Semiconductor manufacturing equipment components
By incorporating a spinel-containing surface layer and a tungsten carbide-titanium nitride skeleton in the conductor of semiconductor manufacturing equipment components, the issue of conductivity variations is addressed, resulting in a more uniform and stable electrical conductivity.
Patent Information
- Application Number
- JP2025528643
- Authority / Receiving Office
- JP · JP
- Patent Type
- Patents
- Current Assignee / Owner
- Priority Date
- 2024-05-27
- Filing Date
- 2025-01-22
- Publication Date
- 2025-09-30
- Estimated Expiration
- 2045-01-22
AI Technical Summary
Semiconductor manufacturing equipment components experience local variations in electrical conductivity due to uneven distribution of spinel in the conductor, which affects the uniformity and efficiency of electrical conductivity.
A semiconductor manufacturing equipment member with a ceramic substrate and conductor that includes a surface layer containing spinel and a skeleton made of tungsten carbide and titanium nitride, where the spinel is concentrated at the interface between the ceramic substrate and the conductor to stabilize electrical conductivity and improve uniformity.
The configuration achieves a conductor with enhanced uniformity and stability in electrical conductivity, ensuring efficient and uniform application of voltage across the conductor.
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Abstract
Description
[Technical Field]
[0001] The present invention relates to a member for a semiconductor manufacturing device. [Background technology]
[0002] Conventionally, semiconductor manufacturing equipment for manufacturing semiconductor devices includes various components according to their functions. Such semiconductor manufacturing equipment may use a component for semiconductor manufacturing equipment that includes a ceramic base and a conductor disposed within the ceramic base. As such a component for semiconductor manufacturing equipment, for example, a substrate holder has been proposed in which the ceramic base material is made from ceramic raw material powder containing aluminum nitride and magnesium oxide, and the conductor is made from a conductive paste containing tungsten carbide and aluminum oxide (see Patent Document 1). [Prior art documents] [Patent documents]
[0003] [Patent Document 1] Patent No. 5032444 Summary of the Invention [Problem to be solved by the invention]
[0004] However, in the semiconductor manufacturing equipment member described in Patent Document 1, local variations in electrical conductivity (hereinafter referred to as conductivity variations) may occur in the conductor, which may prevent the desired function from being fully exhibited. A primary object of the present invention is to provide a semiconductor manufacturing equipment member having a conductor with excellent uniformity in electrical conductivity. [Means for solving the problem]
[0005] [1] A semiconductor manufacturing equipment member according to an embodiment of the present invention includes a ceramic substrate and an electric conductor. The electric conductor is provided within the ceramic substrate. The ceramic substrate has a thermal expansion coefficient of 2.0×10 -6 / ℃~10.0×10 -6 The conductor includes a ceramic material having a temperature of 1000° C. / ° C. and a spinel. The conductor has a surface layer containing the spinel and a skeleton located inside the surface layer. [2] In the semiconductor manufacturing equipment member described in [1] above, the skeleton may be made of tungsten carbide and titanium nitride. [3] In the semiconductor manufacturing equipment member described in [2] above, the tungsten carbide content in the skeleton may be 50 wt% to 99 wt%, and the titanium nitride content in the skeleton may be 1 wt% to 50 wt%. [4] In the semiconductor manufacturing equipment member described in [1] above, the skeleton may be made of molybdenum. [5] In the semiconductor manufacturing equipment member according to any one of [1] to [4] above, in a line analysis using an electron probe microanalyzer on a cross section of the ceramic base material on which the conductor is provided, cut in the thickness direction, the average Mg intensity of the surface layer may be three times or more higher than the average Mg intensity of the skeleton. (Line Analysis) The ceramic substrate provided with the conductor is cut in the thickness direction to form a cross section including the conductor; three measurement lines extending in the thickness direction and passing through the conductor are set in the cross section at intervals from each other in a direction perpendicular to the thickness direction; the intensity of Mg characteristic X-rays in each of the three measurement lines is measured using an electron beam microanalyzer; the distance from the first end to the second end of each measurement line is plotted against the intensity of Mg characteristic X-rays to create a Mg characteristic X-ray spectrum for each measurement line; in the Mg characteristic X-ray spectrum, the maximum intensity of a peak located at the interface between the ceramic substrate and the conductor is defined as the Mg intensity of the surface layer, and an average value is calculated from the Mg intensities of the surface layer in the three measurement lines; in the Mg characteristic X-ray spectrum, the maximum intensity of a peak located inside the conductor is defined as the Mg intensity of the skeleton, and an average value is calculated from the Mg intensities of the skeleton in the three measurement lines. [6] In the semiconductor manufacturing equipment member according to any one of [1] to [5] above, the ceramic base may further contain titanium nitride. [7] In the semiconductor manufacturing equipment member described in [6] above, the content of spinel in the ceramic base may be 0.5 wt% to 55 wt%, and the content of titanium nitride in the ceramic base may be 0.1 wt% to 1.0 wt%. [8] In the semiconductor manufacturing equipment member according to any one of [1] to [7] above, the dimension of the conductor in the thickness direction of the ceramic base may be 10 μm to 50 μm. [9] In the semiconductor manufacturing equipment member according to any one of [1] to [8] above, the conductor may be obtained by printing.
[10] The semiconductor manufacturing equipment member according to any one of [1] to [9] above may include, as the conductor, an electrode and / or a resistance heating element, and a terminal portion, which is electrically connected to the electrode and / or the resistance heating element. [Effects of the Invention]
[0006] According to an embodiment of the present invention, a semiconductor manufacturing equipment member having a conductor with excellent uniformity of electrical conductivity can be realized. [Brief explanation of the drawings]
[0007] [Figure 1] FIG. 1 is a schematic cross-sectional view of a heater as a semiconductor manufacturing equipment member according to one embodiment of the present invention. [Figure 2] FIG. 2 is a schematic cross-sectional view of an electrostatic chuck according to another embodiment of the present invention. [Figure 3] FIG. 3 shows a Mg characteristic X-ray spectrum for the heater for semiconductor manufacturing equipment of Example 1. [Figure 4] FIG. 4 shows the Mg characteristic X-ray spectrum of the heater for semiconductor manufacturing equipment of Comparative Example 1. [Figure 5] FIG. 5 is a schematic cross-sectional view of a semiconductor manufacturing equipment member according to still another embodiment of the present invention. [Figure 6A] 6A is a schematic perspective view of an example of a terminal portion included in the semiconductor manufacturing equipment member of FIG. 5. FIG. [Figure 6B] FIG. 6B is a schematic plan view of the terminal portion of FIG. 6A. [Figure 7A] 7A is a schematic perspective view of a modified example of the terminal portion included in the semiconductor manufacturing equipment member of FIG. [Figure 7B] FIG. 7B is a schematic plan view of the terminal portion of FIG. 7A. [Figure 8A] 8A is a schematic perspective view of another modified example of the terminal portion included in the semiconductor manufacturing equipment member of FIG. [Figure 8B] FIG. 8B is a schematic plan view of the terminal portion of FIG. 8A. DETAILED DESCRIPTION OF THE INVENTION
[0008] Hereinafter, embodiments of the present invention will be described, but the present invention is not limited to these embodiments. In addition, in order to clarify the explanation, the width, thickness, shape, etc. of each part may be shown schematically in the drawings compared to the embodiments, but this is merely an example and does not limit the interpretation of the present invention.
