WO2023190437A1 - セラミックス - Google Patents

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WO2023190437A1
WO2023190437A1 PCT/JP2023/012374 JP2023012374W WO2023190437A1 WO 2023190437 A1 WO2023190437 A1 WO 2023190437A1 JP 2023012374 W JP2023012374 W JP 2023012374W WO 2023190437 A1 WO2023190437 A1 WO 2023190437A1
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electrocaloric effect
ceramic
temperature
satisfied
voltage
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French (fr)
Japanese (ja)
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左京 廣瀬
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Murata Manufacturing Co Ltd
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Murata Manufacturing Co Ltd
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Priority to JP2024512513A priority Critical patent/JP7718583B2/ja
Priority to DE112023000459.5T priority patent/DE112023000459T5/de
Priority to CN202380021621.5A priority patent/CN118679134A/zh
Publication of WO2023190437A1 publication Critical patent/WO2023190437A1/ja
Priority to US18/780,844 priority patent/US20240376014A1/en
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Definitions

  • the present disclosure relates to ceramics.
  • PbSc 0.5 Ta 0.5 O 3 (hereinafter, ceramics containing Pb, Sc, and Ta are also referred to as "PST”) is known as the most promising material.
  • PST PbSc 0.5 Ta 0.5 O 3
  • Non-Patent Documents 1 to 3 report that PbSc 0.5 Ta 0.5 O 3 exhibits a large electrocaloric effect.
  • Solid-state cooling elements are required to exhibit a large electrocaloric effect at temperatures appropriate for their use. For example, when a solid cooling element is used in a refrigerator or the like, it may be required to exhibit a large electric heating effect at temperatures below 4°C.
  • the withstand voltage of the PST is improved, it will be possible to apply a larger voltage, and the electric heat amount effect will be improved. Furthermore, the higher the degree of order of Sc and Ta, which are cations at the B site of PST, the better the ferroelectric properties can be obtained, and the electrocaloric effect can be improved.
  • PST in which a part of Pb is partially replaced with Na, has an improved withstand voltage, making it possible to apply a high voltage, and also making it possible to control the ferroelectric transition temperature to 20°C or less.
  • the electrocaloric effect at low temperatures has been improved because the degree of site order can be easily increased, the effect is limited and further improvements are desired.
  • the present disclosure aims to provide ceramics that exhibit a greater electrocaloric effect at lower temperatures than before.
  • the present disclosure provides formula (1): (1-m) PbSc 0.5-x Ta 0.5+x O 3 -mPbMg 0.5-y W 0.5+y O 3 (1)
  • medium, m satisfies 0.03 ⁇ m ⁇ 0.60, In the case of 0 ⁇ x, y, x, y ⁇ 0.1 and 0 ⁇ x+y ⁇ 0.13 are satisfied, If 0>x, 0 ⁇ y, -0.1 ⁇ x ⁇ 0 and 0 ⁇ y ⁇ 0.1, If 0 ⁇ x, 0>y, -0.1 ⁇ x,y and -0.13 ⁇ x+y ⁇ 0, In the case of 0 ⁇ x,0>y, 0 ⁇ x ⁇ 0.1 and ⁇ 0.1 ⁇ y ⁇ 0 are satisfied.
  • Formula (1) (1-m) PbSc 0.5-x Ta 0.5+x O 3 -mPbMg 0.5-y W 0.5+y O 3 (1)
  • m satisfies 0.03 ⁇ m ⁇ 0.60, In the case of 0 ⁇ x, y, x, y ⁇ 0.1 and 0 ⁇ x+y ⁇ 0.13 are satisfied, If 0>x, 0 ⁇ y, -0.1 ⁇ x ⁇ 0 and 0 ⁇ y ⁇ 0.1, If 0 ⁇ x, 0>y, -0.1 ⁇ x,y and -0.13 ⁇ x+y ⁇ 0, In the case of 0 ⁇ x,0>y, 0 ⁇ x ⁇ 0.1 and ⁇ 0.1 ⁇ y ⁇ 0 are satisfied.
  • the present disclosure it is possible to provide ceramics that exhibit a large electrocaloric effect at low temperatures. More specifically, it is possible to provide ceramics that exhibit a large electrocaloric effect even at temperatures below 0°C.
  • FIG. 1 is a schematic cross-sectional view of an electrocaloric effect element according to an embodiment of the present disclosure.
