Setter for burning and method of manufacturing setter for burning

Abstract

To prolong the life of a setter for firing.SOLUTION: The setter for firing is provided with a base material made of ceramic and a coating layer made of stabilized zirconia formed on the surface of the base material and excessively containing a stabilizing material. The method for producing the setter for firing includes a coating step of forming a coating layer on the surface of a ceramic substrate by using a coating raw material containing stabilized zirconia and an additional stabilizing material.SELECTED DRAWING: Figure 2

Description

[Technical Field]

[0001] The present invention relates to a firing setter and a method for manufacturing the firing setter. [Background technology]

[0002] Conventionally, when manufacturing ceramic products such as ceramic capacitors, the object to be fired is set in a firing setter and fired. As a firing setter, one in which a stabilized zirconia coating layer is formed on the surface of a ceramic base material has been proposed (see, for example, Patent Document 1). By providing a stabilized zirconia coating layer, it is possible to suppress reaction between the firing setter and the object to be fired when firing the object. [Prior art documents] [Patent documents]

[0003] [Patent Document 1] Japanese Patent Publication No. 2023-160735 Summary of the Invention [Problem to be solved by the invention]

[0004] Stabilized zirconia is made by adding a stabilizer to zirconia to suppress volume changes associated with temperature changes. Therefore, when stabilized zirconia is used in the coating layer of a firing setter, it is expected that the coating layer will be less likely to expand or contract even when repeatedly exposed to temperature changes during firing, and that the coating layer will be less likely to peel off from the substrate. However, in practice, even when stabilized zirconia is used in the coating layer, repeated use can lead to the coating layer peeling off relatively early, or reaching the end of its life.

[0005] The present invention has been made to solve such problems, and its main object is to extend the life of a firing setter. [Means for solving the problem]

[0006] [1] The firing setter of the present invention is A ceramic substrate; a coating layer made of stabilized zirconia formed on the surface of the substrate and containing an excess of a stabilizer; Equipped with.

[0007] In this firing setter, the coating layer made of stabilized zirconia contains an excess amount of stabilizer. This allows the firing setter to have a longer service life. The reason for this effect is presumed to be as follows: When ordinary stabilized zirconia is used in the coating layer, repeated use can cause the stabilizer to be desorbed, making the zirconia unstable and resulting in peeling from the substrate. On the other hand, in the present invention, the coating layer made of stabilized zirconia contains an excess amount of stabilizer. Therefore, even if the stabilizer is desorbed with use, the excess amount can compensate for the desorbed amount, thereby preventing the zirconia from becoming unstable and presumably achieving a longer service life.

[0008] [2] In the firing setter of the present invention (the firing setter described in [1] above), the coating layer may further contain a stabilizer in an amount of 0.5% by mass to 20% by mass based on the stabilized zirconia. This can extend the lifespan.

[0009] [3] In the setter for firing of the present invention (the setter for firing according to the above [1] or [2]), the stabilizing material may contain calcium or yttrium.

[0010] [4] In the firing setter of the present invention (the firing setter according to any one of [1] to [3] above), the stabilizing agent may contain calcium and the zirconia stabilization rate of the coating layer may be 90% or more, or the stabilizing agent may contain yttrium and the zirconia stabilization rate of the coating layer may be 98% or more.

[0011] [5] In the setter for firing of the present invention (the setter for firing according to any one of the above [1] to [4]), the ceramic of the substrate may contain any one of silicon carbide, alumina, and mullite.

[0012] [6] In the setter for firing of the present invention (the setter for firing according to any one of the above [1] to [5]), the ceramic substrate may be a Si—SiC composite material.

[0013] [7] In the setter for firing of the present invention (the setter for firing according to any one of the above [1] to [6]), the coating layer may be such that the ratio IB / IA of the height IB of the main peak of unstabilized zirconia to the height IA of the main peak of stabilized zirconia in an XRD pattern is 0.1 or less.