[0009] A. Overview of semiconductor manufacturing equipment components FIG. 1 is a schematic cross-sectional view of a heater as a semiconductor manufacturing equipment member according to one embodiment of the present invention. The semiconductor manufacturing equipment member 100 is typically a component of semiconductor manufacturing equipment for manufacturing semiconductor devices. The semiconductor manufacturing equipment member 100 is an industrially applicable device that can be distributed independently.
[0010] As shown in FIG. 1, in one embodiment, a semiconductor manufacturing equipment member 100 includes a ceramic base 1 and a conductor 2. The ceramic base 1 typically has a mounting surface 1a on which a semiconductor substrate 8 can be mounted. The mounting surface 1a is one surface of the ceramic base 1 in the thickness direction. The ceramic base 1 has a thermal expansion coefficient of 2.0×10 -6 / ℃~10.0×10 -6 / °C ceramic material and spinel. The conductor 2 is provided in the ceramic substrate 1. The conductor 2 has a surface layer 21 and a skeleton 22. The surface layer 21 of the conductor 2 contains spinel. In other words, the surface layer 21 contains a spinel crystal phase. The skeleton 22 of the conductor 2 is located inside the surface layer 21. In other words, the skeleton 22 is located on the opposite side of the ceramic substrate 1 from the surface layer 21. The present inventors have discovered that in a semiconductor manufacturing equipment component having a conductor provided within a ceramic substrate, uneven distribution of spinel within the conductor causes variations in electrical conductivity in the conductor. Consequently, after extensive research into the location of spinel, they have found that forming a surface layer containing spinel on the conductor can reduce variations in electrical conductivity in the conductor and improve the uniformity of the electrical conductivity of the conductor. More specifically, since the surface layer containing spinel is located at the interface between the skeleton of the conductor and the ceramic substrate, it is possible to suppress the diffusion of Mg into the skeleton of the conductor and the formation of spinel in the skeleton of the conductor, thereby improving the electrical conductivity of the conductor and suppressing variations in electrical conductivity. Furthermore, since the surface layer containing spinel is located at the interface between the ceramic substrate and the skeleton of the conductor, it is possible to improve the adhesion between the ceramic substrate and the skeleton of the conductor.
[0011] The surface layer 21 of the conductor 2 may be provided continuously over the entire interface between the ceramic substrate 1 and the skeleton 22 of the conductor 2, or may be provided partially at the interface between the ceramic substrate 1 and the skeleton 22 of the conductor 2. In the illustrated example, the surface layer 21 is provided continuously over the entire interface between the ceramic substrate 1 and the skeleton 22, and surrounds the periphery of the conductor 2. With this configuration, it is possible to stably suppress the diffusion of Mg into the skeleton of the conductor. The thickness of the surface layer 21 is, for example, 0.5 μm to 10 μm, preferably 2.0 μm to 8.0 μm, and more preferably 2.0 μm to 6.0 μm. The thickness of the surface layer 21 is measured, for example, by an electron probe microanalyzer (EPMA).
[0012] The skeleton 22 of the conductor 2 is typically surrounded by a surface layer 21. The skeleton 22 of the conductor 2 is typically made of a conductive material having a volume resistivity lower than that of spinel.
[0013] Such conductive materials include, for example, metal carbide compounds such as tungsten carbide (WC), metal nitride compounds such as titanium nitride (TiN), and transition metals such as molybdenum (Mo), tantalum (Ta), tungsten (W), platinum (Pt), rhenium (Re), and hafnium (Hf). The conductive materials may be used alone or in combination.
[0014] In one embodiment, the skeleton 22 of the conductor 2 is composed of tungsten carbide (WC) and titanium nitride (TiN). In other words, the skeleton 22 of the conductor 2 contains a WC crystalline phase and a TiN crystalline phase. When the skeleton of the conductor is composed of WC and TiN, the volume resistivity of the conductor's skeleton can be stably made smaller than the volume resistivity of the surface layer containing spinel. As a result, the surface layer of the conductor can sufficiently prevent the current flowing through the conductor's skeleton from leaking to the ceramic substrate. This allows voltage to be applied efficiently and uniformly across the entire conductor.
[0015] When the skeleton 22 of the conductor 2 is composed of WC and TiN, the WC content in the skeleton 22 of the conductor 2 is, for example, 50.0 wt% to 99.0 wt%, preferably 90.0 wt% to 99.0 wt%, more preferably 93.0 wt% to 98.0 wt%, and even more preferably 95.0 wt% to 97.0 wt%. The content of TiN in the skeleton 22 of the conductor 2 is, for example, 1.0 wt% to 50.0 wt%, and preferably 1.0 wt% to 5.0 wt%, calculated as oxide. When the content of WC and / or TiN in the skeleton of the conductor falls within this range, the volume resistivity of the skeleton of the conductor can be made sufficiently smaller than the volume resistivity of the surface layer. The content ratio of the constituent elements in the conductor is measured, for example, by ICP-AES (inductively coupled plasma atomic emission spectroscopy) in accordance with JIS-K0116.
[0016] In another embodiment, the skeleton 22 of the conductor 2 is made of molybdenum (Mo). In other words, the skeleton 22 of the conductor 2 includes a Mo crystalline phase. When the skeleton 22 of the conductor 2 is made of Mo, the content of Mo in the skeleton 22 of the conductor 2 is, for example, 95.0 wt % to 99.9 wt %.
[0017] The spinel content in the skeleton 22 of the conductor 2 is typically lower than the spinel content in the surface layer 21 of the conductor 2. The spinel content correlates with the Mg intensity measured using an electron probe microanalyzer (EPMA).