  • FIG. 2 is a diagram for explaining the measurement sequence of the electrocaloric effect.
  • FIG. 3 is a diagram showing the measurement results of the electrocaloric effect of samples Nos. 1 and 6 in the example.
  • FIG. 4 is a diagram showing the results of characteristic tests for various x and y compositions.
  • the ceramic according to an embodiment of the present disclosure has Pb, Sc, Ta, Mg, and W as main components.
  • the ceramic is a composite oxide containing Pb, Sc, Ta, Mg, and W,
  • the content ratio of Pb is substantially equal to the total content ratio of Sc, Ta, Mg, and W,
  • the content ratio of Sc is "0.5-x”
  • the content ratio of Ta is "0.5+x”
  • the content ratio of Mg is "0.5-y”
  • the content ratio of W is The ratio is "0.5+y”
  • the range of x and y is In the case of 0 ⁇ x, y, x, y ⁇ 0.1 and 0 ⁇ x+y ⁇ 0.13 are satisfied, If 0>x, 0 ⁇ y, -0.1 ⁇ x ⁇ 0 and 0 ⁇ y ⁇ 0.1, If 0 ⁇ x, 0>y, -0.1 ⁇ x,y and -0.13 ⁇ x+y ⁇ 0, In the case of 0 ⁇ x,0>y, 0 ⁇ x ⁇ 0.1 and
  • the above-mentioned "the content ratio of Pb is substantially equal to the total content ratio of Sc, Ta, Mg, and W” means the content ratio of Pb and the total content of Sc, Ta, Mg, and W. It is not limited to the case where the ratios are completely equal.
  • the content ratio of Pb is substantially equal to the total content ratio of Sc, Ta, Mg, and W means that the content ratio of Pb is the same as the total content ratio of Sc, Ta, Mg, and W. This also includes cases where the difference in molar ratio is within 3%, for example.
  • composition of the ceramic of the present disclosure can be analyzed and measured by performing a composition analysis using, for example, high-frequency inductively coupled plasma emission spectroscopy, fluorescent X-ray analysis, or the like.
  • the electrocaloric effect is an absorption and heat generation phenomenon caused by a change in entropy when the electric dipole moments in a substance are aligned or disordered due to a change in the electric field.
  • the performance index of the electrocaloric effect in the present invention may be an adiabatic temperature change ( ⁇ T).
  • ⁇ T adiabatic temperature change
  • the electric calorie effect is large may mean that the adiabatic temperature change ( ⁇ T) is large.
  • the larger the adiabatic temperature change ( ⁇ T) the more preferable.
  • Adiabatic temperature change means a temperature change in ceramics caused by applying an electric field to the ceramics and/or removing the electric field applied to the ceramics. Specifically, it may be the difference between the temperature of the ceramic before the electric field is applied and the temperature of the ceramic immediately after the electric field is applied, or the difference between the temperature of the ceramic before the electric field is removed and the temperature of the ceramic immediately after the electric field is removed. It may be a difference from the temperature of ceramics.
  • the adiabatic temperature change ⁇ T increases as the electric field strength applied to the ceramic increases. Further, the adiabatic temperature change ⁇ T increases as the temperature of the ceramic approaches the ferroelectric transition temperature (hereinafter also referred to as "phase transition temperature") when an electric field is applied. For example, as the temperature of the ceramic becomes lower than the transition temperature, the electrocaloric effect decreases rapidly. Specifically, in conventional PST, which has a transition temperature of about 15 to 25°C, the electrocaloric effect is significantly reduced when the temperature of the ceramic is 0°C or lower.
  • the ceramic has the formula (1): (1-m) PbSc 0.5-x Ta 0.5+x O 3 -mPbMg 0.5-y W 0.5+y O 3 (1)
  • m satisfies 0.03 ⁇ m ⁇ 0.60, In the case of 0 ⁇ x, y, x, y ⁇ 0.1 and 0 ⁇ x+y ⁇ 0.13 are satisfied, If 0>x, 0 ⁇ y, -0.1 ⁇ x ⁇ 0 and 0 ⁇ y ⁇ 0.1, If 0 ⁇ x, 0>y, -0.1 ⁇ x,y and -0.13 ⁇ x+y ⁇ 0, In the case of 0 ⁇ x,0>y, 0 ⁇ x ⁇ 0.1 and ⁇ 0.1 ⁇ y ⁇ 0 are satisfied.