[0014] [8] In the setter for firing of the present invention (the setter for firing according to any one of the above [1] to [7]), the coating layer may have a half-width WA of the main peak of stabilized zirconia in an XRD pattern of 0.2° or less. In this specification, the half-width refers to the full width at half maximum (FWHM).

[0015] [9] In the setter for firing of the present invention (the setter for firing according to any one of the above [1] to [8]), the zirconia stabilization rate S of the coating layer after use is compared with the zirconia stabilization rate S of the coating layer before use. x The ratio S x In such a case, the zirconia is stabilized even after use, and a long life can be achieved.

[0016]

[10] The method for producing a setter for firing of the present invention comprises: The method includes a coating step of forming a coating layer on the surface of a ceramic substrate using a coating raw material containing stabilized zirconia and an additional stabilizer.

[0017] This method for manufacturing a setter for firing can provide the setter for firing described above, thereby realizing a longer life for the setter for firing. [Brief explanation of the drawings]

[0018] [Figure 1] FIG. 2 is a perspective view showing a firing setter 10; [Figure 2] FIG. 2 is a cross-sectional view schematically showing a firing setter 10. [Figure 3] 3A to 3C are explanatory diagrams showing a schematic diagram of a method for manufacturing a firing setter 10. [Figure 4] XRD patterns of Experimental Examples 19-23. DETAILED DESCRIPTION OF THE INVENTION

[0019] [Firing setter] The firing setter of the present invention comprises a substrate and a coating layer formed on the surface of the substrate. The firing setter can be suitably used, for example, in the manufacturing process (e.g., firing process or heat treatment process) of ceramic electronic components such as ceramic capacitors. The firing setter may be used to place an object to be fired on it, or may be used to position or fix the object to be fired. The firing setter may be in the shape of a plate, a box, or another shape.

[0020] The substrate is made of ceramic and may be plate-shaped, box-shaped, or other shapes depending on the shape of the firing setter. Examples of ceramics include silicon carbide, alumina, and mullite, with silicon carbide being preferred. Examples of silicon carbide include Si-SiC composite materials containing metallic silicon (e.g., Si-bonded SiC, Si-impregnated SiC, etc.) and recrystallized SiC, with Si-SiC composite materials being preferred. The thickness of the substrate may be, for example, 0.1 mm or more and 5 mm or less.

[0021] The coating layer is made of stabilized zirconia and contains an excess of stabilizers. Zirconia changes its crystalline phase from monoclinic to tetragonal to cubic as the temperature rises from room temperature. Stabilized zirconia is made by adding stabilizers to zirconia, which extends the stable range of cubic and tetragonal crystal phases at high temperatures to the low temperature side, so that the cubic and tetragonal crystal phases remain even at room temperature.

[0022] Examples of stabilizers include those containing calcium, such as CaO, and those containing yttrium, such as Y2O3. Calcium-containing stabilizers are relatively inexpensive and are therefore preferable from a cost perspective. Stabilizers containing yttrium are preferable because even a small amount can extend the service life. "Excessive stabilizer content" refers to an amount greater than the amount of stabilizer at which the proportion of stabilized zirconia no longer increases (also referred to as the "essential stabilizer amount"). The coating layer may further contain 0.5% to 20% by mass of stabilizer relative to the stabilized zirconia (which contains more than the essential stabilizer amount and may be a commercially available product). When the stabilizer contains calcium, the proportion of the additional stabilizer relative to the stabilized zirconia is preferably 1% to 15% by mass, and more preferably 1% to 10% by mass. When the stabilizer contains yttrium, the proportion of the additional stabilizer relative to the stabilized zirconia is preferably 0.5% to 15% by mass. The proportion of the stabilizer in the coating layer may be 10 mol% or more, 15 mol% or more, or 20 mol% or more. The proportion of the stabilizer in the coating layer may be 50 mol% or less, 40 mol% or less, or 30 mol% or less. The proportion of the stabilizer here is based on the metal element (Ca or Y) in the stabilizer. For example, a coating containing 1 mol% Y2O3 is considered to contain 2 mol% of the stabilizer (metal element Y). The proportion of the stabilizer may be measured by inductively coupled plasma (ICP) atomic emission spectroscopy in accordance with JIS R2012:1998 or JIS R1695:2014. The coating layer may contain, for example, uniformly dispersed calcium or uniformly dispersed yttrium due to the stabilizer.

