Classifications

• • 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
  • C04B35/16—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 silicates other than clay
  • C04B35/18—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 silicates other than clay rich in aluminium oxide
  • C04B35/195—Alkaline earth aluminosilicates, e.g. cordierite or anorthite
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
  • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
  • H01B3/02—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
  • H01B3/12—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances ceramics

Definitions

• the present invention relates to a cordierite sintered body and a method for producing the same.
• cordierite sintered bodies have been used, for example, as components exposed to plasma (Patent Document 1).
• the present invention was made in consideration of the above points, and aims to provide a new cordierite sintered body and a method for producing the same.
• the present invention provides the following [1] to [15].
• cordierite sintered body according to any one of [1] to [11] above wherein the yttrium content is 0.2 mass% or more in terms of oxide.
• the cordierite sintered body according to any one of [1] to [12] above having a four-point bending strength of 170 MPa or more.
• a method for producing the cordierite sintered body according to any one of the above [1] to [13], comprising the steps of: preparing a molded body using a raw material powder; heating the molded body; and using, as the raw material powder, a mixed powder containing cordierite powder produced by an electric melting method, mullite powder, and magnesium oxide powder.
• the present invention provides a novel cordierite sintered body and a method for producing the same.
• a numerical range expressed using “to” means a range that includes the numerical values before and after “to” as the lower and upper limits.
• the cordierite sintered body of the present embodiment contains at least calcium, magnesium, aluminum, and silicon among elements belonging to an element group M1 consisting of calcium, magnesium, aluminum, yttrium, and silicon.
• the silicon content is 44.0 mass% or more and 53.0 mass% or less, calculated as oxide.
• the calcium content is 2.0 mass% or less, calculated as oxide.
• the yttrium content is 7.0 mass% or less, calculated as oxide.
• the content of element M2, which is a metal element other than the elements belonging to the element group M1, is 2.5 mass% or less, calculated as oxide.
• the dielectric loss tangent at 20 GHz is 0.00100 or less.
• the cordierite sintered body will be referred to simply as the "sintered body,” and the cordierite sintered body of this embodiment will be referred to as the “sintered body.”
• the present sintered body is a sintered body of metal oxides containing cordierite.
• An example of the chemical formula representing cordierite is, but is not limited to , 2MgO.2Al2O3.5SiO2 .
• the present sintered body contains, in addition to cordierite ( 2MgO.2Al2O3.5SiO2 ), calcium (Ca) but in a small amount.
• the present sintered body contains a small amount of metal elements (element M2 described later) other than Ca and magnesium ( Mg ).
• Such a sintered body has a small dielectric tangent at 20 GHz.
• the present sintered body will be described in more detail below. In the following, the dielectric tangent at 20 GHz and the dielectric tangent at 10 GHz will be collectively referred to simply as the "dielectric tangent".
• Element group M1 The element group consisting of calcium (Ca), magnesium (Mg), aluminum (Al), yttrium (Y) and silicon (Si) is referred to as "element group M1".
• the present sintered body further contains Ca in addition to cordierite (2MgO.2Al 2 O 3.5SiO 2 ). Therefore, the present sintered body contains at least Ca, Mg, Al and Si among the elements belonging to the element group M1.
• the Ca content is 2.0 mass% or less, preferably 1.0 mass% or less, more preferably 0.7 mass% or less, even more preferably 0.4 mass% or less, even more preferably 0.2 mass% or less, particularly preferably 0.15 mass% or less, more particularly preferably 0.1 mass% or less, very preferably 0.05 mass% or less, and most preferably 0.01 mass% or less.
• the Ca content, calculated as an oxide is more than 0 mass%, preferably 0.02 mass% or more, and more preferably 0.05 mass% or more.
• the content of Ca calculated as oxide specifically means the content of CaO.
• the Mg content, calculated as the oxide is preferably 15.0 mass % or less, more preferably 14.5 mass % or less, even more preferably 14.0 mass % or less, particularly preferably 13.5 mass % or less, and most preferably 13.0 mass % or less.
