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  • 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
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  • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
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  • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
  • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
  • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
  • C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
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  • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
  • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
  • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
  • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
  • C04B2235/3418—Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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  • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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  • C04B2235/95—Products characterised by their size, e.g. microceramics
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  • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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  • C04B2235/963—Surface properties, e.g. surface roughness
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  • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
  • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
  • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
  • C04B2235/9646—Optical properties
  • C04B2235/9661—Colour

Definitions

• This disclosure relates to ceramic sintered bodies.
• Ceramic sintered bodies are known that are used for mounting substrates, components for exposure processing equipment, light shielding materials, heat absorbing materials, etc.
• Such ceramic sintered bodies are, for example, black in color and have a composite oxide that contains multiple metal elements such as Ti and Fe.
• a ceramic sintered body contains Al, Ti, Fe, and at least one of Si, Ca, and Mg, contains 67% or more of Al in terms of Al2O3 , contains 10% or more of Ti and Fe in terms of TiO2 and Fe2O3 in total in a range of 10% or more by mass and 30 % or less by mass, has TiO2 /( TiO2 + Fe2O3 ) of 5% or more and 20% or less, contains 0.5% or more by mass and 3.0% or less by mass of at least one of Si, Ca, and Mg in terms of SiO2 , CaO, and MgO in total, and has a volume resistivity of 1.0 x 104 ⁇ cm or more and 1.0 x 1011 ⁇ cm or less.
• Ceramic sintered bodies are known that are used for mounting substrates, components for exposure processing equipment, light shielding materials, heat absorbing materials, etc.
• Such ceramic sintered bodies are, for example, black in color and have a composite oxide that contains multiple metal elements such as Ti and Fe.
• the ceramic sintered body of the present disclosure contains Al, Ti, and Fe. Furthermore, the ceramic sintered body of the present disclosure contains at least one of Si, Ca, and Mg. The ceramic sintered body of the present disclosure contains multiple metal oxides.
• the ceramic sintered body of the present disclosure exhibits a black color.
• the ceramic sintered body of the present disclosure has a * and b * of -2.0 or more and 2.0 or less.
• a * and b * are values based on the CIE1976 (L * a * b * ) color space. Note that a * and b * can be adjusted by the composition of the metal oxide contained in the ceramic sintered body of the present disclosure, as well as the firing temperature and firing time.
• the ceramic sintered body of the present disclosure contains 67 mass% or more of Al in terms of Al2O3 , and may further contain 75 mass% or more of Al.
• the ceramic sintered body of the present disclosure may contain 89.5 mass% or less of Al in terms of Al2O3 .
• the content of Al may be adjusted according to the content of other components described later.
• the ceramic sintered body of the present disclosure may contain a total of 10 mass% or more and 30 mass% or less of Ti and Fe, calculated as TiO2 and Fe2O3 , and may further contain a total of 20 mass% or more and 25 mass % or less of Ti and Fe, calculated as TiO2 and Fe2O3 .
• the resistivity of the ceramic sintered body can be reduced. Also, by containing 30 mass% or less of Ti and Fe calculated as TiO2 and Fe2O3 in total , the mechanical strength of the ceramic sintered body can be maintained at a good level.
• TiO 2 /(TiO 2 +Fe 2 O 3 ) may be 5% or more and 20% or less, and further, TiO 2 /(TiO 2 +Fe 2 O 3 ) may be 15% or more and 20% or less.
• the resistivity of the ceramic sintered body can be reduced. Also, when TiO2 /( TiO2 + Fe2O3 ) is 20% or less, the ceramic sintered body can exhibit a good black color.
• the ceramic sintered body of the present disclosure may contain at least one of Si, Ca, and Mg in a total amount of 0.5 mass% or more and 3.0 mass% or less in terms of SiO2 , CaO, and MgO.
• the resistivity of the ceramic sintered body can be reduced. Also, by containing at least one of Si, Ca and Mg in a total amount of 3.0 mass% or less calculated as SiO2, CaO and MgO, the low reflectance of the ceramic sintered body can be well maintained.
• the ceramic sintered body of the present disclosure may have a volume resistivity of 10 4 ⁇ cm or more and 10 11 ⁇ cm or less, and may further have a volume resistivity of 10 10 ⁇ cm or less. This provides a ceramic sintered body suitable for applications requiring semiconductivity.
• the grain boundary phase is primarily responsible for reducing the specific volume resistivity.
• the volume resistivity tends to be low. This is presumably because the network of the grain boundary phase becomes thicker as the average crystal grain size increases.
• the ceramic sintered body of the present disclosure has a specific three-point bending strength as a mechanical strength of 260 MPa or more, and may further have a three-point bending strength of 300 MPa or more. This makes it possible to obtain a ceramic sintered body suitable for applications requiring high physical strength.