  • It may be a ceramic represented by
  • x, y, and m within the above ranges, a large electrocaloric effect at low temperatures (for example, ⁇ T of 1.5 K or more when an electric field strength of 15 MV/m is applied) can be obtained.
  • PbMg 0.5 W 0.5 O 3 is an antiferroelectric material, and has a characteristic that it transforms into a ferroelectric material by applying a voltage equal to or higher than a threshold voltage.
  • a threshold voltage Generally, it is known that the larger the difference in ionic radius between two cations at the B site, the easier they are to align, and the B site is easier to align in PMW than in PST.
  • Ferroelectricity is greatly affected by the degree of alignment of the B sites, so by adding PMW to PST, which makes it easy for the B sites to align, the ferroelectric transition temperature can be lowered without significantly reducing the ferroelectricity. As a result, it is considered that an excellent electric heating effect was obtained at temperatures below 0°C.
  • the production of PST requires firing at a high temperature of 1,400°C, and in addition, after firing, heat treatment at a high temperature of 1,000°C for 1,000 hours is essential.
  • the ceramics within the scope of the present invention do not require long-term heat treatment, significantly improving productivity, and can be fired at temperatures below 1250°C, which significantly reduces wear and tear on the furnace body, setter, sheath, etc. during manufacturing. It becomes possible to suppress this.
  • the range of x and y is In the case of 0 ⁇ x, y, x, y ⁇ 0.1 and 0 ⁇ x+y ⁇ 0.12 are satisfied, If 0>x, 0 ⁇ y, -0.1 ⁇ x ⁇ 0 and 0 ⁇ y ⁇ 0.1, If 0 ⁇ x, 0>y, -0.1 ⁇ x,y and -0.12 ⁇ x+y ⁇ 0, In the case of 0 ⁇ x,0>y, 0 ⁇ x ⁇ 0.1 and ⁇ 0.1 ⁇ y ⁇ 0 are satisfied.
  • the range of x and y is In the case of 0 ⁇ x, y, x, y ⁇ 0.1 and 0 ⁇ x+y ⁇ 0.11 are satisfied, If 0>x, 0 ⁇ y, -0.1 ⁇ x ⁇ 0 and 0 ⁇ y ⁇ 0.1, If 0 ⁇ x, 0>y, -0.1 ⁇ x,y and -0.11 ⁇ x+y ⁇ 0, In the case of 0 ⁇ x,0>y, 0 ⁇ x ⁇ 0.1 and ⁇ 0.1 ⁇ y ⁇ 0 are satisfied.
  • the range of x and y is In the case of 0 ⁇ x,y, 0 ⁇ x+y ⁇ 0.1 is satisfied, If 0>x, 0 ⁇ y, -0.1 ⁇ x ⁇ 0 and 0 ⁇ y ⁇ 0.1, If 0 ⁇ x, 0>y, satisfy -0.1 ⁇ x+y ⁇ 0, In the case of 0 ⁇ x,0>y, 0 ⁇ x ⁇ 0.1 and ⁇ 0.1 ⁇ y ⁇ 0 are satisfied.
  • the range of x and y is In the case of 0 ⁇ x,y, 0 ⁇ x+y ⁇ 0.08 is satisfied, If 0>x, 0 ⁇ y, satisfy -0.08 ⁇ x ⁇ 0 and 0 ⁇ y ⁇ 0.08, If 0 ⁇ x, 0>y, satisfy -0.08 ⁇ x+y ⁇ 0, In the case of 0 ⁇ x, 0>y, 0 ⁇ x ⁇ 0.08 and ⁇ 0.08 ⁇ y ⁇ 0 are satisfied.
  • the range of x and y is In the case of 0 ⁇ x,y, satisfy 0 ⁇ x ⁇ 0.05 and 0 ⁇ y ⁇ 0.05, If 0>x, 0 ⁇ y, satisfy -0.05 ⁇ x ⁇ 0 and 0 ⁇ y ⁇ 0.05, If 0 ⁇ x, 0>y, satisfy -0.05 ⁇ x ⁇ 0 and -0.05 ⁇ y ⁇ 0, In the case of 0 ⁇ x,0>y, 0 ⁇ x ⁇ 0.05 and ⁇ 0.05 ⁇ y ⁇ 0 are satisfied.
