Method for manufacturing ceramic components

Abstract

To provide ceramic components with excellent appearance stability. [Solution] A method for manufacturing a ceramic member, comprising: a heat treatment step of obtaining a raw material powder by nitriding metallic Si by a direct nitriding method, preparing a mixed powder containing the raw material powder, and subjecting the mixed powder to heat treatment; and a firing step of firing the heat-treated mixed powder after the heat treatment step to obtain a ceramic member, wherein the heat treatment is held in a vacuum atmosphere at a heat treatment temperature of 1000 to 1400°C for 1 to 5 hours, and in the firing step, the mixture is heated from the heat treatment temperature to the firing temperature and fired in a nitrogen atmosphere.

Description

[Technical Field]

[0001] This invention relates to a method for manufacturing ceramic components. [Background technology]

[0002] In testing whether an integrated circuit is functioning correctly, for example, a probe card is used. Figure 1 shows a cross-sectional view illustrating the configuration of a probe card, and Figure 2 shows a top view illustrating the configuration of a probe guide component. As shown in Figures 1 and 2, the probe card 10 comprises needle-shaped probes 11 and probe guide components 12 having a plurality of through holes 12a for inserting each probe 11. In testing an integrated circuit, the probes 11 are brought into contact with the integrated circuit 14 formed on the wafer 13 and current is passed through to test the conductivity of the integrated circuit, the insulation between circuits, and other aspects of the integrated circuit.

[0003] For example, ceramic materials containing Si3N4 are used for probe guide components and the like (see, for example, Patent Document 1). [Prior art documents] [Patent Documents]

[0004] [Patent Document 1] Japanese Patent Publication No. 2023-73077 [Overview of the project] [Problems that the invention aims to solve]

[0005] Direct nitriding and imide pyrolysis are known methods for producing Si3N4 powder, a raw material for ceramic components. Imide pyrolysis has the problem of a complex manufacturing process and high production costs. Therefore, direct nitriding is widely used.

[0006] However, although the direct nitridation method is excellent in that it can produce Si3N4 powder at a low cost, there is a problem that the sintered body produced using this Si3N4 powder (hereinafter also referred to as a ceramic member) is likely to have color unevenness and the appearance is unstable. That is, in the prior art, there is a problem that a ceramic member excellent in appearance stability cannot be obtained.

[0007] An object of the present invention is to provide a ceramic member excellent in appearance stability.

Means for Solving the Problems

[0008] The gist of the present invention is a method for manufacturing a ceramic member as described below.

[0009] (1) A method for manufacturing a ceramic member, comprising: a heat treatment step of nitriding metallic Si by a direct nitridation method to obtain a raw material powder, preparing a mixed powder containing the raw material powder, and subjecting the mixed powder to heat treatment; and a firing step of firing the heat-treated mixed powder to obtain a ceramic member, wherein the heat treatment is carried out in a vacuum atmosphere at a heat treatment temperature of 1000 to 1400 °C for 1 to 5 h, and in the firing step, heating is carried out from the heat treatment temperature to a firing temperature and firing is carried out in a nitrogen atmosphere. A method for manufacturing a ceramic member.

[0010] (2) A method for manufacturing a ceramic member, comprising: a heat treatment step of nitriding metallic Si by a direct nitridation method to obtain a raw material powder, preparing a mixed powder containing the raw material powder, and subjecting the mixed powder to heat treatment; and a firing step of firing the heat-treated mixed powder to obtain a ceramic member, wherein the heat treatment is carried out in a nitrogen atmosphere at a heat treatment temperature of 1000 to 1400 °C for 1 to 5 h, and in the firing step, heating is carried out from the heat treatment temperature to a firing temperature and firing is carried out in a nitrogen atmosphere. A method for manufacturing a ceramic member.

Advantages of the Invention

[0011] According to the present invention, a method for manufacturing a ceramic member excellent in appearance stability can be provided.

Brief Description of the Drawings

[0012] [Figure 1] FIG. 1 is a cross-sectional view illustrating the configuration of a probe card. [Figure 2] FIG. 2 is a top view illustrating the configuration of a probe guide component. [Figure 3] FIG. 3 is a schematic view showing the surface of a ceramic member in which color unevenness has occurred. [Figure 4] FIG. 4 is a graph showing an example of an X-ray diffraction spectrum.

Embodiments for Carrying Out the Invention

[0013] In order to solve the above-described problems, the inventors of the present invention conducted a detailed investigation on the color unevenness of a ceramic member using Si3N4 powder produced by a direct nitridation method, and as a result, obtained the following findings.