[0023] The stabilized zirconia in the coating layer may be a single cubic phase, a single tetragonal phase, or a mixture of cubic and tetragonal phases. Depending on the type of stabilizer, increasing the amount of stabilizer may not stabilize all of the zirconia, resulting in unstabilized zirconia (monoclinic) remaining in the coating layer. The coating layer may contain such unavoidably remaining unstabilized zirconia. However, it is preferable that the amount of unstabilized zirconia contained in the coating layer be as small as possible.

[0024] The coating layer preferably has an X-ray diffraction (XRD) pattern where the ratio IB / IA, the height of the main peak of stabilized zirconia to the height of the main peak of unstabilized zirconia, is 0.1 or less, more preferably 0.07 or less, and even more preferably 0.05 or less, although this ratio varies depending on the type of stabilizer. The IB / IA value is 0 or greater, but may be, for example, 0.01 or greater or 0.02 or greater. Generally, the main peak of stabilized zirconia appears at 2θ=29.5° to 30.5°, while the main peak of unstabilized zirconia appears at 2θ=27.5° to 28.5°. The XRD pattern is measured by peeling off the coating layer and powdering it (the same applies hereinafter).

[0025] The coating layer preferably has a half-width WA of the main peak of stabilized zirconia in the XRD pattern of 0.3° or less, more preferably 0.2° or less, and even more preferably 0.17° or less, depending on the type of stabilizer. This peak half-width WA may be, for example, 0.01° or more or 0.1° or more. The coating layer may have a half-width WA within the above range before use of the sintering setter (passing through a kiln), or may have a half-width WA within the above range after use of the sintering setter (passing through a kiln).

[0026] The coating layer preferably has a zirconia stabilization rate S [%] of 90% or more, more preferably 92% or more, depending on the type of stabilizer. The zirconia stabilization rate S is calculated from the formula S = A / (A + B) × 100 × 1.075, where A is the integrated intensity of the main peak of stabilized zirconia and B is the integrated intensity of the main peak of unstabilized zirconia in the XRD pattern of the coating layer. When the stabilizer contains calcium, the zirconia stabilization rate S is preferably 92% or more. When the stabilizer contains yttrium, the zirconia stabilization rate S is preferably 98% or more, more preferably 100% or more. It is preferable that the zirconia stabilization rate S of the coating layer does not decrease much due to the use of a firing setter. For example, the zirconia stabilization rate S of the coating layer after use is calculated by comparing the zirconia stabilization rate S of the coating layer before use with the zirconia stabilization rate S of the coating layer after use with the zirconia stabilization rate S of the coating layer before use. x The ratio S x / S0 is preferably 0.9 or more, more preferably 0.95 or more, and even more preferably 0.98 or more. Note that "after use" may refer to, for example, after a heating treatment in an inert atmosphere within a temperature range of 1100°C to 1350°C for 2 hours has been carried out 10 or more times (preferably 20 or more times, more preferably 100 or more times).

[0027] The coating layer may be one in which a peak attributable to the stabilizer (e.g., a CaO peak or a Y2O3 peak) is confirmed in the XRD pattern. As the amount of stabilizer in the coating layer increases, a peak attributable to the stabilizer is confirmed in the XRD pattern (e.g., if the stabilizer is CaO, a peak at 2θ = 37.4° is confirmed, and if the stabilizer is Y2O3, a peak at 2θ = 29.2° is confirmed). Furthermore, the coating layer may be one in which a crystalline phase corresponding to the stabilizer (CaO or Y2O3) is confirmed in a crystalline phase mapping image obtained by energy dispersive X-ray spectroscopy (EDS), electron backscatter diffraction (EBSD), or the like.