  • the range of x and y is In the case of 0 ⁇ x,y, 0 ⁇ x+y ⁇ 0.05 is satisfied, If 0>x, 0 ⁇ y, satisfy -0.05 ⁇ x ⁇ 0 and 0 ⁇ y ⁇ 0.05, If 0 ⁇ x, 0>y, -0.05 ⁇ x+y ⁇ 0, In the case of 0 ⁇ x,0>y, 0 ⁇ x ⁇ 0.05 and ⁇ 0.05 ⁇ y ⁇ 0 are satisfied.
  • the ranges of x and y include the above-mentioned "0 ⁇ x, y", “0>x, 0 ⁇ y”, “ ⁇ x, 0>y”, and The range may be determined by arbitrarily combining the ranges of x and y in the case of 0 ⁇ x, 0>y.
  • x and y are 0. That is, the formula represented by (1-m)PbSc 0.5-x Ta 0.5+x O 3 -mPbMg 0.5-y W 0.5+y O 3 is (1-m)PbSc 0.5 Ta 0 .5 O 3 -mPbMg 0.5 W 0.5 O 3 .
  • the range of m is preferably 0.05 ⁇ m ⁇ 0.5, more preferably 0.05 ⁇ m ⁇ 0.4, and even more preferably 0.05 ⁇ . m ⁇ 0.3.
  • the crystal structure of the ceramic according to one embodiment of the present invention may be a perovskite structure.
  • Ceramics having a perovskite structure include not only ceramics having a "perovskite-type crystal structure” but also ceramics having a "perovskite-type crystal structure".
  • a ceramic having a perovskite structure may have a crystal structure that can be recognized as a perovskite crystal structure by a person skilled in the ceramics field in X-ray diffraction.
  • the electrocaloric effect element of the present disclosure has a laminate in which electrode layers and ceramic layers containing the ceramic of the present disclosure as a main component are alternately laminated.
  • an electrocaloric effect element 1 includes electrode layers 2a and 2b (hereinafter also collectively referred to as "electrode layers 2") and a ceramic layer 4 that are alternately laminated. It has a laminate 6 and external electrodes 8a and 8b (hereinafter also collectively referred to as “external electrodes 8") connected to the electrode layer 2.
  • the electrode layers 2a and 2b are electrically connected to external electrodes 8a and 8b arranged on the end faces of the laminate 6, respectively.
  • the electrode layer 2 is a so-called internal electrode. In addition to the function of applying an electric field to the ceramic layer 4, the electrode layer 2 may also have the function of transporting heat between the ceramic layer 4 and the outside.
  • the above electrode layer may be an electrode layer whose main component is a noble metal.
  • the "main component" in the electrode layer means that the electrode layer consists of 80% by mass or more of a noble metal, for example, 95% by mass or more of the electrode layer, more preferably 98% by mass or more, and even more preferably means that 99% or more, even more preferably 99.5% by mass or more, particularly preferably 99.9% by mass or more is noble metal.
  • the "noble metal” may be, for example, Au, Ag, Pt, or Pd.
  • the main component of the electrode layer used in the present disclosure may be Pt or Pd. That is, it may be a Pt or Pd electrode layer.
  • the noble metal electrode layer may be an alloy or mixture of Pt and/or Pd and other elements (for example, Ag, Pd, Rh, Au, etc.). Good too.
  • the alloy may be an Ag-Pd alloy. Similar effects can be obtained even if the Pt or Pd electrode layer is composed of an alloy or a mixture thereof. It may also contain other elements that may be mixed in as impurities, particularly unavoidable elements (eg, Fe, Al 2 O 3 , etc.). In this case as well, similar effects can be obtained.
  • the thickness of the electrode layer 2 is preferably 0.2 ⁇ m or more and 10 ⁇ m or less, more preferably 1.0 ⁇ m or more and 5.0 ⁇ m or less, for example, 2.0 ⁇ m or more and 5.0 ⁇ m or less, or 2.0 ⁇ m or more and 4.0 ⁇ m or less. .
  • the thickness of the electrode layer By setting the thickness of the electrode layer to 0.5 ⁇ m or more, the resistance of the electrode layer can be reduced and the heat transport efficiency can be increased. Further, by setting the thickness of the electrode layer to 10 ⁇ m or less, the thickness (and thus the volume) of the ceramic layer can be increased, and the amount of heat that can be handled by the electric calorie effect of the entire device can be increased. Furthermore, the element can be made smaller.
