Ceramic component and method for manufacturing the same

The ceramic member with controlled Si and Cl content, manufactured via direct nitridation and heat treatment, addresses color unevenness and cost issues, achieving stable and cost-effective ceramic components.

JP2026057834APending Publication Date: 2026-04-03FERROTEC CORPORATION
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Patent Information

Authority / Receiving Office
JP · JP
Patent Type
Applications
Current Assignee / Owner
Filing Date
2024-09-24
Publication Date
2026-04-03

AI Technical Summary

Technical Problem

Existing ceramic members made from Si3N4 powder using the direct nitridation method suffer from color unevenness and instability due to unreacted metallic Si residues, leading to appearance issues and increased manufacturing costs with acid treatment for removal.

Method used

A ceramic member composed of at least 85% Si3N4 with controlled Cl content of 70 ppm or less, manufactured through direct nitridation followed by heat treatment in a vacuum or nitrogen atmosphere to remove metallic Si, and sintered under specific conditions to maintain a Si peak intensity ratio below 0.010, ensuring uniform appearance.

Benefits of technology

The method produces ceramic members with enhanced appearance stability and reduced manufacturing costs by eliminating metallic Si and controlling Cl content, resulting in consistent color and improved fracture toughness.

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Abstract

To provide ceramic components with excellent appearance stability. [Solution] A ceramic member containing 85% by mass or more of Si3N4 and having a Cl content of 70 ppm or less, wherein when the surface of the ceramic member is measured using an X-ray diffraction apparatus with CuKα radiation as the radiation source, I=(I Si -I b ) / (I β -I b The Si peak intensity ratio I, defined by ), is less than 0.010, and the brightness L on the surface is less than 0.010. * When measuring, the brightness L * A ceramic component in which the difference between the maximum and minimum values ​​is 2.00 or less.
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Description

Technical Field

[0001] The present invention relates to a ceramic member and a method for manufacturing the same.

Background Art

[0002] In the inspection of whether an integrated circuit operates normally, for example, a probe card is used. FIG. 1 shows a cross-sectional view illustrating the configuration of a probe card, and FIG. 2 shows a top view illustrating the configuration of a probe guiding component. As shown in FIGS. 1 and 2, the probe card 10 includes needle-like probes 11 and a probe guiding component 12 having a plurality of through-holes 12a for inserting each probe 11. In the inspection of an integrated circuit, the probes 11 are brought into contact with the integrated circuit 14 formed on the wafer 13 to allow current to flow, thereby performing inspections such as conduction of the integrated circuit and insulation between circuits.

[0003] For probe guiding components and the like, for example, a ceramic material containing Si3N4 is used (for example, Patent Document 1).

Prior Art Documents

Patent Documents

[0004]

Patent Document 1

Summary of the Invention

Problems to be Solved by the Invention

[0005] As methods for manufacturing Si3N4 powder, which is a raw material of a ceramic member, a direct nitridation method and an imide thermal decomposition method are known. The imide thermal decomposition method has problems such as a complicated manufacturing process and an increase in manufacturing cost. Therefore, the direct nitridation method is widely adopted.

[0006] However, although the direct nitridation method is excellent in that it can produce Si3N4 powder at a low cost, the sintered body produced using this Si3N4 powder (hereinafter also referred to as a ceramic member) has a problem that color unevenness is likely to occur and the appearance is unstable.

[0007] That is, in the prior art, there is a problem that a ceramic member excellent in appearance stability cannot be obtained.

[0008] An object of the present invention is to provide a ceramic member excellent in appearance stability.

Means for Solving the Problems

[0009] The gist of the present invention is the following ceramic member and a method for manufacturing the same.

[0010] (1) A ceramic member containing 85% by mass or more of Si3N4 and having Cl of 70 ppm or less, When the surface of the ceramic member is measured with an X-ray diffractometer using CuKα ray as a radiation source, the Si peak intensity ratio I defined by the following formula (i) is less than 0.010, the brightness L on the surface * when measured, the difference between the maximum value and the minimum value of the brightness L * is 2.00 or less, a ceramic member. 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 I b : The minimum value of the X-ray diffraction intensity observed at 2θ = 28.2° to 29.1° I β : The diffraction peak intensity derived from the (200) plane of β-Si3N4

[0011] (2) The ceramic member described in (1) above, which is used as a probe guide component.

