power factor (S 2 σ) derived from the Seebeck coefficient and the electric conductivity, which determine the figure of merit.
Accordingly, in one embodiment, the electrical resistivity, the Seebeck coefficient, and the carrier concentration were measured at 410 K in order to evaluate the thermoelectric performance of the thermoelectric material. As a result, the electrical resistivity (1 / σ) was 2.08 × 10 -3 Ω · cm and the Seebeck coefficient (S) was 107.84 μV / K. From these, the output factor (S 2 σ) -4 W / K 2 m. Further, the carrier concentration of the thermoelectric material was found to be 7.30 x 10 20 / cm 3 , and it was confirmed that the figure of merit (ZT) was about 0.5. This means that the thermoelectric material according to the present invention is a degenerate semiconductor showing the behavior of a p-type semiconductor, and many carriers present in the material are holes. From these results, it can be seen that the thermoelectric material according to the present invention has excellent thermoelectric performance (see Experimental Example 3).
In addition, the present invention, in one embodiment,
Manganese (Mn) is vapor-deposited on a substrate containing silicon (Si) to deposit on silicon (Si)
A compound represented by the following general formula (1)
And forming a thin film of polycrystalline structure in which crystals of the compound are regularly arranged.
[Chemical Formula 1]
MnSi 2 .1-x (0≤x≤0.2) .
The method for producing a thermoelectric material according to the present invention is a method for producing manganese (Mn) on a substrate containing silicon (Si) using a molecular beam epitaxy (MBE) under ultrahigh vacuum and high temperature, A thin film of a polycrystalline structure in which crystals of the compound represented by the formula (1) are uniformly arranged can be formed.
At this time, in order to perform the molecular beam epitaxy method according to the present invention, the deposition pressure can be controlled to 10 -7 to 10 -10 Torr, specifically 10 -7 to 10 -9 Torr have. Also, the deposition temperature may be 773 to 973 K, more specifically 800 to 950 K; 830 to 910K; Or 850 to 900K. In addition, the deposition rate can be determined using a quartz crystal tracer analyzer, specifically 0.2 to 0.5 Å / s, more specifically 0.3 to 0.4 Å / s.
According to the present invention, manganese silicide particles are formed by inducing a reaction between silicon (Si) and manganese (Mn) on the surface of a substrate by using a molecular beam evaporation source for deposition of manganese. Which is about 2.6 times the thermal expansion coefficient. This difference, and to provide a thin film driving force to relatively reduce the volume of the manganese silicide on the substrate at the temperature conditions in which the manganese silicide Mn 4 Si 7 have the bulk and manganese silicide crystal structure of the composition, the thus formed Mn 4 Si 7 Composition The crystal is bound to two silicon atoms per manganese element present in the crystal for stabilization to form a thin film of polycrystalline structure in which crystals of the compound represented by the formula (1) are arranged in a uniform manner. That is, the method for producing a thermoelectric material according to the present invention can control the pressure, manganese deposition rate, and deposition temperature conditions for performing the molecular beam epitaxy method stacked on a substrate within the above range, A thermoelectric material in the form of a thin film having a thickness effective for realizing a thermoelectric performance can be effectively produced.
On the other hand, the method of manufacturing the thermoelectric material may further include a step of surface-treating the substrate containing silicon (Si) before the step of forming the thin film.
The surface treatment is not particularly limited as long as it is a method capable of removing the oxide film formed on the substrate surface together with the impurities present on the surface of the substrate. For example, cleaning can be performed by washing the silicon (Si) wafer with methanol and keeping the washed wafer immersed in dilute fluoric acid for a period of time.
Further, the present invention, in one embodiment,
A compound represented by the following general formula (1)
A thermoelectric material having a thin film form of a polycrystalline structure in which crystals of the compound are regularly arranged; And
There is provided a thermoelectric device further comprising a substrate containing silicon (Si) on one surface of a thin film thermoelectric material:
[Chemical Formula 1]
MnSi 2 .1-x (0≤x≤0.2) .
The thermoelectric device according to the present invention may include a thermoelectric material in the form of a thin film composed of a crystal of the compound represented by the formula (1), and thus may have excellent thermoelectric performance, especially cooling performance.
In general, the thin film thermoelectric material can be manufactured by the conventional semiconductor deposition method. In addition, it is possible to arrange the thermocouple more than 5 times per unit area in comparison with the bulk material. In consideration of the thickness of the thin film, Is 100 times or more small. That is, since the thermoelectric material according to the present invention has a thin film structure of a polycrystalline structure in which crystals of the compound represented by the formula (1) are uniformly arranged, the cooling performance per unit area can be remarkably excellent as compared with the bulk thermoelectric material. Therefore, the thermoelectric element including the same can be used not only for a thermoelectric generator utilizing natural energy such as solar heat, geothermal heat, and industrial ship / waste heat, but also an on / off type chip cooling apparatus of an optical microchip; A main / auxiliary power source of a microscale device requiring minute power supply; LED, a water purifier, a small refrigerator, a wine cooler, and the like.