  • the ceramic layer 4 may contain one type of ceramic as a main component, or may contain two or more types of ceramics as a main component.
  • the "main component" in the ceramic layer means that the ceramic layer essentially consists of the target ceramic, for example, 90% by mass or more, more preferably 95% or more, even more preferably 95% or more by mass of the ceramic layer. This means that 98% by mass or more, even more preferably 99% by mass or more, particularly preferably 99.5% by mass or more is the subject ceramic.
  • Other components may include a crystalline phase having a structure different from the perovskite structure called a pyrochlore structure, other elements mixed as impurities, and particularly unavoidable elements (for example, Zr, C, etc.).
  • the composition of the ceramic layer 4 can be determined by high-frequency inductively coupled plasma emission spectroscopy, fluorescent X-ray analysis, or the like. Further, the structure of the ceramic layer 4 can be determined by powder X-ray diffraction.
  • the thickness of the ceramic layer 4 is preferably 5 ⁇ m or more and 100 ⁇ m or less, more preferably 5 ⁇ m or more and 50 ⁇ m or less, even more preferably 10 ⁇ m or more and 50 ⁇ m or less, even more preferably 20 ⁇ m or more and 50 ⁇ m or less, and particularly preferably 20 ⁇ m or more and 40 ⁇ m or less. .
  • the amount of heat that the element can handle can be increased.
  • By making the thickness of the ceramic layer thinner a higher ⁇ T can be obtained. Furthermore, withstand voltage can also be improved.
  • the withstand voltage of the ceramic layer 4 may be preferably 15 MV/m or more, more preferably 20 MV/m or more, even more preferably 25 MV/m or more. By increasing the withstand voltage of the ceramic layer, a larger voltage (electric field) can be applied, and a larger ⁇ T can be obtained.
  • Materials constituting the pair of external electrodes 8a, 8b include, but are not limited to, Ag, Cu, Pt, Ni, Al, Pd, Au, or alloys thereof (for example, Ag-Pd, etc.).
  • the electrode may be made of metal and glass or may be made of metal and resin. Among the metals, Ag is preferred.
  • the electrode layers 2 and the ceramic layers 4 are alternately laminated, but in the electrocaloric effect element of the present disclosure, the number of laminated electrode layers and ceramic layers is not particularly limited. Further, all of the internal electrodes do not need to be connected to external electrodes, and internal electrodes that are not connected to external electrodes may be included as necessary for heat transfer or stress relaxation due to piezoelectricity or electrostriction.
  • the internal electrode and the ceramic layer are in contact with each other on substantially the entire surface, but the electrocaloric effect element of the present disclosure is not limited to such a structure, and a voltage (electric field) is applied to the ceramic layer. It is not particularly limited as long as it has a structure that can apply .
  • the electrocaloric effect element 1 has a rectangular parallelepiped block shape, the shape of the electrocaloric effect element of the present disclosure is not limited to this, and may be, for example, cylindrical or sheet-like, and may also have unevenness or through holes. etc. may be included.
  • internal electrodes may be exposed on the surface for heat transport and heat exchange with the outside.
  • the ceramics and electrocaloric effect element of this embodiment described above are manufactured, for example, as follows.
  • high-purity lead oxide (Pb 3 O 4 ), tantalum oxide (Ta 2 O 5 ), scandium oxide (Sc 2 O 3 ), magnesium carbonate (MgCO 3 ), and tungsten oxide (WO 3 )) were calcined. Afterwards, it is weighed to obtain the desired composition ratio.
  • the above raw materials are pulverized and mixed with partially stabilized zirconia (PSZ) balls, pure water, a dispersant, etc. in a ball mill. Thereafter, the pulverized and mixed slurry is dried, sized, and then calcined, for example, at 800° C. to 900° C.
  • PSZ partially stabilized zirconia
  • the obtained calcined powder is mixed with PSZ balls, ethanol, toluene, a dispersant, etc., and pulverized.
  • a binder solution dissolved in the obtained pulverized powder is added and mixed to prepare a slurry for sheet molding.
  • the prepared slurry is formed into a sheet on a support, and a Pt electrode paste is printed on it.