[0014] First, the color unevenness that is an issue in the present invention will be described. FIG. 3 is a schematic view showing an example of the surface of a ceramic member in which color unevenness has occurred. In FIG. 3, the case where the ceramic member 15 is a rectangular plate-shaped member will be described. As shown in FIG. 3, on the surface 16 of the ceramic member 15, the color tone is different between the edge portion 17 and the central portion 18, and the central portion 18 has a darker color compared to the edge portion 17. Such a state where the color of the surface of the ceramic member 15 is not uniform is referred to as color unevenness.

[0015] Figure 3 illustrates a case where the surface 16 of the ceramic member 15 has different colors at the edges 17 and the center 18. However, the location and extent of the darkening can vary depending on the processing and shape of the ceramic member. In this invention, color unevenness refers to a state in which the surface of a ceramic member has areas that are close to white (hereinafter also referred to as "normal areas") and areas that are dark (hereinafter also referred to as "color uneven areas"), resulting in an uneven color on the surface of the ceramic member.

[0016] Referring to Figure 3, the inventors investigated the cause of color unevenness by comparing the chemical composition of the edge portion 17 and the central portion 18 on the surface 16 of the ceramic member 15. As a result, it was found that metallic Si was the main cause of the color unevenness. This metallic Si is thought to be unreacted residue from the process of producing Si3N4 powder by direct nitriding. Further investigation by the inventors revealed that color unevenness can be reduced by keeping the Si peak intensity ratio defined by equation (i) above within a predetermined range on the surface 16 of the ceramic member 15.

[0017] To reduce color unevenness, it is necessary to remove metallic Si from ceramic components. However, known methods for removing metallic Si, such as acid treatment, have the problem of high costs. Therefore, the inventors investigated a method for removing metallic Si from Si3N4 powder without acid treatment. As a result, they found that by performing heat treatment at a predetermined temperature in a vacuum atmosphere, metallic Si melts into a liquid and then evaporates, thereby removing the metallic Si. They also found that by performing heat treatment at a predetermined temperature in a nitrogen atmosphere, the metallic Si content can be reduced by nitriding the metallic Si.

[0018] This invention is based on the above findings. The requirements of this invention will be described in detail below.

[0019] <Manufacturing method according to one embodiment> A manufacturing method according to one embodiment of the ceramic component according to the present invention comprises a heat treatment step and a firing step. Each step will be described in detail below.

[0020] 1. Heat treatment process In the heat treatment process according to one embodiment of the present invention, first, metallic Si is nitrided by a direct nitriding method to obtain raw material powder. The direct nitriding method generally includes the steps of crushing metallic Si, nitriding metallic Si, crushing, and purifying. The conditions for each step can be known conditions. However, in the present invention, as described above, the purifying step is omitted in order to reduce costs. In addition, the purifying step may involve acid treatment using an acid containing Cl. As a result, Cl may be mixed into the raw material powder, and Cl may remain in the ceramic member. Therefore, the purifying step is omitted. In this way, by nitriding metallic Si by a direct nitriding method that omits the purifying step, a raw material powder containing Si3N4 and having a Cl content of 70 ppm or less can be obtained.

[0021] The raw material powders obtained in this manner, along with any additional sintering aid raw material powders and / or sintering aid powders as needed, are mixed using a known method such as a ball mill. Specifically, each powder, solvent, and ceramic or iron-cored resin balls are mixed in a container to form a slurry. At this time, the slurry is prepared so that the Si3N4 content is 85% by mass or more when the total mass of each powder is 100% by mass. Water or alcohol can be used as the solvent. Furthermore, additives such as dispersants, binders, and colorants may be used as needed.

[0022] Examples of sintering aids include alumina, yttria, and magnesia. Examples of dispersants include quaternary ammonium salts. Examples of binders include polyvinyl alcohol (PVA). Examples of colorants include elements and / or oxides of Ti, V, Zr, and / or Mo.

[0023] The obtained slurry is granulated by spray drying with a spray dryer, or powdered by drying with a vacuum evaporator. The resulting granules or powder are hereinafter referred to as mixed powder.