[0018] The Mg concentration in each of the surface layer 21 and the skeleton 22 of the conductor 2 is measured as Mg intensity in the following line analysis using, for example, an electron probe microanalyzer (EPMA). (Line Analysis) (1) First, the ceramic substrate 1 on which the conductor 2 is provided is cut in the thickness direction to form a cross section including the conductor 2. (2) Next, a plurality of measurement lines are set on the cross section, extending in the thickness direction of the ceramic substrate 1 and passing through the conductor 2. The plurality of measurement lines are positioned at arbitrary intervals from one another in a direction perpendicular to the thickness direction of the ceramic substrate 1. The number of measurement lines is typically three. Each of the plurality of measurement lines has a first end located between the mounting surface 1a of the ceramic substrate 1 and the conductor 2, and a second end located on the opposite side of the conductor 2 from the first end. (3) Next, the intensity of the Mg characteristic X-rays is measured for each of the multiple measurement lines using an EPMA. The distance from the first end to the second end of the measurement line is plotted against the intensity of the Mg characteristic X-rays, with the X-axis representing the distance from the first end to the second end of the measurement line and the Y-axis representing the intensity of the Mg characteristic X-rays, to create a Mg characteristic X-ray spectrum. (4) Then, in each of the multiple Mg characteristic X-ray spectra, the maximum intensity of the peak located at the interface between the ceramic substrate 1 and the conductor 2 is extracted as the Mg intensity of the surface layer 21. The highest numerical value among the Mg intensities of the surface layer 21 extracted from the multiple Mg characteristic X-ray spectra is determined as the maximum value of the Mg intensity of the surface layer 21. Furthermore, in each of the multiple Mg characteristic X-ray spectra, the maximum intensity of the peak located inside the conductor 2 is extracted as the Mg intensity of the skeleton 22. The highest numerical value among the Mg intensities of the skeleton 22 extracted from the multiple Mg characteristic X-ray spectra is taken as the maximum value of the Mg intensity of the skeleton 22.
[0019] In the above line analysis using EPMA, the maximum value of the Mg intensity in the skeleton 22 of the conductor 2 is typically smaller than the maximum value of the Mg intensity in the surface layer 21 of the conductor 2 . In the above line analysis using EPMA, the maximum value of the Mg intensity of the skeleton 22 of the conductor 2 is, for example, 5000 or less, preferably 3000 or less, and more preferably 2000 or less. On the other hand, in the above line analysis using EPMA, the maximum value of the Mg intensity of the skeleton 22 of the conductor 2 is, for example, 500 or more. In the above line analysis using EPMA, the maximum value of the Mg intensity of the surface layer 21 of the conductor 2 is, for example, 3000 or more, preferably 4000 or more. On the other hand, in the above line analysis using EPMA, the maximum value of the Mg intensity of the surface layer 21 of the conductor 2 is, for example, 20000 or less. If the maximum values of the Mg intensities of the surface layer and skeleton of the conductor are within these ranges, the electrical conductivity of the conductor can be further improved, and variations in the conductivity of the conductor can be stably suppressed.
[0020] In the above-mentioned line analysis, the average value of the Mg intensity of the multiple surface layers 21 is, for example, 2.5 times or more, preferably 3.0 times or more, and more preferably 3.5 times or more, the average value of the Mg intensity of the multiple skeletons 22. When the ratio of the average Mg intensity of the surface layer to the average Mg intensity of the skeleton is within this range, the electrical conductivity of the conductor can be further improved and the variation in conductivity of the conductor can be more stably suppressed. On the other hand, the average value of the Mg intensity of the surface layer 21 is, for example, 13 times or less, or, for example, 12 times or less, the average value of the Mg intensity of the skeleton 22 .
[0021] The thickness of such an electric conductor 2 (the dimension in the thickness direction of the ceramic base 1) is, for example, 10 μm to 50 μm, and preferably 20 μm to 30 μm.
[0022] B. Details of semiconductor manufacturing equipment components Each component of the semiconductor manufacturing equipment will be described in detail below.
[0023] B-1. Ceramic substrate The ceramic base 1 may have any appropriate shape depending on the application of the heater for semiconductor manufacturing equipment. A typical shape of the ceramic base 1 is a plate shape. The ceramic base 1 preferably has a disk shape. The thickness of the ceramic base 1 is, for example, 10 mm to 50 mm.
[0024] The ceramic substrate 1 typically has a thermal expansion coefficient of 2.0×10 -6 / ℃~10.0×10 -6 It is composed of a composite sintered body containing ceramic material and spinel at 1000K / ℃. Thermal expansion coefficient is 2.0 x 10 -6 / ℃~10.0×10 -6 Examples of ceramic materials that can be used at temperatures above 100°C include aluminum nitride (AlN) and alumina (Al2O3). These ceramic materials can be used alone or in combination.
[0025] The absolute value of the difference in thermal expansion coefficient between the ceramic material and the conductive material constituting the conductor 2 is, for example, 0.3 ppm / °C or less, preferably 0.2 ppm / °C or less, in the range of 40°C to 100°C. On the other hand, the lower limit of the absolute value of the difference in thermal expansion coefficient between the ceramic material and the conductive material is typically 0.03 ppm / °C. When the absolute value of the difference in thermal expansion coefficient between the ceramic material and the conductive material is in this range, damage such as cracks can be sufficiently suppressed in the ceramic base material during the manufacture of semiconductor manufacturing equipment components.
[0026] In one embodiment, the ceramic substrate 1 is composed of a composite sintered body containing aluminum nitride (AlN) and spinel. In other words, the ceramic substrate 1 contains an AlN crystalline phase and a spinel crystalline phase. The crystalline phase in the ceramic substrate is measured, for example, by XRD (X-ray diffraction) in accordance with JIS Z2201 and JIS K0114.
[0027] In one embodiment, the ceramic substrate 1 has a polycrystalline structure including a plurality of AlN crystal grains. Among the plurality of AlN crystal grains, adjacent AlN crystal grains are typically bonded to each other. The average grain size of the plurality of AlN crystal grains is, for example, 1 μm to 5 μm, and preferably 1 μm to 3 μm.