[0028] The thickness of the coating layer may be, for example, 5 μm or more, or 50 μm or more. The thickness of the coating layer may be, for example, 1000 μm or less, or 200 μm or less. The surface of the coating layer may be provided with irregularities. The surface roughness Ra of the coating layer may be, for example, 0.5 μm or more and 50 μm or less.

[0029] The coating layer may be formed on the surface of the substrate via an intermediate layer. The intermediate layer may be one layer or two or more layers. The intermediate layer is made of ceramic. Examples of ceramic include silicon carbide, alumina, mullite, silica, magnesia, yttria, and mixtures of two or more of these. The total thickness of the intermediate layer may be, for example, 5 μm or more, or 50 μm or more. The total thickness of the intermediate layer may be, for example, 1000 μm or less, or 300 μm or less.

[0030] A firing setter 10, which is an example of a firing setter according to the present invention, will be described with reference to the drawings. FIG. 1 is a perspective view schematically illustrating the firing setter 10. FIG. 2 is a cross-sectional view schematically illustrating the firing setter 10. In FIG. 2, the mechanism of action of the present invention is schematically illustrated using CaO as a stabilizer. As shown in FIGS. 1 and 2, the firing setter 10 includes a ceramic substrate 12 and a coating layer 16 formed on the surface of the substrate 12 via an intermediate layer 14. The coating layer 16 is made of stabilized zirconia containing an excess amount of stabilizer. The surface 16a of the coating layer 16 may be provided with irregularities. In this firing setter 10, as shown in FIG. 2, even if there are areas where CaO is released from stabilized ZrO2 during use (for example, due to temperature changes or reaction with the firing target), the excess stabilizer CaO is supplied to those areas, preventing ZrO2 from becoming unstabilized. It is believed that this will enable the firing setter 10 to have a longer life.

[0031] [Manufacturing method of firing setter] The method for producing a setter for firing of the present invention includes a coating step of forming a coating layer on the surface of a ceramic substrate using a coating raw material containing stabilized zirconia and an additional stabilizer. This production method may also be used to produce the setter for firing described above. In this production method, the configuration and conditions described for the setter for firing may be applied.

[0032] The stabilized zirconia used in the coating process contains a stabilizer in an amount equal to or greater than the required amount, and may be a commercially available product. This stabilized zirconia may be stabilized with a calcium-containing stabilizer such as CaO, or with an yttrium-containing stabilizer such as Y2O3. This stabilized zirconia may be in the form of a powder. The average particle size of the stabilized zirconia may be, for example, 0.1 μm or more, or 0.2 μm or more. The average particle size of the stabilized zirconia may be, for example, 700 μm or less, or 300 μm or less. In this specification, the average particle size is the volume-based median diameter D50 measured by laser diffraction.

[0033] The additional stabilizer used in the coating process may contain calcium, such as CaO, or yttrium, such as Y2O3. The additional stabilizer is preferably the same type as the stabilizer used in the stabilized zirconia used in the coating process. The additional stabilizer may be in the form of a powder. The average particle size of the additional stabilizer may be, for example, 0.1 μm or more, or 0.2 μm or more. The average particle size of the additional stabilizer may be, for example, 700 μm or less, or 300 μm or less. The amount of the additional stabilizer is preferably 0.5% by mass or more and 20% by mass or less relative to the stabilized zirconia used in the coating process. When the additional stabilizer contains calcium, the amount of the additional stabilizer is preferably 1% by mass or more and 15% by mass or less, and more preferably 1% by mass or more and 10% by mass or less, relative to the stabilized zirconia used in the coating process. When the additional stabilizer contains yttrium, the amount of the additional stabilizer is preferably 0.5% by mass or more and 15% by mass or less relative to the stabilized zirconia used in the coating process.