[0024] If a dispersant and / or binder is used, the mixed powder may be degreased. The degreasing process is performed to remove organic binders contained in the mixed powder and can be carried out by known methods, such as heating the mixed powder. For example, the degreasing process of the mixed powder is preferably carried out in air, vacuum, or in an inert gas atmosphere. Vacuum means that the pressure is in the range of 0 Pa to 1000 Pa. An inert gas atmosphere can be a nitrogen gas atmosphere or a noble gas atmosphere such as helium, neon, or argon. The temperature for degreasing the mixed powder should be set according to the type and content of organic binders contained in the mixed powder, for example, 300°C or higher, 500°C or higher, or 600°C or higher. Alternatively, the temperature for degreasing the mixed powder should usually be 1000°C or lower, or 900°C or lower. The holding time at the above temperature can be, for example, 12 hours or more, 24 hours or more, or 36 hours or more. Furthermore, the time for holding at the above temperature should be 84 hours or less, 72 hours or less, or 60 hours or less.

[0025] The mixed powder is filled into a jig of the desired shape and subjected to heat treatment in a vacuum atmosphere at a heat treatment temperature of 1000-1400°C for 1-5 hours. If the heat treatment temperature is less than 1000°C or the heat treatment time is less than 1 hour, metallic Si cannot be sufficiently removed. On the other hand, if the heat treatment temperature exceeds 1400°C in a vacuum atmosphere, thermal decomposition of Si3N4 occurs. Also, if the heat treatment time exceeds 5 hours, the manufacturing cost increases. Therefore, the heat treatment temperature is set to 1000-1400°C and the heat treatment time to 1-5 hours. The vacuum atmosphere conditions are 1.0 × 10⁻⁶ -1 It should be less than or equal to Pa.

[0026] 2. Firing process In the firing process according to one embodiment of the present invention, a ceramic member is obtained by firing the mixed powder following the heat treatment process. Specifically, the mixture is heated from the heat treatment temperature to the firing temperature and fired in a nitrogen atmosphere. The firing temperature should be in the range of 1500 to 1900°C. By using this temperature range, the mixed powder can be sufficiently sintered, and the occurrence of problems such as oxide components dissolving and the liquid phase adhering to jigs, equipment, etc., can be suppressed. As for the nitrogen atmosphere conditions, for example, the partial pressure of nitrogen gas should be 0.05 MPa or higher.

[0027] There are no specific restrictions on the timing of the change from a vacuum atmosphere to a nitrogen atmosphere. However, if the temperature exceeds 1400°C in a vacuum atmosphere, thermal decomposition of Si3N4 will occur. Therefore, it is desirable to switch from a vacuum atmosphere to a nitrogen atmosphere in a temperature range of 1400°C or lower after holding at the heat treatment temperature for 1 to 5 hours.

[0028] The firing method can be any known method, such as hot pressing or hot isostatic pressing (HIP). The applied pressure should be in the range of 5 to 50 MPa for hot pressing and 5 to 200 MPa for HIP. In addition, other known firing methods such as atmospheric pressure firing and atmospheric pressure firing may be used. The duration of the applied pressure depends on the firing temperature and dimensions, but is usually around 1 to 5 hours.

[0029] <Manufacturing method according to another embodiment> Another embodiment of the manufacturing method for the ceramic component according to the present invention comprises a heat treatment step and a firing step. Each step will be described in detail below.

[0030] 1. Heat treatment process In the heat treatment step according to another embodiment of the present invention, first, metallic Si is nitrided by a direct nitriding method to obtain a raw material powder. The method for obtaining the raw material powder is the same as the method according to the above-described embodiment, so a description is omitted.

[0031] In the heat treatment step according to another embodiment of the present invention, the mixed powder containing the obtained raw material powder is then subjected to heat treatment. Here, the method for preparing the mixed powder is the same as the method according to the above-described embodiment, so a description is omitted.

[0032] The resulting mixed powder is subjected to a heat treatment in a nitrogen atmosphere, held at a heat treatment temperature of 1000-1400°C for 1-5 hours. If the heat treatment temperature is below 1000°C or the heat treatment time is less than 1 hour, metallic Si cannot be sufficiently nitrided and thus cannot be removed. On the other hand, if the heat treatment temperature exceeds 1400°C or the heat treatment time exceeds 5 hours, the manufacturing cost increases. Therefore, the heat treatment temperature is set to 1000-1400°C and the heat treatment time to 1-5 hours. For the nitrogen atmosphere conditions, the partial pressure of the nitrogen gas should be 0.05 MPa or higher.