[0028] The AlN content in the ceramic base 1 is, for example, 50.0 wt% or more, preferably 55 wt% or more, more preferably 95.0 wt% or more, even more preferably 97.0 wt% or more, and particularly preferably 98.0 wt% or more. On the other hand, the AlN content in the ceramic base 1 is, for example, 99.8 wt% or less, preferably 99.5 wt% or less, and more preferably 99.0 wt% or less. When the content of AlN in the ceramic substrate is within this range, high thermal conductivity, high toughness, and high dielectric strength voltage can be achieved. The content ratio of the composition elements in the ceramic substrate is measured, for example, by ICP-AES (inductively coupled plasma atomic emission spectroscopy) in accordance with JIS-K0116.
[0029] Spinel typically exists at the grain boundaries between AlN crystal grains, or is formed by the reaction of magnesium oxide and aluminum oxide at the grain boundaries between AlN crystal grains. The content of spinel in the ceramic substrate 1, calculated as oxide, is, for example, 0.1 wt% or more, preferably 0.4 wt% or more, more preferably 0.5 wt% or more, and even more preferably 0.8 wt% or more. On the other hand, the content of spinel in the ceramic substrate 1, calculated as oxide, is, for example, 55 wt% or less, preferably 50 wt% or less, more preferably 45 wt% or less, and even more preferably 1.2 wt% or less. When the content of the spinel in the ceramic base is within this range, the volume resistivity of the ceramic base can be stably improved in the high temperature range.
[0030] In one embodiment, the ceramic substrate 1 further contains titanium nitride (TiN). In other words, the ceramic substrate 1 contains a TiN crystalline phase in addition to the AlN crystalline phase and the spinel crystalline phase. TiN is typically present at the grain boundaries between AlN crystal grains.
[0031] When the ceramic substrate 1 and the skeleton 22 of the conductor 2 each contain TiN, the content of TiN in the ceramic substrate 1 is typically lower than the content of TiN in the skeleton 22 of the conductor 2 . The content of TiN in the ceramic base 1, calculated as oxide, is, for example, 0.01 wt% or more, preferably 0.1 wt% or more, and more preferably 0.3 wt% or more. On the other hand, the content of TiN in the ceramic base 1, calculated as oxide, is, for example, 1.0 wt% or less, and preferably 0.8 wt% or less. When the content of TiN in the ceramic base is within this range, the formation of conductive paths in the grain boundary layers is suppressed, and a decrease in the resistivity of the ceramic base is suppressed, which is preferable.
[0032] The ceramic substrate 1 may further contain other crystal phases in addition to the AlN crystal phase, the spinel crystal phase, and the TiN crystal phase. Examples of other crystal phases include α-aluminum oxide (α-alumina). The content of the other crystalline phase in the ceramic base 1 is, for example, 1.0 wt % or less. On the other hand, the lower limit of the content of the other crystalline phase in the ceramic base 1 is typically 0 wt %. When the content ratio of the other crystalline phase in the ceramic base is within this range, the volume resistivity of the ceramic base can be sufficiently ensured in the high temperature range.
[0033] Such a ceramic base 1 has a relatively high volume resistivity in the high temperature range. The volume resistivity of the ceramic substrate 1 at 600°C is, for example, 1.0 × 10 9 Ω·cm or more, preferably 1.2×10 9 Ω·cm or more, preferably 2.0×109 Ω·cm or more, more preferably 5.0×10 9 Ω·cm or more, particularly preferably 1.0×10 10 Ω·cm or more, particularly preferably 7.0×10 10 Ω·cm or more, most preferably 8.0×10 10 Ω·cm or more. On the other hand, the volume resistivity of the ceramic substrate 1 at 600°C is, for example, 1.0 × 10 12 Ω·cm or less, e.g., 1.5×10 11 Ω·cm or less. The volume resistivity of the ceramic substrate at 600° C. is measured in accordance with, for example, JIS C2141-1992.
[0034] The thermal conductivity of the ceramic base 1 at 600° C. is, for example, 20 W / m·K to 50 W / m·K. The thermal conductivity of the ceramic substrate at 600°C is measured, for example, in accordance with the flash method specified in JIS R1611:2010.
[0035] The open porosity of the ceramic substrate 1 is, for example, 1.0% or less. The open porosity of the ceramic substrate is measured in accordance with, for example, JIS R1634.
[0036] The relative density of the ceramic substrate 1 is, for example, 99.0% or more, and preferably 99.5% or more. On the other hand, the upper limit of the relative density of the ceramic substrate 1 is typically 100%. The relative density of the ceramic substrate is measured, for example, in accordance with JIS R1634.
[0037] B-2. Conductors The conductor 2 has any appropriate function depending on the application of the semiconductor manufacturing equipment member 100. There is no particular limitation on the number of elements of the conductor 2 provided on the ceramic substrate 1. A plurality of conductors 2 may be provided on the ceramic substrate 1. In this case, the plurality of conductors 2 may be positioned apart from each other in the thickness direction of the ceramic substrate 1, or may be in contact with each other in the thickness direction of the ceramic substrate 1. Examples of the conductor 2 include electrodes such as ESC electrodes and RF electrodes; a resistance heating element; and a terminal portion.
[0038] In one embodiment, the semiconductor manufacturing equipment member 100 includes a resistance heating element 2a as the conductor 2. The resistance heating element 2a is configured to generate heat when a voltage is applied thereto. The resistance heating element 2a may have any suitable shape, such as a coil shape, a zigzag shape, or a mesh shape.
[0039] As described above, the resistance heating element 2a has a surface layer 21 containing spinel and a skeleton 22 containing a conductive material. The skeleton 22 of the resistance heating element 2a is preferably made of WC and TiN, or made of Mo.
[0040] In one embodiment, the semiconductor manufacturing equipment member 100 further includes the ESC electrodes 2b as the conductor 2. In the illustrated example, the ESC electrodes 2b are spaced apart from the resistance heating body 2a in the thickness direction of the ceramic base 1 and are located between the mounting surface 1a and the resistance heating body 2a. When a DC voltage is applied to the ESC electrodes 2b in a state in which the semiconductor substrate 8 is mounted on the mounting surface 1a, the ESC electrodes 2b are charged with either positive or negative charges in accordance with the polarity of the applied DC voltage, and the other of the positive and negative charges present in the semiconductor substrate 8 moves toward the mounting surface 1a in the semiconductor substrate 8. As a result, a Johnsen-Rahbek (JR) force is generated between the semiconductor substrate 8 and the ESC electrodes 2b, and the semiconductor substrate 8 is chucked to the ceramic base material 1. Although not shown, the semiconductor manufacturing equipment member 100 may include a plurality of ESC electrodes 2b.