[0034] Examples of methods for forming the coating layer include spraying, printing, and thermal spraying. Of these, spraying and printing are preferred, with spraying being more preferred. In the spraying method, stabilized zirconia and an additional stabilizer are dispersed in a solvent such as water or an organic solvent to prepare a slurry-like coating raw material, which is then sprayed using a spray device to form a raw material layer, and dried or fired as needed to form the coating layer. In the printing method, a solvent such as water or an organic solvent is added to stabilized zirconia and an additional stabilizer to prepare a slurry or paste-like coating raw material, which is then used to form a raw material layer using a printing method such as screen printing, and dried or fired as needed to form the coating layer. In the spraying and printing methods, the firing temperature may be, for example, 1200°C or higher and 1400°C or lower, the firing atmosphere may be, for example, air, and the firing time may be, for example, 1 hour to 5 hours.

[0035] An intermediate layer may be formed on the surface of the substrate prior to the coating step, and a coating layer may be formed on the surface of the intermediate layer on the substrate in the coating step. The intermediate layer may be formed using an intermediate layer raw material containing ceramic powder. Examples of ceramic powder that can be used include silicon carbide, alumina, mullite, silica, magnesia, yttria, and mixtures of two or more of these. The average particle size of the ceramic powder may be, for example, 0.1 μm or more, or 0.2 μm or more. The average particle size of the ceramic powder may be, for example, 700 μm or less, or 300 μm or less. Examples of methods for forming the intermediate layer include spraying, printing, and thermal spraying, which can be performed in accordance with the methods described in the coating step.

[0036] An example of a manufacturing method for a setter for firing of the present invention will be described with reference to the drawings. FIG. 3 is an explanatory diagram schematically illustrating a manufacturing method for a setter for firing 10. FIG. 3A is a schematic diagram of the coating process, and FIG. 3B is a schematic diagram of the state after the coating process is completed. In the coating process, as shown in FIG. 3A, a coating raw material 20 containing stabilized zirconia 22 and an additional stabilizer 24 is used. An intermediate layer 14 is formed on the surface of the substrate 12. Then, a spray device 30 is used to spray the coating raw material 20 onto the surface of the intermediate layer 14 on the substrate 12 to form a raw material layer 26. The raw material layer 26 is then dried and fired as necessary to form the coating layer 16. This results in a setter for firing 10, as shown in FIG. 3B. The substrate 12 and intermediate layer 14 may be fired or may be used in a green body state before firing. The intermediate layer 14 may also be omitted.

[0037] According to the setter for firing and the method for manufacturing the setter for firing of the embodiment described above, it is possible to realize a longer life of the setter for firing, as described above.

[0038] It goes without saying that the present invention is not limited to the above-described embodiment, and can be embodied in various forms as long as they fall within the technical scope of the present invention.

[0039] For example, the setter for firing of the present invention does not have to be manufactured by the above-mentioned manufacturing method, and may be manufactured by forming a coating layer on the surface of a ceramic substrate using a coating raw material containing unstabilized zirconia and a stabilizer in an amount exceeding the essential amount of the stabilizer. [Example]

[0040] Examples in which the firing setter of the present invention was investigated are described below as examples. Experimental Examples 2 to 9, 11 to 18, and 22 to 23 correspond to examples of the present invention, Experimental Examples 1, 10, and 20 to 21 correspond to comparative examples, and Experimental Example 19 corresponds to a reference example.

[0041] [Experimental Examples 1-18] A coating material was prepared by blending stabilized ZrO2 (average particle size 9.3 μm) with CaO (average particle size 9.3 μm) or Y2O3 (average particle size 9.3 μm) as a stabilizer in the ratios shown in Table 1, and adding water as a solvent. This coating material was sprayed onto the surface of a 2 mm thick plate-shaped Si-impregnated SiC substrate using a spray device to form a 50 μm thick layer of the material, which was then fired at 1300°C for 3 hours in an air atmosphere to form a coating layer. In this way, a setter for firing was obtained. The coating layer was formed on the surface of a 100 μm thick intermediate layer made of mullite formed on the substrate.