  • the green chips are heat-treated at 500°C to 600°C in the atmosphere to remove the binder.
  • the binder-removed chip is fired at 1000° C.
  • the electrocaloric effect element of the present disclosure exhibits an excellent electrocaloric effect, it can be used as a heat management element, especially a cooling element (including cooling/heat pump elements for air conditioners such as air conditioners, refrigerators, and freezers).
  • a cooling element including cooling/heat pump elements for air conditioners such as air conditioners, refrigerators, and freezers.
  • the present disclosure also provides an electronic component comprising the electrocaloric effect element of the present disclosure, and an electronic device comprising the electrocaloric effect element or electronic component of the present disclosure.
  • Examples of electronic components include, but are not limited to, electronic components used in air conditioners, refrigerators, or freezers, or electronic components used in air conditioning of electric vehicles and hybrid cars (e.g., batteries); central processing units (CPUs); , integrated circuits (ICs) such as hard disks (HDDs), power management ICs (PMICs), power amplifiers (PAs), transceiver ICs, and voltage regulators (VRs), light-emitting elements such as light-emitting diodes (LEDs), incandescent light bulbs, and semiconductor lasers.
  • components that can be heat sources such as field effect transistors (FETs), and other components such as lithium ion batteries, substrates, heat sinks, casings, and other components commonly used in electronic devices.
  • FETs field effect transistors
  • Examples of electronic devices include, but are not limited to, air conditioners, refrigerators, or freezers; air conditioners used as heat pumps, air conditioners for electric vehicles or hybrid cars, mobile phones, smartphones, personal computers (PCs), tablet terminals, and hard disk drives. Examples include small electronic devices such as drives and data servers.
  • the electrocaloric element of the present disclosure can be used as a thermal management system (or temperature management system) that manages heat (temperature) of the electronic component and the electronic device.
  • thermal management system or temperature management system
  • examples of the thermal management system include a cooling system that cools the electronic components and electronic equipment.
  • the obtained calcined powder was mixed with PSZ balls having a diameter of 5 mm, ethanol, toluene, and a dispersant for 16 hours, and then pulverized.
  • a dissolved binder solution was added to the obtained pulverized powder and mixed for 4 hours to prepare a slurry for sheet molding.
  • the produced slurry was formed into a sheet shape with a thickness corresponding to the thickness of a predetermined ceramic layer on a PET film by a doctor blade method, and after cutting into strips, a platinum internal electrode paste was screen printed. Note that the sheet thickness of the laminated element to be produced was controlled by changing the gap of the doctor blade used during sheet forming.
  • a green chip was produced by laminating a predetermined number of sheets printed with platinum internal electrode paste and sheets without printing, then press-bonded with a pressure of 150 MPa, and cut. The green chips were heat-treated at 550° C. for 24 hours in the air to remove the binder. Next, the green chip was sealed in an alumina sealed sheath together with PbZrO 3 powder for creating a Pb atmosphere, and fired at 1150 to 1400° C. for 4 hours. Sample number 1 as a comparative example shown in Table 1 was fired at a high temperature of 1400°C and then heat treated at 1000°C for 1000 hours.
  • the size of the obtained element was approximately L10.2 mm x W7.2 mm x T0.88 for an element in which the thickness of the ceramic layer was 40 ⁇ m.
  • the number of ceramic layers sandwiched between the internal electrode layers was 19, the electrode area was 49 mm 2 /layer, and the total electrode area was 49 mm 2 ⁇ 19 layers.
  • the thickness of the ceramic layer of the element obtained above was confirmed using a scanning electron microscope after cross-sectional polishing of the element.
  • composition The ceramic composition of the obtained element was confirmed using high frequency inductively coupled plasma emission spectroscopy and fluorescent X-ray analysis.
  • Crystal structure In order to evaluate the crystal structure of the obtained device, powder X-ray diffraction measurement was performed. One element was randomly selected from each lot, ground in a mortar, and then an X-ray diffraction profile was obtained. From the obtained X-ray diffraction profile, it was confirmed whether the crystal structure of the ceramic was a perovskite structure, and the presence or absence and abundance ratio of impurity phases (mainly pyrochlore phase) were estimated from the intensity ratio. When the abundance ratio of perovskite structure was 0.95 or more, it was determined that the main component had a perovskite structure, and when it was less than 0.95, it was determined that there was a different phase.