• the Mg content, calculated as an oxide is preferably 11.0 mass % or more, more preferably 12.0 mass % or more, and even more preferably 12.5 mass % or more.
• the content of Mg calculated as oxide specifically means the content of MgO.
• the Al content, calculated as oxide is preferably 33.0 mass% or more, more preferably 34.0 mass% or more, even more preferably 35.0 mass% or more, and particularly preferably 36.0 mass% or more.
• the Al content, calculated as the oxide is preferably 40.0 mass % or less, more preferably 39.0 mass % or less, and even more preferably 38.0 mass % or less.
• the content of Al calculated as oxide specifically means the content of Al 2 O 3 .
• the Si content, calculated as oxide is 44.0 mass % or more and 53.0 mass % or less. Because the dielectric tangent of the present sintered body becomes small, the Si content, calculated as the oxide, is 53.0 mass% or less, preferably 51.0 mass% or less, more preferably 50.0 mass% or less, even more preferably 49.0 mass% or less, particularly preferably 48.5 mass% or less, and most preferably 48.0 mass% or less.
• the Si content, calculated as an oxide is 44.0 mass % or more, preferably 45.0 mass % or more, and more preferably 46.0 mass % or more.
• the content of Si calculated as oxide specifically means the content of SiO2 .
• the Y content may be 0 mass %.
• the present sintered body since the present sintered body has a large four-point bending strength, it is preferable that the present sintered body contains Y.
• the content of Y, calculated as oxide is preferably 0.2 mass% or more, more preferably 1.0 mass% or more, even more preferably 1.5 mass% or more, particularly preferably 2.0 mass% or more, very preferably 2.5 mass% or more, and most preferably 3.0 mass% or more.
• the Y content is 7.0 mass% or less, calculated as an oxide.
• the Y content is preferably 6.0 mass% or less, more preferably 5.0 mass% or less, and even more preferably 4.0 mass% or less, calculated as an oxide.
• the content of Y calculated as oxide specifically means the content of Y2O3 .
• the content of element M2 which is a metal element other than the above-mentioned element group M1 is small, so that the present sintered body has a small dielectric loss tangent.
• the content of element M2 is 2.5 mass% or less, preferably 2.0 mass% or less, more preferably 1.0 mass% or less, even more preferably 0.5 mass% or less, even more preferably 0.3 mass% or less, particularly preferably 0.2 mass% or less, very preferably 0.15 mass% or less, and most preferably 0.1 mass% or less, calculated as an oxide.
• the lower limit is preferably zero.
• Element M2 may be, for example, at least one element selected from the group consisting of sodium (Na), potassium (K), strontium (Sr), titanium (Ti), phosphorus (P), chromium (Cr), manganese (Mn), iron (Fe), nickel (Ni), lanthanum (La), gallium (Ga), zirconium (Zr), zinc (Zn) and niobium (Nb).
• the total content of Na, K, Sr, Ti, P, Cr, Mn, Fe, Ni, La, Ga, Zr, Zn and Nb is preferably 3000 mass ppm or less (0.3 mass% or less) in terms of oxide, more preferably 2100 mass ppm or less, even more preferably 1600 mass ppm or less, even more preferably 1200 mass ppm or less, particularly preferably 800 mass ppm or less, and most preferably 400 mass ppm or less.
• P is not a metallic element, it is considered to be a metallic element when it is treated as element M2.
• the content of Na calculated as oxide specifically means the content of Na 2 O.
• the content of K calculated as an oxide specifically means the content of K 2 O.
• the content of Sr calculated as oxide specifically means the content of SrO.
• the content of Ti calculated as oxide specifically means the content of TiO2 .
• the content of P calculated as oxide specifically means the content of P2O5 .
• the Cr content calculated as an oxide specifically means the Cr 2 O 3 content.
• the content of Mn calculated as an oxide specifically means the content of MnO.
• the content of Fe calculated as oxide specifically means the content of Fe2O3 .
• the Ni content calculated as oxide specifically means the NiO content.