[0042] The coating layer was peeled off from the obtained setter for firing to obtain a powder, which was then subjected to powder XRD diffraction measurement, and the ZrO2 stabilization rate was measured from the obtained XRD pattern.

[0043] The object to be fired (a general-purpose ceramic capacitor) was placed on the resulting firing setter and fired at 1200°C for 2 hours in an inert atmosphere. This procedure was repeated until the firing setter reached the end of its service life. The end of its service life was defined as when peeling of the coating layer was confirmed visually. This test was performed on four samples for each experimental example. After repeating the procedure the number of times shown in Table 1 (100 times for "≧100"), the percentage of samples for which peeling of the coating layer was confirmed visually was calculated. Coating peeling was evaluated by assigning a "good" rating to a percentage of peeling less than 10%, a "fair" rating to a percentage of peeling less than 50%, and an "unsatisfactory" rating to a percentage of peeling 50% or more.

[0044] Table 1 summarizes the stabilizer type, stabilizer addition ratio, ZrO2 stabilization rate, number of uses, and coating peeling evaluation results for Experimental Examples 1 to 18. As shown in Table 1, compared to Experimental Example 1 and Experimental Example 10, which did not contain a stabilizer, Experimental Examples 2 to 9 and Experimental Examples 11 to 18, which contained an added stabilizer, had longer lifespans. When CaO was used as the stabilizer, Experimental Examples 3 to 8 had longer lifespans and excellent coating peeling evaluation results, and Experimental Examples 3 to 7 had even longer lifespans. Therefore, it was found that the stabilizer addition ratio is preferably 0.5% to 20% by mass, more preferably 1% to 15% by mass, and even more preferably 1% to 10% by mass. Furthermore, when Y2O3 was used as the stabilizer, Experimental Examples 11 to 18 had longer lifespans and excellent coating peeling evaluation results. Therefore, it was found that the stabilizer addition ratio is preferably 0.5% to 20% by mass, more preferably 0.5% to 15% by mass.

[0045] [Table 1]

[0046] [Experimental Examples 19-23] A coating material was prepared by blending stabilized ZrO2 (average particle size 9.3 μm) and CaO (average particle size 9.3 μm) as a stabilizer in the ratio shown in Table 2, and adding water as a solvent. This coating material was sprayed onto the surface of a 2 mm thick plate-shaped Si-impregnated SiC substrate using a spray device to form a 100 μm thick layer of the material, which was then fired at 1300°C for 3 hours in an air atmosphere to form a coating layer. In this way, a setter for firing was obtained. The coating layer was formed on the surface of a 150 μm thick intermediate layer made of mullite formed on the substrate.

[0047] The object to be fired (a general-purpose ceramic capacitor) was placed on the resulting firing setter and fired in an inert atmosphere at 1200°C for 2 hours. This procedure was repeated the specified number of times shown in Table 2. After the specified number of times of firing, the firing setter was visually inspected for peeling of the coating layer. In addition, the coating layer was peeled off from the firing setter after the specified number of times of firing, and powder was subjected to powder XRD diffraction measurement. The ZrO2 stabilization rate, half-width WA, and ratio IB / IA were determined from the obtained XRD pattern.