[0012] (3) A method for manufacturing a ceramic member as described in (1) above, A heat treatment step involves heat-treating a raw material powder obtained by nitriding metallic Si using a direct nitriding method to obtain a heat-treated powder. The process includes a sintering step of sintering a mixed powder containing the heat-treated powder to obtain a ceramic member, The heat treatment involves holding the raw material powder in a vacuum atmosphere or nitrogen atmosphere at a temperature range of 1000 to 1400°C for 1 to 5 hours. A method for manufacturing ceramic components. [Effects of the Invention]

[0013] According to the present invention, it is possible to provide a ceramic member with excellent appearance stability and a method for manufacturing the same. [Brief explanation of the drawing]

[0014] [Figure 1] Figure 1 is a cross-sectional view illustrating the configuration of a probe card. [Figure 2] Figure 2 is a top view illustrating the configuration of the probe guide component. [Figure 3] Figure 3 is a schematic diagram showing an example of the surface of a ceramic component where color unevenness has occurred. [Figure 4] Figure 4 is a graph showing an example of an X-ray diffraction spectrum. [Modes for carrying out the invention]

[0015] In order to solve the aforementioned problems, the inventors conducted a detailed investigation into the color unevenness of ceramic components using Si3N4 powder manufactured by direct nitriding, and as a result obtained the following findings.

[0016] First, let's explain the color unevenness that is the problem addressed in this invention. Figure 3 is a schematic diagram showing an example of the surface of a ceramic member where color unevenness has occurred. In Figure 3, we will explain the case where the ceramic member 15 is a rectangular plate-shaped member. As shown in Figure 3, on the surface 16 of the ceramic member 15, the color differs between the edge 17 and the central part 18, with the central part 18 being darker than the edge 17. This state in which the color of the surface of the ceramic member 15 is not uniform is called color unevenness.

[0017] 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.

[0018] 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.

[0019] 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.

[0020] Furthermore, although the present invention targets sintered bodies manufactured using Si3N4 powder obtained by direct nitriding, it has been found that Si3N4 powder manufactured by imide pyrolysis has a higher Cl content than Si3N4 powder manufactured by direct nitriding. Therefore, in the ceramic members according to the present invention, the Cl content is specified to be 70 ppm or less.

[0021] This invention is based on the above findings. The requirements of this invention will be described in detail below.

[0022] <Composition of ceramic components> The ceramic component according to the present invention contains 85% by mass or more of Si3N4. If the Si3N4 content is less than 85% by mass, sufficient strength cannot be obtained as a ceramic component. It is more preferable that the Si3N4 content be 90% by mass or more. Furthermore, there is no particular upper limit to the Si3N4 content, but in the manufacturing method described later, the upper limit of the Si3N4 content is 98% by mass.

[0023] The ceramic member according to the present invention may contain, in addition to Si3N4, a sintering aid and / or a coloring agent. 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 coloring agent, simple substances and / or oxides of Ti, V, Zr, and / or Mo may be included.

[0024] 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.

[0025] <Cl content>[[ID=⑨]] As described above, in the ceramic member using Si3N4 powder produced by the imide thermal decomposition method, the Cl content exceeds 70 ppm. In the present invention, Si3N4 powder produced by the direct nitridation method is used. In addition, a ceramic member used for a probe guide component or the like may be required to have high fracture toughness. When the Cl content is high, the phase transition of Si3N4 from the α-phase to the β-phase is suppressed during sintering. As a result, grain growth is suppressed and the structure has a small particle size, which may reduce the fracture toughness value. Therefore, the Cl content in the ceramic member according to the present invention is set to 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.

[0026] 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.

[0027] <Si peak intensity ratio> When measuring the surface of a ceramic component using an X-ray diffractometer with CuKα radiation as the source, the Si peak intensity ratio I, defined by equation (i) below, should be less than 0.010. If the Si peak intensity ratio I on the surface of the ceramic component is 0.010 or higher, color unevenness becomes noticeable. I=( I Si -I b ) / (I β -I b ) ···(i) However, the meaning of each symbol in equation (i) above is as follows: I Si :I Si : Intensity of diffraction peaks originating from the (111) plane of metallic Si I b Minimum 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

[0028] 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 trace 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.

[0029] 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.

[0030] 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.

[0031] 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.

[0032] 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.

[0033] Such measurements are taken at three points at 5 mm intervals in an area of ​​the ceramic member's surface with minimal 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.

[0034] <Lightness L * > Brightness L on the surface of a ceramic component * When the difference between the maximum and minimum values ​​exceeds 2.00, significant color unevenness occurs. Therefore, in the present invention, the brightness L on the surface of the ceramic member is * The difference between the maximum and minimum values ​​shall be 2.00 or less. Brightness L* The difference between the maximum and minimum values ​​is preferably 1.50 or less.