[0041] The ESC electrodes 2b may function as RF electrodes (i.e., radio frequency electrodes) for plasma processing. That is, the ESC electrodes 2b preferably function as RF / ESC electrodes. Examples of the plasma processing include a film formation process and an etching process. When such plasma processing is performed on the semiconductor substrate 8 on the mounting surface 1a, the upper electrode is disposed on the opposite side of the ESC electrodes 2b with respect to the semiconductor substrate 8. When high-frequency power is supplied to the ESC electrode 2b in this state, the processing gas is excited in the space between the ceramic base 1 and the upper electrode, and plasma can be generated. The plasma processing is performed on the semiconductor substrate 8 by the plasma.
[0042] The ESC electrodes 2b can have any appropriate shape. The ESC electrodes 2b typically have a plate shape. In one embodiment, the ESC electrodes 2b have a shape similar to the outer shape of the ceramic base 1 when viewed in the thickness direction of the ceramic base 1. In the illustrated example, the centers of the ESC electrodes 2b and the center of the ceramic base 1 substantially coincide with each other when viewed in the thickness direction of the ceramic base 1.
[0043] As described above, the ESC electrode 2b includes the surface layer 21 containing spinel and the skeleton 22 containing a conductive material. Preferred examples of the conductive material that forms the skeleton 22 of the ESC electrode 2b include metals and inorganic compounds. Specific examples of the metal include molybdenum, niobium, tantalum, and alloys thereof. A specific example of the inorganic compound is molybdenum carbide. These conductive materials may be used alone or in combination.
[0044] C. Manufacturing method for semiconductor manufacturing equipment components Next, a method for manufacturing a semiconductor manufacturing equipment member according to one embodiment will be described. The manufacturing method of the semiconductor manufacturing equipment component 100 includes a mixing step of mixing raw material powder of the ceramic substrate 1; a forming step of preparing a plurality of molded bodies from the substrate raw material mixture obtained in the mixing step; an arrangement step of arranging a precursor of a conductor between the plurality of molded bodies; and a firing step of firing the laminate obtained in the arrangement step.
[0045] C-1.Mixing process In the mixing step, the raw material of the ceramic material described above is mixed with a magnesium oxide raw material (hereinafter referred to as an MgO raw material) or a spinel raw material to prepare a substrate raw material mixture.
[0046] In one embodiment, the raw material of the ceramic material is an AlN raw material. The AlN raw material contains AlN as a main component. The AlN raw material may contain oxygen and carbon in addition to AlN. The amount of oxygen in the AlN raw material is, for example, 0.7 wt % to 0.9 wt % The amount of carbon in the AlN raw material is, for example, 200 ppm to 400 ppm. The AlN raw material is typically in a powder form, and the average particle size D50 of the AlN raw material is, for example, 1.0 μm to 1.5 μm.
[0047] The MgO raw material contains MgO as a main component. The MgO raw material is typically in a powder form. The average particle size D50 of the MgO raw material is, for example, 0.2 μm to 0.8 μm.
[0048] The amount of the MgO raw material or spinel raw material added is, for example, 0.01 part by weight or more, preferably 0.05 part by weight or more, and more preferably 0.1 part by weight or more, relative to 100 parts by weight of the AlN raw material. On the other hand, the amount of the MgO raw material or spinel raw material added is, for example, 1.1 parts by weight or less, preferably 1.0 part by weight or less, relative to 100 parts by weight of the AlN raw material.
[0049] In the mixing step, if necessary, a titanium oxide raw material (hereinafter referred to as TiO2 raw material) is further mixed with the substrate raw material mixture. The TiO2 raw material contains TiO2 as a main component. The TiO2 raw material is typically in a powder form. The average particle size D50 of the TiO2 raw material is, for example, 0.1 μm to 0.5 μm.
[0050] The amount of TiO2 raw material added is, for example, 0.1 part by weight or more, preferably 0.3 part by weight or more, relative to 100 parts by weight of AlN raw material, while the amount of TiO2 raw material added is, for example, 1.0 part by weight or less, relative to 100 parts by weight of AlN raw material.
[0051] In one embodiment, in the mixing step, a binder is added to the above-mentioned substrate raw material mixture. Examples of binders include polyvinyl acetal resins, cellulose ether resins, (meth)acrylic resins, and paraffin wax. The term "(meth)acrylic resin" includes acrylic resins and / or methacrylic resins. Binders may be used alone or in combination. Of these binders, (meth)acrylic resins are preferred.
[0052] In the mixing step, any suitable mixing device can be used, such as a ball mill, a bead mill, a vibration mill, a rocking mixer, a blender, a homogenizer, or the like.
[0053] The mixing method may be dry mixing or wet mixing. In one embodiment, the mixing step is performed by wet mixing. In the wet mixing, any suitable organic solvent is used. Examples of organic solvents include alcohols, esters, and hydrocarbons. The organic solvents may be used alone or in combination. Among the organic solvents, alcohols are preferred. Examples of alcohols include ethyl alcohol, isopropyl alcohol, ethyl cellosolve, butyl carbitol, and hexyl carbitol, and isopropyl alcohol is preferred.
[0054] The environmental conditions in the mixing step are not particularly limited, and the mixing step is typically carried out at room temperature (23°C) and atmospheric pressure (0.1 MPa). The mixing time can be set arbitrarily and appropriately, for example, from 1 hour to 24 hours.
[0055] In this way, the substrate raw material mixture is prepared. If the mixing step is dry mixing, the substrate raw material mixture is in a powder state, and if the mixing step is wet mixing, the substrate raw material mixture is in a slurry state.
[0056] C-2. Granulation process In one embodiment, the method for manufacturing the semiconductor manufacturing equipment member 100 includes a granulation step after the mixing step and before the molding step. In the granulation step, the substrate raw material mixture obtained in the mixing step is granulated by any appropriate granulation method, such as spray granulation or tumbling granulation, preferably spray granulation. In this way, granulated material of the substrate raw material mixture (hereinafter referred to as raw material granules) is prepared.
[0057] C-3. Molding process Next, in the molding step, the substrate raw material mixture (preferably raw material granules) is molded into a desired shape by any appropriate molding method to prepare a plurality of molded bodies.
[0058] Examples of molding methods include press molding, sheet molding, cold isostatic pressing (CIP) molding, and doctor blade molding, and press molding is preferred. The pressure in press molding is, for example, 10 kgf / cm. 2 ~500kgf / cm 2 is. In this way, a plurality of molded bodies having the desired shape are prepared. In one embodiment, two disk-shaped molded bodies are prepared.