  • the electrocaloric effect was evaluated by applying voltage to the sample in the sequence shown in the upper graph of FIG. That is, first, a voltage was applied to the sample, the voltage was maintained as it was, then the applied voltage was removed and the voltage was maintained as it was, and this operation was repeated to measure changes in the electrocaloric effect.
  • voltage is applied in this sequence, in the step of applying voltage, the sample temperature rises at the same time as the voltage is applied, and in the step of maintaining the applied state, the heat is gradually diffused and the sample temperature remains the same as before voltage application.
  • the sample temperature decreases simultaneously with the removal, and in the process of maintaining the non-applied state, the sample temperature gradually increases to the original temperature.
  • the adiabatic temperature change ⁇ T is determined from the temperature change when the above voltage is applied and removed. Specifically, in this example, after applying a voltage of 15 MV/m, the temperature was measured by holding the applied voltage for 50 seconds, and then after removing the voltage, the temperature was measured by holding the voltage in a non-applied state for 50 seconds. did. This sequence was repeated three times. During the sequence of voltage application and voltage removal, the temperature of the element was constantly measured, and the adiabatic temperature change ⁇ T was determined from the temperature change. In addition, cases where the absolute value of the adiabatic temperature change ⁇ T at -10°C and 0°C were each 1.5K or more were judged as Go. The results are shown in Tables 1 to 4.
  • sample number 1 which is a conventional PST ceramic and has a composition of PbSc 0.5 Ta 0.5 O 3 , has an adiabatic temperature change of 1.5 K or more in a temperature range of 20°C or more. It was confirmed that it exhibited an excellent electrocaloric effect.
  • Sample No. 1 is suitable for driving at room temperature or higher. However, as shown in Table 1, in sample No. 1, the adiabatic temperature change at 0°C and -10°C is smaller than 1.5K, confirming that the electrocaloric effect is significantly reduced at low temperatures. Ta.
  • samples Nos. 3 to 8 having compositions within the range of the present invention had adiabatic temperature changes of more than 1.5K at 0°C and -10°C.
  • sample No. 6 had an excellent adiabatic temperature change of 2K or more over a wide temperature range from 20°C to -40°C.
  • sample number 2 where the value of m is outside the range of the present invention, an excellent electrocaloric effect is obtained at temperatures above 0°C, but the electrocaloric effect at 0°C and -10°C is 0.9 K and It was small at 0.3K. This is considered to be because the value of m is small and the ferroelectric transition temperature of the ceramic is not lowered sufficiently.
  • substances having the desired crystal structure were most stable when both x and y were near 0 and could be obtained at a rate close to 100%. Even when both x and y are not near 0, no foreign phase is generated, but when they deviate significantly from 0, the proportion of foreign phases increases (see the crystal structure column of Tables 2 to 4).
  • the change in adiabatic heat value at 0°C and -10°C was 1.5K or more.
  • FIG. 4 shows the composition ranges of x and y in Table 2 that were determined to be Go as a result of the characteristic test. From FIG. 4, it can be seen that ceramics within the scope of the present invention are judged as Go in the characteristic test. Tables 3 and 4 also show the same results as FIG. 4.
  • the electrocaloric effect element of the present disclosure can exhibit a high electrocaloric effect, it can be used, for example, in electric vehicles or hybrid cars, air conditioners (e.g., air conditioners used in electric cars or hybrid cars, air conditioners used as heat pumps, etc.), refrigerators, etc. It can also be used as a heat management element in a freezer, etc., and can also be used in various electronic devices, such as small electronic devices such as mobile phones, smartphones, tablet terminals, hard disk drives, or data servers, where heat countermeasure problems are becoming more prominent. Alternatively, it can be used as a cooling device for a personal computer (PC) or the like.
  • PC personal computer
  • Electrocaloric effect element 2a, 2b Electrode layer 4
  • Ceramic layer 6 Ceramic layer 6
  • Laminated body 8a, 8b External electrode

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WO2016194700A1 (ja) * 2015-06-04 2016-12-08 株式会社村田製作所 冷却デバイス
JP2017110838A (ja) * 2015-12-15 2017-06-22 株式会社村田製作所 熱搬送デバイス
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JP2017110838A (ja) * 2015-12-15 2017-06-22 株式会社村田製作所 熱搬送デバイス
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