• the average crystal grain size may be in the range of 5 ⁇ m or more and 7 ⁇ m or less.
• the average crystal grain size can be controlled by appropriately adjusting the firing temperature and firing time.
• the average crystal grain size may also be measured by the cord method.
• the ceramic sintered body of the present disclosure has a composition within the above-mentioned range, making it possible to realize a black ceramic sintered body that is semiconductive and has excellent mechanical strength.
• the ceramic sintered body of the present disclosure can exhibit semiconductivity even when fired in a non-reducing atmosphere. This allows for easy production of semiconductive ceramic sintered bodies, thereby reducing the production costs of ceramic sintered bodies.
• the ceramic sintered body of the present disclosure has a reflectance of 15% or less, and may further have a reflectance of 10% or less. This makes it possible to obtain a ceramic sintered body suitable for applications requiring a low reflectance.
• the ceramic sintered body of the present disclosure may have a * and b * of -2.0 or more and 2.0 or less, thereby obtaining a ceramic sintered body that is particularly suitable for applications requiring a black color.
• Each metal element contained in the ceramic sintered body of the present disclosure can be quantified using an ICP (Inductively Coupled Plasma) emission spectroscopic analyzer.
• the content of each metal element obtained by the measurement is converted into a metal oxide to obtain the content of each metal element.
• Al is converted into Al 2 O 3 , Ti into TiO 2 , Fe into Fe 2 O 3 , Si into SiO 2 , Ca into CaO, and Mg into MgO.
• the ceramic sintered body contains other metal elements, it is sufficient to convert them into representative metal oxides of each element.
• Particulate or powdered Al 2 O 3 , TiO 2 and Fe 2 O 3 are mixed, and at least one of SiO 2 , CaO and MgO is added as a sintering aid.
• the particle size of each raw material powder may be, for example, 0.1 ⁇ m to 5 ⁇ m.
• the molded body can be produced using known techniques, such as press molding.
• the firing temperature during firing may be, for example, 1350°C or higher and 1550°C or lower.
• the firing time may be, for example, about 2 hours.
• the firing atmosphere may be air.
• Ceramic sintered bodies having different compositions were prepared, and the volume resistivity, reflectance, a * , b * and three-point bending strength as an indicator of mechanical strength were measured.
• Al 2 O 3 powder, TiO 2 powder, Fe 2 O 3 powder, SiO 2 powder, CaO powder, and MgO powder were prepared.
• the sintered ceramics were weighed so that the mass ratios of Al oxide (Al 2 O 3 ), Fe oxide (Fe 2 O 3 ), Ti oxide (TiO 2 ), Si oxide (SiO 2 ), Ca oxide (CaO), and Mg oxide (MgO) were the values shown in Table 1.
• the compacts were fired in a firing furnace in an air atmosphere, i.e., an oxidizing atmosphere, to obtain sintered bodies for each sample.
• the firing temperature was in the range of 1350°C to 1550°C, and the firing time was 2 hours.
• each sample was measured using XRD to confirm the presence of aluminum oxide (alumina).
• each sample was measured for Al, Si, Ca, Mn, Ti, Fe and Mg using an ICP optical emission spectrometer to determine the content of each element, which was then converted into the content of each oxide to calculate the content of each element shown in Table 1. Note that ICP optical emission spectroscopic analysis is sometimes simply referred to as ICP.
• the volume resistivity of the obtained sintered body was measured by the three-terminal method using a commercially available electrical resistance measuring device, for example, HIOKI's ultra insulation resistance meter DSM-8104, and the results are shown in Table 1.
• the reflectance of the obtained sintered body was measured in the visible light range using a color difference meter, such as a Konica Minolta CR-13, and the results are shown in Table 1.
• a * and b * based on the CIE1976 (L * a * b * ) color space were measured at wavelengths of 400 nm to 700 nm using a spectrophotometer, for example, CM-700dl manufactured by Konica Minolta, in accordance with JIS Z 8722-2000, and the measurement results of a * and b * are shown in Table 1. Note that the notation (%) shown in Table 1 is an abbreviation for mass % except for reflectance.
• the three-point bending strength of the obtained sintered body was also measured in accordance with JIS R 1601-2008, and the results are shown in Table 1.
• the average crystal grain size of sample No. 18 was 4.6 ⁇ m, which was smaller than the average crystal grain size of sample No. 19, which had an average crystal grain size of 5.1 ⁇ m.
• the average crystal grain sizes of samples Nos. 2 to 5, 8 to 11, and 14 to 17 were all within the range of 5 ⁇ m to 7 ⁇ m.
• sample No. 20 was less than 260 MPa, resulting in a ceramic sintered body with poor mechanical strength.
• the ceramic sintered body of the present disclosure has good semiconductivity and physical strength.
• the ceramic sintered body of the present disclosure has a reflectance of 15% or less, a * and b * of -2.0 or more and 2.0 or less, and exhibits a black color.
• a disk with a thickness of 30 mm and a diameter of 800 mm after firing was prepared, and a * , b * , and reflectance were measured at five points on the surface of the disk with an equal width in the diametric direction. This measurement was performed on the polished surface.
• the color tone was measured using a spectrophotometer CM-26dg manufactured by Konica Minolta, Inc., and the measurement wavelength was 360 nm to 740 nm.
• the surface roughness Ra after polishing was about 0.2 to 0.6 ⁇ m.
• the difference between the maximum and minimum values of a* was 0.28.
• the difference between the maximum and minimum values of b* was 0.31.
• the difference between the maximum and minimum values of reflectance was 0.68%.
• the ceramic sintered body of the present disclosure has small color tone difference depending on the location, even in a large product.

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