At this time, the thermoelectric element may further include a base material such as a silicon (Si) wafer, for example, but not limited to, a substrate containing silicon (Si) on one side of a thin thermoelectric material.
Hereinafter, the present invention will be described in more detail with reference to Examples and Experimental Examples.
However, the following Examples and Experimental Examples are merely illustrative of the present invention, and the present invention is not limited to the following Examples and Experimental Examples.
Example One.
The surface of a silicon (Si) wafer [1, 1, 1] having a width of 3 cm and a width of 3 cm was washed with methanol and immersed in diluted fluoric acid (HF) solution to remove impurities and oxide layer on the surface of the wafer . Thereafter, the wafer was placed in a chamber and preheated at 873K (600 DEG C) for 30 minutes to perform molecular beam epitaxy (MBE) of manganese (Mn) to form a thin film containing a high manganese silicide compound Was prepared. At this time, the molecular beam epitaxy was performed at a speed of 0.35 Å / s for 2857 seconds at 10 -8 Torr using a VG Semicon model V80. The thickness of the thin film formed on the wafer was 276 nm.
Comparative Example One.
In the same manner as in Example 1 except that the molecular beam epitaxy was performed at 473K (200 ° C) instead of 873K (600 ° C) in Example 1, MnSi 1 .75 thin films were prepared. At this time, the thickness of the thin film formed on the wafer was 276 nm.
Experimental Example One.
The following experiment was conducted to confirm the composition of the compound included in the thermoelectric material according to the present invention.
1) X-rays diffraction Measure
X-ray diffraction of the thin film of the thermoelectric material prepared in Example 1 was measured. At this time, X-ray diffraction was carried out by using D / max-RC (Rigaku Co., Tokyo, Japan, Cu-Kα irradiation, 40 kV, 30 mA) and 1.5406 Å wavelength at a scan rate of 0.02 ° / and a pattern was obtained within a range where ? is in the range of 10 to 90 degrees. Showed the measured results in Fig. 1 and Table 1, the measurement result of X-ray diffraction analysis and has a MnSi 1 .72 ~ 1.75 composition range in order to compare manganese silicide based compound, MnSi 1 .72 ~ 1.75 the composition of the compound having The X-ray diffraction measurement results (2 ? = 10 to 60) are shown in Table 2 with reference to
Referring to Figure 1, table 1 and 2, the thermal conductive material according to the invention it can be seen that it has a crystal structure similar to the high manganese silicide-based compounds MnSi 1 .72 ~ 1.75 composition.
For a thermoelectric material produced in particular in Example 1 and the lattice constants are a = 0.5518 nm, c = 1.7445 nm were found to be, aspects of a diffraction peak represented by
This means that the thermal transfer material according to the invention has a crystal structure similar to the high manganese silicide compound of MnSi 1 .72 ~ 1.75 composition.
2) Energy dispersive X-ray spectroscopy
The compositions of the thermoelectric materials prepared in Example 1 were analyzed by line scanning of energy dispersive spectroscopy (EDS) using high-angle annular dark-field imaging (HAADF). As shown in FIG. 2, the spectrum of the energy dispersive spectroscopy was measured by selecting three regions and four points in the material, and the results are shown in Table 3 below.
As shown in Table 3, the thermoelectric material according to the invention it can be seen that having high MnSi 2 .1-x (0≤x≤0.2) the composition contains manganese silicide based compound.
Specifically, manganese and silicon contents of the selected thermoelectric materials prepared in Example 1 were measured, and the content ratio (Mn / Si) was 1: 1.91 to 2.09 And the average was 1: 2.00. This is to the composition of the high manganese silicide based compound constituting the thermoelectric material means that the non-MnSi 2 MnSi 1 .72 ~ 1.75.
From these results, the thermoelectric material according to the invention MnSi 1 .72 ~ 1.75 has a crystal structure similar to the high manganese silicide compounds of the composition, MnSi 2 .1-x and manganese silicide having a composition of (0≤x≤0.2) Based compound.
Experimental Example 2.
In order to confirm the structure of the thermoelectric material according to the present invention, high-resolution transmission electron microscopy (HRTEM, JEM-2100F) was performed on the thermoelectric materials prepared in Example 1 and Comparative Example 1, The results for the material are shown in Fig.
Referring to FIG. 3, it was confirmed that the thermoelectric material produced in Example 1 had a thin film shape formed on a silicon wafer having a Miller index of [1,1,1]. Also, it was confirmed that the thin film had a thin film shape of a polycrystalline structure with uniformly oriented crystals having a uniform orientation, and the directionality thereof progressed along the lattice direction of the silicon wafer. In contrast, the thermoelectric material prepared in Comparative Example 1 had a low deposition temperature and a small deposition amount on the substrate. This means that the reactivity between silicon and manganese is reduced at low temperatures.
Experimental Example 3.