[0059] C-4. Placement process In the arrangement step, a laminate is typically prepared by arranging a precursor of the conductor 2 between two molded bodies. In the following, one of the two molded bodies may be referred to as a first molded body and the other as a second molded body.
[0060] In one embodiment, the precursor of the conductor 2 is formed on a sheet material by printing. When forming the precursor of the conductor 2 by printing, first, the raw materials of the conductive material described above are added to an organic solvent and mixed to prepare a conductor raw material slurry. In this case, the raw materials of the conductive material described above are preferably WC raw material and TiN raw material.
[0061] The WC raw material contains WC as a main component. The WC raw material is typically in a powder form. The average particle size D50 of the WC raw material is, for example, 0.1 μm to 5.0 μm.
[0062] The TiN raw material contains TiN as a main component. The TiN raw material is typically in a powder form. The average particle size D50 of the TiN raw material is, for example, 0.1 μm to 5.0 μm. The amount of TiN raw material added is, for example, 0.5 parts by weight or more, preferably 1.0 parts by weight or more, and more preferably 3.0 parts by weight or more, relative to 100 parts by weight of the WC raw material. On the other hand, the amount of TiN raw material added is, for example, 20.0 parts by weight or less, preferably 10.0 parts by weight or less, and more preferably 5.0 parts by weight or less, relative to 100 parts by weight of the WC raw material.
[0063] Examples of the organic solvent include the same organic solvents as those used in the mixing step described above, and alcohols are preferred.
[0064] Furthermore, a binder is mixed into the conductor raw material slurry as required. Examples of the binder include the same binders as those used in the mixing step described above, and preferably (meth)acrylic resins.
[0065] The preparation of such a conductor raw material slurry is typically carried out using any appropriate mixing device, such as the same mixing device as used in the mixing step described above. The environmental conditions for preparing the conductor raw material slurry are not particularly limited. The preparation of the conductor raw material slurry is typically carried out at room temperature (25° C.) and atmospheric pressure (0.1 MPa).
[0066] This prepares a conductor raw material slurry, which typically contains a WC raw material and a TiN raw material.
[0067] Next, the conductor raw material slurry is printed onto the sheet material by any suitable printing method. Examples of printing methods include screen printing, letterpress printing, offset printing, and gravure printing, with screen printing being preferred.
[0068] The sheet material has any appropriate configuration capable of holding the precursor of the conductor 2. Examples of the sheet material include a gel sheet, a ceramic sheet, and an acrylic sheet. Of the sheet materials, a ceramic sheet is preferable. Examples of materials constituting the ceramic sheet include the same materials as those constituting the ceramic substrate 1 described above, preferably the ceramic materials described above, and more preferably aluminum nitride (AlN). The thickness of the sheet material is, for example, 50 μm to 1000 μm, and preferably 100 μm to 500 μm.
[0069] The printed conductor raw material slurry is then dried, typically in the atmosphere.
[0070] As a result, a precursor of the conductor 2 having a desired shape is formed on the sheet material, and a precursor-holding sheet is prepared. The precursor-holding sheet includes a sheet material and the precursor of the conductor 2 formed on the sheet material. The thickness of the precursor of the conductor 2 is, for example, 10 μm to 100 μm, and preferably 20 μm to 80 μm.
[0071] Next, the precursor-holding sheet is placed on the first compact so that the ceramic sheet is in contact with the first compact.
[0072] Alternatively, a precursor of the conductor 2 can be prepared by printing the conductor raw material slurry directly onto the first compact. Furthermore, the method for preparing the precursor of the conductor 2 is not limited to printing. For example, a precursor of the conductor 2 having a desired shape may be prepared in advance by any appropriate method and placed on the first molded body. In one embodiment, a precursor of the conductor 2 having a desired shape is prepared from a transition metal (preferably Mo) by any appropriate method and placed on the first molded body. Furthermore, a liquid containing an MgO raw material and / or a spinel raw material may be applied to the surface of the precursor of the conductor 2 prepared in advance by any appropriate method. Furthermore, a thin film containing an MgO raw material and / or a spinel raw material may be formed on the surface of the precursor of the conductor 2. Examples of methods for forming the thin film include transfer, powder molding, and sputtering.
[0073] By these means, the precursor of the conductor 2 placed on the first compact is sandwiched between the first compact and the second compact. More specifically, the second compact is placed on the opposite side of the precursor of the conductor 2 from the first compact. This prepares a laminate having a structure of first compact / electrical conductor precursor / second compact.
[0074] C-5. Firing process In the subsequent firing step, the laminate is typically fired in a vacuum or a non-oxidizing atmosphere. More specifically, the temperature is raised from room temperature (23°C) to a predetermined firing temperature, and then the firing temperature is maintained for a predetermined firing time. A degreasing step may be performed before the firing step, if necessary.
[0075] The firing temperature is, for example, 1600°C to 1900°C, and preferably 1650°C to 1850°C. The firing time is, for example, 0.5 to 100 hours. The environmental pressure in the firing step is, for example, 100 kPa to 900 kPa.
[0076] Examples of the firing method include hot pressing and hot isostatic pressing (HIP), with hot pressing being preferred. In the hot press, typically, the laminate is placed in a hot press die (for example, a carbon jig), heated to the firing temperature as described above, and pressed at a predetermined pressure, for example, 5 MPa to 50 MPa.
[0077] In this firing process, the first and second compacts are sintered to form a single body, and the conductor precursor becomes a conductor and is embedded in the ceramic substrate. More specifically, the ceramic material (typically AlN) contained in the compacts is sintered, and Mg reacts with AlN as needed to form a spinel. This results in the preparation of a ceramic substrate. Furthermore, since the conductor precursor is sandwiched between two compacts during firing, atoms within the compact can be more smoothly transferred (diffused) than when the conductor precursor is sandwiched between two sintered bodies, allowing for the spinel to concentrate at the interface between the ceramic substrate and the conductor precursor. This allows for the stable formation of a conductor having a spinel-containing surface layer and a skeleton located inside the surface layer from the conductor precursor. In particular, the spinel-containing surface layer can be more stably formed when the conductor precursor is held in a sheet material. When the precursor of the conductor is formed by printing, the conductor 2 is a conductor 2 obtained by printing (printed conductor). In this manner, a semiconductor manufacturing equipment member 100 including a ceramic base and a conductor is prepared.
[0078] D. Applications of semiconductor manufacturing equipment components The semiconductor manufacturing equipment member 100 can be applied to any appropriate semiconductor manufacturing equipment. Examples of uses for the semiconductor manufacturing equipment member 100 include heaters, susceptors, electrostatic chucks, ceramic conductors, feedthroughs, and shower heads.