• the La content calculated as an oxide specifically means the La2O3 content.
• the Ga content calculated as oxide specifically means the Ga 2 O 3 content.
• the content of Zr calculated as an oxide specifically means the content of ZrO2 .
• the content of Zn calculated as oxide specifically means the content of ZnO.
• the content of Nb calculated as an oxide specifically
• the Fe content is preferably 2000 ppm by mass (0.2% by mass) or less, more preferably 1000 ppm by mass or less, even more preferably 500 ppm by mass or less, even more preferably 300 ppm by mass or less, particularly preferably 200 ppm by mass or less, very preferably 150 ppm by mass or less, and most preferably 100 ppm by mass or less.
• the total content of Cr, Mn, Fe and Ni, calculated as oxide is preferably 1000 ppm by mass or less (0.1% by mass or less), more preferably 800 ppm by mass or less, even more preferably 600 ppm by mass or less, even more preferably 400 ppm by mass or less, very preferably 350 ppm by mass or less, particularly preferably 200 ppm by mass or less, and most preferably 100 ppm by mass or less.
• ICP-MS inductively coupled plasma mass spectrometry
• the dielectric loss tangent of the present sintered body at 20 GHz is 0.00100 or less, preferably 0.00080 or less, more preferably 0.00060 or less, even more preferably 0.00050 or less, particularly preferably 0.00040 or less, and most preferably 0.00035 or less.
• the dielectric loss tangent at 10 GHz of the present sintered body is preferably 0.00100 or less, more preferably 0.00080 or less, even more preferably 0.00060 or less, even more preferably 0.00050 or less, particularly preferably 0.00040 or less, and most preferably 0.00035 or less.
• the lower limit is not particularly limited, and the dielectric loss tangent at 20 GHz and the dielectric loss tangent at 10 GHz are both, for example, 0.00010, and preferably 0.00020.
• the dielectric loss tangent is a value measured by the SPDR (split post dielectric resonator) method in an environment within the range of 23° C. ⁇ 2° C. and 50 ⁇ 5% RH at a frequency of 20 GHz or 10 GHz.
• SPDR split post dielectric resonator
• the relative dielectric constant at 20 GHz of the present sintered body (hereinafter also simply referred to as "relative dielectric constant”) is preferably 4.80 or more, more preferably 4.82 or more, still more preferably 4.85 or more, and even more preferably 4.90 or more.
• the upper limit is not particularly limited, and is, for example, 5.20, and preferably 5.10.
• the relative dielectric constant is a value measured by a split post dielectric resonator (SPDR) method in an environment within the range of 23° C. ⁇ 2° C. and 50 ⁇ 5% RH at a frequency of 20 GHz.
• SPDR split post dielectric resonator
• the porosity of the present sintered body is preferably 3.0% by volume or less, more preferably 1.5% by volume or less, even more preferably 0.5% by volume or less, particularly preferably 0.2% by volume or less, very preferably 0.15% by volume or less, and most preferably 0.1% by volume or less.
• the lower limit is preferably zero.
• Porosity is calculated in accordance with the calculation method for open porosity described in JIS R 1634:1998 "Method of measurement for sintered density and open porosity of fine ceramics.”
• the four-point bending strength of the present sintered body is preferably 170 MPa or more, more preferably 180 MPa or more, even more preferably 190 MPa or more, and particularly preferably 200 MPa or more. There is no particular upper limit, and the four-point bending strength of the present sintered body is, for example, 300 MPa or less, and may be 250 MPa or less.
• the four-point bending strength is measured at 25°C on a sintered test piece (flat plate, length 50 mm, width 4 mm, thickness 3 mm) in accordance with JIS R 1601 (2008).
• each component In order to achieve a four-point bending strength within the above range, it is preferable to set each component to the above-mentioned content and to manufacture the sintered body using the method described below (this manufacturing method).