[0035] 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.

[0036] <Application> The ceramic member according to the present invention has excellent appearance stability and is suitable for components such as probe guide components and package inspection sockets. Furthermore, a probe guide component using the ceramic member according to the present invention is 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.

[0037] <Shape and dimensions of ceramic components> The shape of the ceramic member according to 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.

[0038] <Manufacturing method> The ceramic component according to the present invention can be stably manufactured by the following method.

[0039] 1. Heat treatment process In the heat treatment process, first, metallic Si is nitrided by direct nitriding to obtain the raw material powder. Direct nitriding generally includes the steps of crushing metallic Si, nitriding metallic Si, crushing, and refining. The conditions for each step can be known conditions. However, in this invention, as mentioned above, the refining step is omitted in order to reduce costs. In addition, the refining 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 component. Therefore, the refining step is omitted. In this way, by nitriding metallic Si by direct nitriding without the refining step, a raw material powder containing Si3N4 and having a Cl content of 70 ppm or less can be obtained.

[0040] In the heat treatment process, the obtained raw material powder is then subjected to heat treatment to obtain heat-treated powder. The heat treatment conditions are to maintain a temperature range of 1000 to 1400°C for 1 to 5 hours in a vacuum atmosphere or a nitrogen atmosphere. If the heat treatment temperature is less than 1000°C, or if 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. Furthermore, if the heat treatment time exceeds 5 hours, or if the heat treatment temperature exceeds 1400°C in a nitrogen atmosphere, the manufacturing cost increases. Therefore, the heat treatment temperature is set to 1000 to 1400°C, and the heat treatment time to 1 to 5 hours. The vacuum atmosphere conditions are 1.0 × 10 -1 The pressure should be below Pa. Furthermore, for the nitrogen atmosphere, for example, the partial pressure of nitrogen gas should be 0.05 MPa or higher.

[0041] Furthermore, the heat-treated powder after the heat treatment process is preferably Si3N4 and has the following characteristics. The heat-treated powder preferably has a Cl content of 70 ppm or less, and when the heat-treated powder is measured using an X-ray diffraction apparatus with CuKα radiation as the source, the Si peak intensity ratio I' defined by the following equation (ii) is preferably less than 0.029. I'=(I' Si -I' b ) / (I' α -I' b ) ···(ii) However, the meaning of each symbol in equation (ii) above is as follows: I' Si : Intensity of diffraction peaks originating from the (111) plane of metallic Si I' b Minimum X-ray diffraction intensity observed at 2θ = 28.2° to 29.1° I' α :Diffraction peak intensity originating from the (101) plane of α-Si3N4

[0042] The Si peak intensity ratio I' mentioned above is measured and calculated using the following method: An X-ray diffraction spectrum is obtained from the heat-treated powder by XRD. In the measurement, the radiation source is CuKα, and the measurement angle (2θ) is set to 5-90°.

[0043] Furthermore, the intensity I' of the diffraction peak originating from the (111) plane of metallic Si is observed at a position around 2θ = 28.5°. Si The intensity I' of the diffraction peak originating from the (101) plane of α-Si3N4, observed at a position around 2θ = 20.6°, is measured. α The minimum value I' of the X-ray diffraction intensity observed at 2θ = 28.2 to 29.1 is measured. b Measure the I' obtained in this way. Si , I' α , and I' b Substitute the value of into equation (ii) above to calculate the Si peak intensity ratio I'.

[0044] 2. Sintering process In the sintering process, a slurry containing heat-treated powder is sintered to obtain a ceramic component. The heat-treated powder, and, if necessary, sintering aid raw material powder and / or sintering aid powder are mixed by 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 adjusted 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.

[0045] 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.

[0046] 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.

[0047] 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.

[0048] The mixed powder is filled into a jig of the desired shape and sintered under high temperature and pressure using known methods such as hot pressing or HIP (hot isostatic pressing) to obtain a ceramic component. When firing by hot pressing, firing can be performed in a nitrogen atmosphere or in pressurized nitrogen. The firing temperature should be in the range of 1200 to 1900°C. This temperature range allows for sufficient sintering of the mixed powder and suppresses the problem of oxide components leaching out and the liquid phase adhering to the jig, equipment, etc. Furthermore, the applied pressure should be in the range of 5 to 50 MPa for hot pressing and 5 to 200 MPa for HIP. The duration of the applied pressure depends on the firing temperature and dimensions, but in either case, it is usually about 1 to 5 hours.