[0033] 3. Firing process In a firing process according to another embodiment of the present invention, the mixed powder is fired following the heat treatment process to obtain a ceramic member. Specifically, the mixture is heated from the heat treatment temperature to the firing temperature in a nitrogen atmosphere and fired. The firing temperature should be in the range of 1500 to 1900°C. This temperature range allows for sufficient sintering of the mixed powder and suppresses the occurrence of problems such as the elution of oxide components and the adhesion of the liquid phase to jigs, devices, etc. The nitrogen atmosphere conditions should be such that the partial pressure of the nitrogen gas is 0.05 MPa or higher.

[0034] The firing method can be any known method, such as hot pressing or hot isostatic pressing (HIP). The applied pressure should be in the range of 5 to 50 MPa for hot pressing and 5 to 200 MPa for HIP. In addition, other known firing methods such as atmospheric pressure firing and atmospheric pressure firing may be used. The duration of the applied pressure depends on the firing temperature and dimensions, but is usually around 1 to 5 hours.

[0035] <Composition of ceramic components> The content of Si3N4 in the ceramic member produced by the method of the present invention is 85% by mass or more. If the content of Si3N4 is less than 85% by mass, sufficient strength as a ceramic member cannot be obtained. The content of Si3N4 is more preferably 90% by mass or more. The upper limit of the content of Si3N4 is not particularly limited, but in the above-described manufacturing method, the upper limit of the content of Si3N4 is 98% by mass.

[0036] In the ceramic member according to the present invention, in addition to Si3N4, a sintering aid and / or a colorant may be included. The sintering aid can be selected from those conventionally used for sintering Si3N4. Preferred sintering aids are aluminum oxide (alumina), magnesium oxide (magnesia), yttrium oxide (yttria), oxides of lanthanoid metals, composite oxides such as spinel, and two or more of these oxides may be included. As the colorant, Ti, V, Zr, and / or Mo, alone and / or oxides thereof, may be included.

[0037] The content of Si3N4 is specified by the following method. At an arbitrary point in a region with few irregularities on the surface of the ceramic member, the amount of Si is specified using an ICP emission spectroscopic analyzer, and the content of Si3N4 is obtained by converting it to nitride.

[0038] <Cl content> As described above, in the ceramic member using the Si3N4 powder produced by the imide thermal decomposition method, the Cl content exceeds 70 ppm. In the present invention, the Si3N4 powder produced by the direct nitridation method is used. In addition, the ceramic member used for the probe guide member or the like may be required to have high fracture toughness. When the Cl content is high, the phase transition from the α-phase to the β-phase of Si3N4 is suppressed during sintering. As a result, grain growth is suppressed and the structure has a small grain size, and there is a risk that the fracture toughness value decreases. Therefore, the Cl content in the ceramic member according to the present invention is 70 ppm or less. The lower the Cl content in the ceramic member, the more preferable it is. The Cl content is preferably less than 60 ppm, more preferably 50 ppm or less, 40 ppm or less, or 30 ppm or less.

[0039] The Cl content in the ceramic member is specified by glow discharge mass spectrometry (GDMS) at an arbitrary point in a region with few irregularities on the surface of the ceramic member.

[0040] <Si peak intensity ratio> On the surface of the ceramic member produced by the method of the present invention, when measured with an X-ray diffractometer using CuKα rays as a radiation source, the Si peak intensity ratio I defined by the following formula (i) is less than 0.010. When the Si peak intensity ratio I on the surface of the ceramic member is 0.010 or more, color unevenness becomes prominent. I=(I Si -I b ) / (I β -I b ) ···(i) However, the meanings of the symbols in the above formula (i) are as follows. I Si : The intensity of the diffraction peak derived from the (111) plane of metallic Si Si : The minimum value of the X-ray diffraction intensity observed at 2θ = 28.2° to 29.1° I b : The minimum value of the X-ray diffraction intensity observed at 2θ = 28.2° to 29.1° I β:Diffraction peak intensity originating from the (200) plane of β-Si3N4

[0041] Figure 4 is a graph showing examples of X-ray diffraction spectra. (a) is an example of an X-ray diffraction spectrum in a discolored area, and (b) is an example of an X-ray diffraction spectrum in a normal area. In (a) and (b), the horizontal axis represents the measurement angle (2θ), and the vertical axis represents the peak intensity. Comparing (a) and (b), it can be seen that the peak intensity originating from the (111) plane of metallic Si is higher in the discolored area than in the normal area. Thus, even a small amount of metallic Si remaining in the sintered body causes discoloration. Therefore, in this invention, the Si peak intensity ratio I is reduced to less than 0.010.