• the Weibull coefficient of the present sintered body is preferably 9.0 or more, more preferably 10.0 or more, more preferably 10.5 or more, even more preferably 11.0 or more, even more preferably 11.5 or more, particularly preferably 12.0 or more, more particularly preferably 12.2 or more, and most preferably 12.5 or more.
• the Weibull coefficient of the present sintered body is, for example, 14.0 or less, and may be 13.0 or less.
• the Weibull coefficient (Weibull coefficient of four-point bending strength) is an index showing the degree of variation in four-point bending strength, and a larger value means a smaller variation in four-point bending strength.
• the Weibull modulus is determined as follows: First, the four-point bending strength of 30 test pieces is measured by the above-mentioned method. Next, the Weibull modulus is calculated according to JIS R 1625 (2010) using the bending strength data of the 30 pieces.
• each component it is preferable to set to the above-mentioned content and to manufacture the sintered body using the method described below (this manufacturing method).
• the thermal conductivity of the present sintered body is preferably 3.0 W/(m ⁇ K) or more, more preferably 3.4 W/(m ⁇ K) or more, even more preferably 3.5 W/(m ⁇ K) or more, even more preferably 3.8 W/(m ⁇ K) or more, and particularly preferably 4.0 W/(m ⁇ K) or more.
• the thermal conductivity of the present sintered body is, for example, 6.0 W/(m ⁇ K) or less, and may be 5.5 W/(m ⁇ K) or less.
• Thermal conductivity is measured on a test piece of the sintered body (12 mm x 12 mm plate, 6.0 mm thick) at 21°C using a NETZSCH laser flash method thermal property measuring device, the Xenon Flash Analyzer LFA 467 HyperFlash.
• each component In order to achieve a thermal conductivity within the above range, it is preferable to set each component to the above-mentioned content and to manufacture the sintered body using the method described below (this manufacturing method).
• ⁇ Amount of foreign phase (number of foreign particles)>
• the sintered body is observed at a magnification of 1,000 times using a scanning electron microscope (SEM), and SEM images are obtained from 50 random fields of view.
• SEM scanning electron microscope
• foreign particles containing element M2 particles composed of element M2
• EDX energy dispersive X-ray spectroscopy
• the number of foreign particles having a circle equivalent diameter of 5 ⁇ m or more (unit: pieces/cm 2 ) is measured, and the average value of 50 fields of view is calculated.
• the circle equivalent diameter is calculated by importing each captured SEM image into image processing software (WinROOF: manufactured by Mitani Shoji Co., Ltd.) and performing binarization processing to calculate the circle equivalent diameter of each foreign particle previously specified.
• the average value of the calculated number of foreign particles is taken as the number of foreign particles in the sintered body (this is conveniently called the "heterogeneous phase amount").
• the amount of heterogeneous phases in the present sintered body is preferably 150 pieces/cm2 or less , more preferably 100 pieces/cm2 or less , even more preferably 50 pieces/cm2 or less , particularly preferably 30 pieces/cm2 or less , and most preferably 10 pieces/cm2 or less .
• the lower limit is preferably zero.
• each component In order to keep the amount of heterogeneous phases within the above range, it is preferable to set each component to the above-mentioned content and to manufacture the sintered body by the method described below (this manufacturing method).
• the shape of the sintered body may be plate-like (for example, disk-like or flat), spherical, or spheroidal, and may be appropriately selected depending on the application.
• this sintered body has a small dielectric tangent, it is suitable for use as a dielectric material with low energy loss, for example, in technical fields where high-frequency electromagnetic waves are used.
• ⁇ Raw material powder a mixed powder containing cordierite powder produced by an electric melting method, mullite powder, and magnesium oxide powder is used.
• the raw material powder commercially available products can be used as appropriate.
• Cordierite powder is the raw material of Mg, Al, and Si that constitute the present sintered body. Furthermore, the cordierite powder may contain Ca as an impurity, and in this case, the Ca constituting the present sintered body is supplied. By using a cordierite powder with high purity, the Ca content in the sintered body can be reduced.
• cordierite powder manufactured by an electric fusion method (for convenience, also referred to as “electrically fused cordierite powder") is used.