[0049] Even when firing by HIP, firing conditions such as temperature and pressure can be set appropriately. In addition, known firing methods such as atmospheric pressure firing and atmospheric pressure firing may be employed. In this way, the ceramic member according to the present invention can be obtained.

[0050] The ceramic members according to the present invention will be described in more detail below with reference to examples, but the embodiments are not limited to these examples. [Examples]

[0051] Si3N4 powder was prepared using the method shown in Table 1. The Si3N4 powder was then heat-treated at the temperatures and times listed in Table 1, and the Si peak intensity ratio I' was calculated using the method described later. Subsequently, water was used as the solvent to mix a sintering aid and a dispersant with ceramic balls, so that the Si3N4 content was as shown in Table 2. The resulting slurry was spray-dried using a spray dryer to obtain granules. After degreasing using a known method, the obtained granules were packed into graphite dies (molds) and hot-pressed under the conditions shown in Table 1 to obtain plate-shaped test materials (Test Nos. A1-A5 and B1-B3) measuring 300mm x 300mm x 20mm thick. A quaternary ammonium salt was used as the dispersant. The vacuum atmosphere conditions 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.

[0052] <Si peak intensity ratio I´> The Si peak intensity ratio I´ was measured and calculated by the following method. For the heat-treated powder, 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° Si was measured. The intensity I´ of the diffraction peak derived from the (101) plane of α-Si3N4 observed at a position near 2θ = 20.6° α was measured. Also, the minimum value I´ of the X-ray diffraction intensity observed at 2θ = 28.2 to 29.1 b was measured. The I´ Si , I´ α , and I´ b values obtained were substituted into the above equation (ii) to calculate the Si peak intensity ratio I´.

[0053]

Table 1

[0054] Using the obtained test specimens, the Si peak intensity ratio, Cl content, Si3N4 content, and difference in 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.

[0055] <Si3N4 content> The Si3N4 content was specified by the following method. On 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 on 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 using the following method. The central surface of the test material was used as the observation plane, and an X-ray diffraction spectrum was obtained by XRD. In the measurement, the radiation source was CuKα, and the measurement angle (2θ) was 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°, was then calculated. Si The intensity of the diffraction peak I, originating from the (200) plane of β-Si3N4, was measured. β We measured it.

[0058] Furthermore, the minimum value of X-ray diffraction intensity observed at 2θ = 28.2 to 29.1 is I. b The following was measured. Si , I β , and I b The Si peak intensity ratio I was calculated by substituting the value of into equation (i) above. This measurement and calculation of the Si peak intensity ratio I was performed at three points on the central surface of the test material at 5 mm intervals, and the maximum value of the Si peak intensity ratio 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 A4, which satisfied all the provisions of the present invention. In contrast, in Test No. B1, since the Si3N4 powder obtained by the direct nitriding method was not heat-treated, 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. In Test No. B3, although Si3N4 powder was manufactured by the direct nitriding method, the Cl content was high because it was acid-treated. [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. 85% by mass or more of Si 3 N 4 A ceramic member containing a certain substance and having a Cl content of 70 ppm or less, When the surface of the ceramic member is measured using an X-ray diffraction apparatus with CuKα radiation as the source, the Si peak intensity ratio I, defined by the following equation (i), is less than 0.

010. Brightness L of the aforementioned surface * When measured, the brightness L * The difference between the maximum and minimum values ​​is 2.00 or less. Ceramic components. I=(I Si -I b ) / (I β -I b ) ・・・(i) However, the meaning of each symbol in equation (i) above is as follows: I Si : Intensity of diffraction peak derived from (111) plane of metallic Si I b : Minimum X-ray diffraction intensity observed between 2θ = 28.2° and 29.1° I β : β-Si 3 N 4 Diffraction peak intensity originating from the (200) plane

2. A ceramic member according to claim 1, used as a probe guide component.

3. A method for manufacturing a ceramic member according to claim 1, A heat treatment step involves heat-treating a raw material powder obtained by nitriding metallic Si using a direct nitriding method to obtain a heat-treated powder. The process includes a sintering step of sintering a mixed powder containing the heat-treated powder to obtain a ceramic member, The heat treatment involves holding the raw material powder in a vacuum atmosphere or nitrogen atmosphere at a temperature range of 1000 to 1400°C for 1 to 5 hours. A method for manufacturing ceramic components.

Citation Information

Patent Citations

  • Silicon nitride composite material and probe-guiding component

    JP2023073077A