[0042] The Si peak intensity ratio I on the surface of the ceramic member is preferably 0.009 or less, and more preferably 0.008 or less.

[0043] The Si peak intensity ratio I is measured and calculated using the following method: An X-ray diffraction spectrum is obtained using X-ray diffraction (XRD) on the surface of a ceramic component. In the measurement, the source is CuKα radiation, and the measurement angle (2θ) is set to 5-90°. The intensity I of the diffraction peak originating from the (111) plane of metallic Si, observed at approximately 2θ = 28.5°, is then calculated. Si The intensity of the diffraction peak I, which originates from the (200) plane of β-Si3N4, is measured at a position around 2θ = 27.1°. β Measure.

[0044] Furthermore, the minimum value of X-ray diffraction intensity observed at 2θ = 28.2 to 29.1 is I. b (Hereafter also referred to as "background") is measured. The I obtained in this way Si , I β , and I b Substitute the value of into equation (i) above to calculate the Si peak intensity ratio I.

[0045] Note that equation (i) above is obtained by dividing the peak intensity of metallic Si with the background subtracted by the peak intensity of β-Si3N4 with the background subtracted, and simply put, it represents the ratio of the peak intensity of metallic Si to the peak intensity of β-Si3N4.

[0046] Such measurements are taken at three points at 5 mm intervals on the surface of the central part of the ceramic member, at arbitrary points in a region with few irregularities. In this invention, a Si peak intensity ratio I of less than 0.010 on the surface of the ceramic member means that all three Si peak intensity ratios I measured as described above are less than 0.010.

[0047] <Lightness L * > On the surface of a ceramic member manufactured by the method of the present invention, the brightness L * The difference between the maximum and minimum values ​​is 2.00 or less. Brightness L on the surface of the ceramic material. * When the difference between the maximum and minimum values ​​exceeds 2.00, color unevenness becomes noticeable. (Brightness L) * The difference between the maximum and minimum values ​​is preferably 1.50 or less.

[0048] Lightness L * The following method is used for measurement: Three points are measured at 5mm intervals at arbitrary points on the surface of the ceramic component in an area with minimal irregularities, using a Konica Minolta CM-26d colorimeter, with a standard illuminant D as the light source. 65 The field of view is 10°, and the color system is L * a * b * Measurements are performed using the SCI (Specular Component Include) method, which does not remove color space or specular reflection.

[0049] <Application> The ceramic components manufactured by the method of the present invention have excellent appearance stability and are suitable for components such as probe guide components and package inspection sockets. Furthermore, probe guide components using the ceramic components according to the present invention are suitable for probe cards. A package inspection socket is a socket for holding an IC chip in order to inspect the IC chip without mounting it on a printed circuit board.

[0050] <Shape and dimensions of ceramic components> The shape of the ceramic member manufactured by the method of the present invention is not particularly limited. When used as a probe guide component, it is preferable to have a plate shape. Furthermore, the dimensions of the ceramic member according to the present invention are not particularly limited. When used as a probe guide component, it is preferable to have a length and width of 100 to 400 mm and a thickness of 0.1 to 10 mm.

[0051] The present invention will be described more specifically below with reference to examples, but the present invention is not limited to these examples. [Examples]

[0052] Si3N4 powder was prepared using the method shown in Table 1. Then, water was used as the solvent to mix a sintering aid and a dispersant with ceramic balls until the Si3N4 content reached the levels shown in Table 2. The resulting slurry was spray-dried using a spray dryer to obtain granules. After degreasing using a known method, the granules were packed into graphite dies (molds), and heat treatment and hot-press firing were performed under the conditions shown in Table 1 to obtain plate-shaped test materials (Test Nos. A1-A5, B1, and B2) measuring 300 mm (length) x 300 mm (width) x 20 mm (thickness). A quaternary ammonium salt was used as the dispersant. Acid treatment was not performed in the preparation of the Si3N4 powder. The vacuum atmosphere conditions in Table 1 were 5.0 × 10⁻⁶ -2 The setting was Pa, and the nitrogen atmosphere conditions were defined as a partial pressure of nitrogen gas of 0.1 MPa.

[0053] [Table 1]

[0054] Using the obtained test specimens, the Si peak intensity ratio, Cl content, Si3N4 content, and lightness L were examined as follows. In the following description, the "surface of the central part of the test specimen" means the central part of the surface of the test specimen with a length of 300 mm and a width of 300 mm. * The difference was examined. In the following description, the "surface of the central part of the test specimen" means the central part of the surface of the test specimen with a length of 300 mm and a width of 300 mm.