• the method for obtaining the electrically fused cordierite powder is roughly as follows, for example.
• the raw material for the electrically fused cordierite powder is placed in a crucible.
• the raw material for the electrically fused cordierite powder include magnesium oxide (MgO), aluminum oxide (Al 2 O 3 ), and silica (SiO 2 ). These raw materials may contain impurities such as Ca.
• a plasma is generated using, for example, a carbon electrode to melt the raw material in the crucible.
• the molten raw material is then air-shattered and rapidly cooled.
• electrically fused cordierite powder is obtained.
• the electrically fused cordierite powder is a mainly amorphous substance (powder) containing some crystals.
• the particles constituting the electrically fused cordierite powder are spherical and have a uniform particle size. In other words, the electrically fused cordierite powder is homogeneous. Therefore, the electrically fused cordierite powder is easily sintered in the presence of mullite powder, which is a sintering aid described later. In other words, the sinterability is good. As a result, a dense sintered body can be obtained and the porosity can be reduced. Furthermore, by manufacturing it by the electric melting method, impurities can also be reduced.
• Mullite powder Mullite is expressed by the chemical formula, for example, 3Al 2 O 3.2SiO 2 or 2Al 2 O 3.SiO 2.
• Mullite powder is used as a sintering aid.
• mullite powder By using mullite powder as a sintering aid, a dense sintered body can be obtained.
• the mullite powder is a raw material of Al and Si which constitute the present sintered body.
• Magnesium oxide powder Magnesium oxide (MgO) powder is the raw material of Mg that constitutes the present sintered body.
• Yttrium oxide powder When the present sintered body contains Y, yttrium oxide (Y 2 O 3 ) powder is further used as a sintering aid.
• the yttrium oxide powder is a raw material of Y that constitutes the present sintered body.
• Each powder used as a raw material powder is preferably magnetically separated before use. This makes it possible to reduce the content of element M2 (Fe, etc.), which is a metal element other than element group M1 (Ca, Mg, Al, Y, and Si), in the present sintered body finally obtained.
• element M2 Fe, etc.
• element group M1 Ca, Mg, Al, Y, and Si
• a method of magnetic separation for example, a method using a wet magnetic filter is preferably mentioned.
• the conditions of magnetic separation are not particularly limited, and may be appropriately adjusted so that the element M2 has a desired content in the obtained present sintered body.
• a raw material powder which is a mixed powder of the powders.
• the mixing method is not particularly limited, and a conventionally known method can be used.
• the content of each powder in the raw material powder (mixed powder) is appropriately adjusted so that the content of each component in the final sintered body is the desired amount.
• the mixed powder is preferably pulverized to reduce the particle size in order to improve the sinterability during heating, which will be described later.
• the particle size of the mixed powder after pulverization is preferably 10 ⁇ m or less, more preferably 2 ⁇ m or less.
• the particle size is the particle size at an integrated value of 50% (D 50 ) in the particle size distribution, determined by a laser diffraction/scattering method (hereinafter the same).
• the pulverization method is not particularly limited, and pulverization can be performed using a ball mill, an attritor, a bead mill, a jet mill, or the like. In the case of wet pulverization, the mixed powder after pulverization is dried.
• a compact is produced using the raw material powder (mixed powder), that is, the raw material powder is molded.
• the molding method is not particularly limited, and a general molding method can be used. For example, molding is performed using a hydrostatic press at a pressure of 100 MPa or more and 200 MPa or less. As another method, a mixture of the mixed powder and an organic binder may be molded into a predetermined shape by press molding, extrusion molding, sheet molding, or the like. The shape obtained by molding is appropriately selected depending on the application of the resulting sintered body.
• the obtained compact is heated, thereby obtaining a sintered body.
• the heating temperature maximum temperature during heating
• the heating temperature is preferably 1400° C. or higher, more preferably 1410° C. or higher, and even more preferably 1430° C. or higher.
• the heating temperature is preferably 1450° C. or less, and more preferably 1440° C. or less.