[0048] Figure 4 shows the XRD patterns of Experimental Examples 19 to 23 after passing through the kiln a predetermined number of times. 0.866 Ca 0.134 O 1.866Powder diffraction data for ZrO (stabilized zirconia, cubic) and ZrO (unstabilized zirconia, monoclinic) are also shown. Experimental Examples 20–21, which were conventionally coated and kiln-passed, showed XRD patterns dominated by peaks of unstabilized zirconia. Experimental Example 19, which was conventionally coated before kiln-passing, and Experimental Examples 22–23, which were overcoated with stabilizers and kiln-passed, showed XRD patterns dominated by peaks of stabilized zirconia. However, in Experimental Example 19 with conventional coating, the ratio IB / IA (the height of the main peak A of stabilized zirconia, IB, to the height of the main peak B of unstabilized zirconia, IB, exceeded 0.1, suggesting that a small amount of unstabilized zirconia may have formed during the coating process. In Experimental Examples 22–23 with overcoated stabilizers, the ratio IB / IA was low, below 0.1, even after kiln-passing, suggesting that little unstabilized zirconia was formed. In addition, in Experimental Examples 22 to 23, the half-width WA of the main peak A of stabilized zirconia was small, at 0.2° or less, suggesting that the crystallinity of the stabilized zirconia was maintained at a high level. The excess stabilizer coating showed the same XRD pattern as Experimental Examples 22 to 23 even before passing through the kiln, and it was suggested that the stabilization rate S, half-width WA, and ratio IB / IA were also similar to those of Experimental Examples 22 to 23.

[0049] Table 2 summarizes the coating type, stabilizer addition ratio, kiln pass count, ZrO2 stabilization ratio after kiln pass count, and whether or not peeling occurred after kiln pass count for Experimental Examples 19-23. As shown in Table 2, peeling of the coating layer was observed for all conventionally coated specimens after kiln pass counts, whereas no peeling of the coating layer was observed for the excessively stabilized specimens, even after kiln pass counts. With the conventionally coated specimens, the ZrO2 stabilization ratio decreased with increasing kiln pass counts. This is thought to be due to a volume change caused by a phase change between monoclinic and tetragonal or cubic crystals due to temperature changes during use, resulting in the coating layer peeling. On the other hand, the ZrO2 stabilization ratio did not decrease for the excessively stabilized specimens after kiln pass counts, suggesting that this prevented volume changes due to phase changes caused by temperature changes during use, thereby preventing coating layer peeling.

[0050] [Table 2] [Industrial Applicability]

[0051] The present invention can be used in a firing tool used in a manufacturing process of ceramic parts, for example, a firing process or a heat treatment process. [Explanation of symbols]

[0052] 10 firing setter, 12 substrate, 14 intermediate layer, 16 coating layer, 16a surface, 20 coating raw material, 22 stabilized zirconia, 24 additional stabilizing material, 26 raw material layer, 30 spray device.

Claims

1. A ceramic substrate; a coating layer made of stabilized zirconia formed on the surface of the substrate and containing an excess of a stabilizer; A baking setter equipped with

2. 2. The setter for firing according to claim 1, wherein the coating layer further contains a stabilizer in an amount of 0.5% by mass to 20% by mass relative to the stabilized zirconia.

3. 3. The setter for firing according to claim 1, wherein the stabilizing material comprises calcium or yttrium.

4. The stabilizing material contains calcium and the zirconia stabilization rate S of the coating layer is 90% or more; the stabilizer contains yttrium and the zirconia stabilization rate S of the coating layer is 98% or more; The firing setter according to claim 3.

5. 3. The firing setter according to claim 1, wherein the ceramic substrate comprises any one of silicon carbide, alumina, and mullite.

6. 3. The firing setter according to claim 1, wherein the ceramic substrate is a Si-SiC composite material.

7. 3. The setter for firing according to claim 1, wherein the coating layer has an XRD pattern in which the ratio IB / IA of the height IB of the main peak of unstabilized zirconia to the height IA of the main peak of stabilized zirconia is 0.1 or less.

8. 3. The setter for firing according to claim 1, wherein the coating layer has a half-width WA of a main peak of stabilized zirconia in an XRD pattern of 0.2° or less.

9. The zirconia stabilization rate S of the coating layer before use 0 The zirconia stabilization rate S of the coating layer after use x The ratio S x / S 0 3. The setter for firing according to claim 1, wherein the value of the sintering coefficient is 0.9 or more.

10. The coating step includes forming a coating layer on a surface of a ceramic substrate using a coating material containing stabilized zirconia and an additional stabilizer. A method for manufacturing a firing setter.

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