[0055] <Si3N4 content> The Si3N4 content was specified by the following method. At the surface of the central part of the test specimen, the amount of Si was specified using an ICP emission spectroscopic analyzer, and the Si3N4 content was obtained by converting it to nitride.

[0056] <Cl content> The Cl content in each test specimen was specified by GDMS at the surface of the central part of the test specimen.

[0057] <Si peak intensity ratio I> The Si peak intensity ratio I was measured and calculated by the following method. Using the surface of the central part of the test specimen as the observation surface, an X-ray diffraction spectrum was obtained by XRD. In the measurement, the radiation source was CuKα radiation, and the measurement angle (2θ) was set to 5 to 90°. Then, the intensity I of the diffraction peak derived from the (111) plane of metallic Si observed at a position near 2θ = 28.5° was measured. Si The intensity I of the diffraction peak derived from the (200) plane of β-Si3N4 observed at a position near 2θ = 27.1° was measured. β was measured.

[0058] Also, the minimum value I of the X-ray diffraction intensity observed at 2θ = 28.2 to 29.1 was measured. The I, I, and I values thus obtained were substituted into the above equation (i) to calculate the Si peak intensity ratio I. Such measurement and calculation of the Si peak intensity ratio I were performed at three points at 5 mm intervals on the surface of the central part of the test specimen, and the maximum value of the Si peak intensity ratios at the three measurement points is shown in Table 2. b obtained in this way, Si I, β and I, b were substituted into the above equation (i) to calculate the Si peak intensity ratio I. Such measurement and calculation of the Si peak intensity ratio I were performed at three points at 5 mm intervals on the surface of the central part of the test specimen, and the maximum value of the Si peak intensity ratios at the three measurement points is shown in Table 2.

[0059] <Lightness L * > Lightness L * The following method was used for measurement: Three points were measured at 5 mm intervals on the central surface of the test material using a Konica Minolta CM-26d colorimeter, with a standard illuminant D as the light source. 65 The field of view is 10°, and the color system is L * a * b * Measurements were performed using the color space and SCI method.

[0060] Table 2 shows the Si peak intensity ratio, Cl content, Si3N4 content, and brightness L for each test specimen. * The results of the difference are shown.

[0061] [Table 2]

[0062] As shown in Table 2, excellent appearance stability was obtained in Tests A1 to A5, which satisfied all the provisions of the present invention. In contrast, in Test No. B1, since no heat treatment was performed on the Si3N4 powder obtained by the direct nitriding method, the Si peak intensity ratio I was high and color unevenness occurred. In Test No. B2, the sintered body was manufactured using Si3N4 powder obtained by the imide pyrolysis method, resulting in a high Cl content. [Industrial applicability]

[0063] According to the present invention, a ceramic member with excellent appearance stability can be obtained. [Explanation of Symbols]

[0064] 10. Probe card 11. Probe 12. Probe guide component 12a.Through hole 13. Silicon wafers 14. Integrated Circuits 15. Ceramic components 16.Surface 17. Edge 18.Central part

Claims

1. A method for manufacturing ceramic members, A heat treatment step is performed in which metallic Si is nitrided by a direct nitriding method to obtain a raw material powder, a mixed powder containing the raw material powder is prepared, and the mixed powder is subjected to heat treatment. The process includes a firing step, in which the mixed powder after the heat treatment is fired to obtain a ceramic member. The aforementioned heat treatment involves holding the material in a vacuum atmosphere at a heat treatment temperature of 1000 to 1400°C for 1 to 5 hours. In the firing process, the temperature is heated from the heat treatment temperature to the firing temperature, and the firing is performed in a nitrogen atmosphere. A method for manufacturing ceramic components.

2. A method for manufacturing ceramic members, A heat treatment step is performed in which metallic Si is nitrided by a direct nitriding method to obtain a raw material powder, a mixed powder containing the raw material powder is prepared, and the mixed powder is subjected to heat treatment. The process includes a firing step, in which the mixed powder after the heat treatment is fired to obtain a ceramic member. The aforementioned heat treatment involves holding the material in a nitrogen atmosphere at a heat treatment temperature of 1000 to 1400°C for 1 to 5 hours. In the firing process, the heat is heated from the heat treatment temperature to the firing temperature in a nitrogen atmosphere, and the firing is performed. A method for manufacturing ceramic components.

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