• the heating time is preferably 1 hour or more, more preferably 2 hours or more, and even more preferably 5 hours or more.
• the heating time is preferably 48 hours or less, more preferably 12 hours or less, and even more preferably 8 hours or less.
• the atmosphere during heating is not particularly limited, and examples thereof include air atmosphere; inert atmospheres such as nitrogen and argon atmosphere; reducing atmospheres such as hydrogen atmosphere and a mixed atmosphere of hydrogen and nitrogen; and the like.
• the resulting sintered body is preferably densified, for example by hot isostatic pressing. Specifically, for example, the material is heated at a temperature of 1000° C. to 1350° C. while applying a pressure of 100 MPa to 200 MPa using a hot isostatic press.
• Examples 1 to 18 are working examples, and Examples 19 to 23 are comparative examples.
• powder A and/or powder B having a higher purity than powder A were used.
• powder A "ELP-150FINE” manufactured by AGC Ceramics Co., Ltd. was used.
• Powder B was prepared as follows. First, high purity magnesia (Kyowamag MF30 manufactured by Kyowa Chemical Industry Co., Ltd.), high purity alumina (AKP-30 manufactured by Sumitomo Chemical Co., Ltd.), and high purity silica (Admafine SO-E5 manufactured by Admatechs Co., Ltd.) were placed in a crucible as raw materials. Next, plasma was generated using a carbon electrode to melt the raw materials in the crucible. The molten raw materials were then air-crushed and quenched to obtain Powder B.
• mullite powder "KM101” manufactured by Kyoritsu Material Co., Ltd. was used.
• the powders were mixed so that the contents of element group M1 and element M2 in the resulting sintered body were the values shown in Table 1 below, to obtain a raw material powder that was a mixed powder.
• Each powder was magnetically separated before mixing. Specifically, a wet magnetic filter ("Wet High Magnetic Flux Tester FG Type" manufactured by Nippon Magnetic Mineral Processing Co., Ltd.) was used to magnetically separate a slurry in which each powder was dispersed in water.
• the conditions for magnetic separation were basically a slurry concentration of 15% by volume, a magnetic flux density of 2.8 Tesla, and three magnetic separations, but the conditions were appropriately changed as necessary.
• the raw material powder (mixed powder) was wet mixed and ground using a ball mill with high purity alumina balls and ethanol as a dispersion medium.
• the particle size (D 50 ) of the ground raw material powder was 2.0 ⁇ m.
• the obtained raw material powder (mixed powder) was pressed at room temperature with a pressure of 180 MPa using an isostatic press to produce a compact.
• the molded body was then heated in air at 1430° C. for 5 hours to obtain a sintered body.
• the obtained sintered body was densified. Specifically, the sintered body was heated at 1300° C. under a pressure of 145 MPa using a hot isostatic press.
• Example 19 the sintered bodies of Examples 1 to 18 had a dielectric loss tangent of 0.00100 or less at 20 GHz.
• Example 19 in which the Ca content (calculated as oxide) exceeded 2.0 mass %, the dielectric tangent at 20 GHz exceeded 0.00100.
• Example 20 in which the content of element M2 (converted into oxide) was more than 2.5 mass %, the dielectric tangent at 20 GHz was more than 0.00100.
• Example 22 in which the yttrium content (oxide equivalent) was more than 7.0 mass %, the dielectric dissipation factor at 20 GHz was more than 0.00100. Moreover, in Example 23 in which the content of element M2 (in terms of oxide) was more than 2.5 mass %, the dielectric tangent at 20 GHz was more than 0.00100.
• the dielectric loss tangent decreases as the frequency decreases. That is, the dielectric loss tangent at 10 GHz is smaller than the dielectric loss tangent at 20 GHz. For this reason, since the dielectric loss tangent at 20 GHz in all of Examples 1 to 18 is 0.00100 or less, it can be inferred that the dielectric loss tangent at 10 GHz is 0.00100 or less.
• the present invention provides a novel cordierite sintered body and a method for producing the same.

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