[0079] In one embodiment, the semiconductor manufacturing equipment member 100 is applied to a heater 101. When the semiconductor manufacturing equipment member 100 is applied to the heater 101, the ceramic base 1 functions as a substrate mounting plate, and the conductor 2 includes a resistance heating element 2 a. In the illustrated example, the conductor 2 further includes ESC electrodes 2 b in addition to the resistance heating element 2 a.
[0080] The heater 101 is a heater for use in semiconductor manufacturing equipment, and includes a member for semiconductor manufacturing equipment 100 (ceramic base 1 and conductor 2), a ceramic shaft 5, a first power feed rod 6, and a second power feed rod .
[0081] The ceramic shaft 5 is capable of supporting the ceramic base (substrate mounting plate) 1. The ceramic shaft 5 is connected to the surface of the ceramic base opposite to the mounting surface 1a.
[0082] The ceramic shaft 5 has any appropriate shape. In one embodiment, the ceramic shaft 5 has a cylindrical shape extending in the thickness direction of the ceramic base 1. In the illustrated example, the axis of the ceramic shaft 5 and the center of the ceramic base 1 substantially coincide with each other when viewed in the thickness direction of the ceramic base 1.
[0083] The ceramic shaft 5 is made of any appropriate ceramic material. The ceramic material constituting the ceramic shaft 5 is preferably the same as the ceramic material contained in the ceramic substrate 1. When the ceramic shaft and the ceramic substrate contain the same ceramic material, the difference in thermal expansion between the ceramic substrate and the ceramic shaft can be reduced, and sufficient bonding strength between the ceramic substrate and the ceramic shaft can be ensured in a high-temperature environment.
[0084] The first power feed rod 6 is electrically connected to the resistance heating element 2a. In the illustrated example, the first power feed rod 6 passes through the internal space of the ceramic shaft 5 and is electrically connected to the resistance heating element 2a. The first power feed rod 6 is made of any appropriate conductive material. A voltage can be applied to the resistance heating element 2a via the first power feed rod 6.
[0085] The second power feed rod 7 is electrically connected to the ESC electrodes 2b. In the illustrated example, the second power feed rod 7 passes through the internal space of the ceramic shaft 5 and is electrically connected to the ESC electrodes 2b. The second power feed rod 7 is made of any appropriate conductive material. A voltage can be applied to the ESC electrodes 2b via the second power feed rod 7.
[0086] 2 , in another embodiment, a semiconductor manufacturing equipment member 100 is applied to an electrostatic chuck 102. When the semiconductor manufacturing equipment member 100 is applied to the electrostatic chuck 102, the ceramic base 1 functions as a substrate mounting plate, and the conductor 2 includes the ESC electrodes 2 b. In the illustrated example, the conductor 2 further includes a resistance heating element 2 a in addition to the ESC electrodes 2 b.
[0087] As shown in FIG. 5, in one embodiment, the semiconductor manufacturing equipment member 100 includes the above-described electrode and / or resistance heating element as a conductor, and a terminal portion 2c. The terminal portion 2c is electrically connected to the electrode and / or resistance heating element. More specifically, the terminal portion 2c is embedded in the ceramic base 1 and is in contact with the electrode and / or resistance heating element in the thickness direction of the ceramic base 1. The terminal portion 2c may be bonded to the electrode and / or resistance heating element. In the illustrated example, the semiconductor manufacturing equipment member 100 includes the above-described resistance heating element 2a and the terminal portion 2c.
[0088] A portion of the surface of the terminal portion 2c is typically exposed from the ceramic base 1. In the illustrated example, the ceramic base 1 has a recess 15. The recess 15 is recessed from the surface of the ceramic base 1 opposite the mounting surface 1a toward the terminal portion 2c. The recess 15 exposes a portion of the surface of the terminal portion 2c. This allows a voltage to be smoothly applied to the terminal from an external power source, and as a result, a voltage can be stably applied to the electrode and / or the resistance heating element. Hereinafter, the portion of the surface of the terminal portion 2c that is exposed from the ceramic base 1 may be referred to as the exposed portion.
[0089] As described above, the terminal portion 2c includes the surface layer 21 containing spinel and the skeleton 22 containing a conductive material. The surface layer 21 of the terminal portion 2c is located on at least a part of the interface between the skeleton 22 and the ceramic substrate 1. The surface layer 21 of the terminal portion 2c is typically not provided on an exposed portion of the surface of the terminal portion 2c.
[0090] The skeleton 22 of the terminal portion 2c is preferably made of WC and TiN. When the skeleton contains WC and TiN, cracks due to the difference in thermal expansion coefficient between the terminal portion and the ceramic base material can be suppressed. Furthermore, when the skeleton 22 of the terminal portion 2c contains WC and TiN and the skeleton 22 of the conductor 2 (electrode and / or resistance heating element) electrically connected to the terminal portion 2c contains WC and TiN, they can be stably joined together and peeling between the components can be stably suppressed.
[0091] The thickness of the terminal portion 2c is, for example, 0.50 mm to 8.00 mm, preferably 1.00 mm to 4.00 mm, and more preferably 1.20 mm to 2.00 mm.
[0092] The terminal portion 2c may have any suitable shape, and in the illustrated example, the terminal portion 2c has a flat plate shape.
[0093] 6A and 6B, the terminal portion 2c may be composed of a plurality of cylindrical members arranged concentrically, with a ceramic material similar to the ceramic substrate 1 typically disposed between the cylindrical members.
[0094] 7A and 7B, the terminal portion 2c may be composed of a plurality of small pieces arranged in a staggered pattern, with the same ceramic material as the ceramic base 1 typically being disposed between the small pieces.
[0095] 8A and 8B, the terminal portion 2c may be composed of a plurality of rod-shaped members spaced apart from one another, with the same ceramic material as the ceramic base 1 typically disposed between the rod-shaped members.
[0096] 6A to 8B, the same ceramic material as that of the ceramic substrate 1 is disposed near the various members that make up the terminal portion 2c. Therefore, in the semiconductor manufacturing equipment member 100 that includes such a terminal portion 2c, cracks and residual stress due to differences in thermal expansion can be reduced.