The electrical resistivity and the Seebeck coefficient of the thermoelectric material prepared in Example 1 were measured to evaluate physical properties related to the thermoelectric effect of the thermoelectric material according to the present invention. Specifically, the thermoelectric material of Example 1 was cut into a size of 5 mm × 5 mm, and the electrical resistivity of the cut material was measured in the range of 0 to 420 K using the 4-probe method. In addition, the Seebeck coefficient was measured using a method of measuring the thermal electromotive force generated by giving a temperature difference to both ends of the material. Furthermore, the power factor (S 2 σ) was derived from the electrical resistivity (1 / σ) and the Seebeck coefficient (S) of the measured material and the hole concentration, ie, carrier concentration, of the thermoelectric material was measured. The measured results are shown in Tables 4, 4 and 5.
As shown in Table 4, Figs. 4 and 5, it can be seen that the thermoelectric material according to the present invention exhibits excellent thermoelectric properties.
Specifically, it was confirmed that the thermoelectric material prepared in Example 1 had an electrical resistivity of 2.08 × 10 -3 Ω · cm and a Seebeck coefficient of 107.84 μV / K at 410 K. The electrical resistivity and the Seebeck coefficient showed that the output factor was 5.6 × 10 -4 W / K 2 m and the carrier concentration was 7.30 × 10 20 / cm 3 , indicating that the thermoelectric performance index of the thermoelectric material was about 0.5 .
Here, the thermoelectric material produced in Example 1, and the output parameter value corresponding to the output factor of the thermoelectric material comprising a compound of the composition Mn 4 Si 7 (MnSi 1 .75 ) having a high Seebeck coefficient of the manganese silicide-based composition shown since it can be seen that as compared with the thermal transfer material comprising a compound having a composition Mn 4 Si 7 (MnSi 1 .75 ) indicating a similar thermal properties. Also, it can be seen that the thermoelectric material exhibits the behavior of the p-type semiconductor because the anti-Seebeck coefficient has a positive value. From this, it can be seen that many carriers in the material are holes. Further, the thermoelectric material is a degenerate semiconductor exhibiting a semimetal characteristic because the electrical resistivity increases as the temperature increases below 500K.
Thus, by having the high thermal conductive material according to the invention, through a molecular beam epitaxy when MnSi 2 .1-x (0≤x≤0.2) the composition has a form of a thin film consisting of crystals of manganese silicide based compound in thermal properties It is useful for thermoelectric devices used in cooling systems such as LED, water purifier, and small refrigerator.
Claims (10)
A thermoelectric material having a thin film form of polycrystalline structure in which crystals of the compound are regularly arranged:
[Chemical Formula 1]
MnSi 2 .1-x (0≤x≤0.2) .
Wherein the average output factor (S 2 σ) of the thermoelectric material is 1.00 × 10 -4 W / k 2 · m or more.
The thermoelectric performance of the thermoelectric material is 0.4 or more.
A compound represented by the following general formula (1)
And forming a thin film of a polycrystalline structure in which crystals of the compound are regularly arranged.
[Chemical Formula 1]
MnSi 2 .1-x (0≤x≤0.2) .
Wherein the deposition is performed by a molecular beam epitaxy method.
Wherein the deposition pressure is 10 -7 to 10 -10 Torr.
Wherein the deposition temperature is 773 to 973K.
Wherein the deposition rate is 0.1 to 2 ANGSTROM / s.
Prior to the step of forming the thin film,
A method for manufacturing a thermoelectric material, comprising the steps of:
A thermoelectric material having a thin film form of a polycrystalline structure in which crystals of the compound are regularly arranged; And
A thermoelectric element further comprising a substrate containing silicon (Si) on one surface of a thin film thermoelectric material:
[Chemical Formula 1]
MnSi 2 .1-x (0≤x≤0.2) .
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| JP2007042963A (en) * | 2005-08-05 | 2007-02-15 | Toyota Central Res & Dev Lab Inc | Thermoelectric material and its manufacturing method |
| KR20110041510A (en) * | 2008-07-11 | 2011-04-21 | 꼼미사리아 아 레네르지 아또미끄 에 오 에네르지 알떼르나띠브스 | Sige matrix nanocomposite materials with an improved thermoelectric figure of merit |
| KR20140019086A (en) | 2012-07-27 | 2014-02-14 | 한국교통대학교산학협력단 | Synthesizing method of higher manganese silicides thermoelectric material and higher manganese silicides thermoelectric material synthesized by the method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2007042963A (en) * | 2005-08-05 | 2007-02-15 | Toyota Central Res & Dev Lab Inc | Thermoelectric material and its manufacturing method |
| KR20110041510A (en) * | 2008-07-11 | 2011-04-21 | 꼼미사리아 아 레네르지 아또미끄 에 오 에네르지 알떼르나띠브스 | Sige matrix nanocomposite materials with an improved thermoelectric figure of merit |
| KR20140019086A (en) | 2012-07-27 | 2014-02-14 | 한국교통대학교산학협력단 | Synthesizing method of higher manganese silicides thermoelectric material and higher manganese silicides thermoelectric material synthesized by the method |
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