[0097] 6A to 8B, a tablet 20 corresponding to the configuration of the terminal portion is prepared using, for example, the substrate raw material mixture and the conductive material raw material described above. A typical example of a tablet preparation device is a 3D printer. Next, in the above-mentioned placement step, the tablet 20 is placed between the first and second compacts as a precursor of the conductor to prepare a laminate having a structure of first compact / tablet / second compact. The laminate is then fired by the firing step described above. That is, the compact and the tablet are fired simultaneously. At this time, since the compact and the tablet contain the substrate raw material mixture, the difference in shrinkage rate between them can be reduced. Therefore, the occurrence of cracks in the manufactured semiconductor manufacturing equipment components can be suppressed and residual stress can be reduced. In this manner, the semiconductor manufacturing equipment member 100 having the terminal portion 2c is manufactured. [Example]
[0098] The present invention will be specifically explained below with reference to examples and comparative examples, but the present invention is not limited to these examples. The methods for measuring each property are as follows.
[0099] (1) Identification of the elemental composition of conductors using EPMA The heaters for semiconductor manufacturing equipment manufactured in the examples and comparative examples were cut into test pieces measuring 10 mm x 10 mm, each having a thickness of 3 mm. The cross section of the ceramic substrate of the test piece along the thickness direction was polished to a mirror finish by lapping to serve as a measurement surface. The measurement surface included a conductor. The polished surface was then analyzed using an EPMA to obtain an elemental mapping image. This allowed the elemental composition of the surface layer and skeleton of the conductor to be identified. Note that in Comparative Example 1, the conductor did not have a surface layer. The results are shown in Table 1.
[0100] (2) Measurement of Mg intensity using EPMA Test pieces were prepared in the same manner as in (1) Identification of elemental composition of conductors by EPMA. Next, three measurement lines were determined on the measurement surface of the test piece, extending along the thickness direction of the ceramic substrate and passing through the conductor. Each of the three measurement lines had a first end on the mounting surface side and a second end opposite the first end. The three measurement lines were positioned at arbitrary intervals from each other in a direction perpendicular to the thickness direction of the ceramic substrate.
[0101] Thereafter, each measurement line was subjected to line analysis using an EPMA under the conditions below, and the intensities of the characteristic X-rays of Mg and Al in each measurement line were measured. <Measurement conditions> Equipment: JEOL Ltd., JXA-8530FPlus Accelerating voltage: 15kv Irradiation current: 1×10-7 A Measurement magnification: 2000x
[0102] The Mg characteristic X-ray spectrum was created for each measurement line, with the intensity of the obtained Mg characteristic X-rays on the Y axis and the distance from the first end to the second end of the measurement line on the X axis. The Mg characteristic X-ray spectrum for Example 1 is shown in Figure 3, and the Mg characteristic X-ray spectrum for Comparative Example 1 is shown in Figure 4. In Figures 3 and 4, the Mg characteristic X-ray spectrum is shown by a solid line, and the Al characteristic X-ray spectrum is shown by a dashed dotted line.
[0103] Next, the maximum intensity of the peak located inside the conductor in the Mg characteristic X-ray spectrum for each measurement line was taken as the Mg intensity of the conductor. The average Mg intensity of the conductor was calculated from the Mg intensities of the conductor for the three measurement lines. In addition, in the Mg characteristic X-ray spectrum for each measurement line, the maximum intensity of the peaks located at the interface between the ceramic substrate and the conductor (specifically, the first interface on the mounting surface side and the second interface on the opposite side) was taken as the Mg intensity of the surface layer. The average value of the Mg intensities of the surface layer for the three measurement lines was calculated. The measurement of Mg intensity by EPMA was carried out twice, and the Mg intensity was measured at different cross sections of the ceramic substrate on which the conductor was provided. The results are shown in Table 2.
[0104] (3) Measurement of the resistivity of a conductor A rectangular parallelepiped test piece containing a conductor was cut out from the heater for semiconductor manufacturing equipment manufactured in the examples and comparative examples. The length of one side of the test piece was 9 mm. The conductor was exposed on the opposing end faces of the test piece. The dimensions of the conductor in the cross section of the test piece were measured using an optical microscope, and the cross-sectional area S (cm 2 The dimension between the end faces where the conductor is exposed was measured with a vernier caliper as the length L (cm) of the conductor. Next, lead wires were connected to the conductor exposed at the end face of the test piece using conductive paste. A current ranging from 0 mA to 150 mA was then supplied to the conductor in the test piece at room temperature (25°C) and atmospheric pressure (0.1 MPa), and the minute voltage V (mV) generated was measured. The resistance R (Ω) of the conductor was calculated from the relationship between the current I and voltage V. The resistivity ρ (Ω·cm) of the conductor was then calculated using the following formula (1). The results are shown in Table 1. ρ=R×S / L (1) (In formula (1), ρ represents the resistivity of the conductor, R represents the resistance of the conductor, S represents the cross-sectional area of the conductor, and L represents the length of the conductor.)
[0105] (4) Measurement of the resistivity variation of a conductor The resistivity of the conductors of the heaters for semiconductor manufacturing equipment manufactured in the examples and comparative examples was measured using a tester four-terminal method. More specifically, the resistance values of multiple arbitrary locations (specifically, four locations) on the same surface of the conductor were measured using the tester four-terminal method. Next, the resistivity of each location of the conductor was calculated from the measured resistance value of each location and the cross-sectional area measurement results of the conductor. Thereafter, the resistivity variation γ (%) of the conductor was calculated based on the following formula (2). The results are shown in Table 1. γ=(α max -α min ) / β×100 (2) (In formula (2), α max represents the maximum resistivity among the resistivities of each point of the conductor, and α min represents the minimum resistivity among the resistivities at each point of the conductor, β represents the average resistivity of multiple points of the conductor, and γ represents the resistivity variation.)
[0106] <<Example 1>> 98.5 parts by weight of AlN raw material powder (average particle size D50: 1.2 μm, oxygen content: 0.8 wt%), 1.0 part by weight of MgO raw material powder (average particle size D50: 0.5 μm), and 0.5 part by weight of TiO raw material powder (average particle size D50: 0.3 μm) were placed in a ball mill, and then acrylic resin (binder) and isopropyl alcohol (IPA) were added to the ball mill and wet mixed for 2 hours. The resulting base material slurry was then dried and granulated using a spray granulator to obtain raw material granules with a particle size of 80 μm.
[0107] The raw material granules were then uniaxially pressed to obtain a first compact having a disk shape. The pressure in the uniaxial pressing was 100 kgf / cm. 2 In addition, a second compact having a disk shape was prepared in the same manner as the first compact.
[0108] 96.0 parts by weight of WC raw material powder, 4.0 parts by weight of TiN raw material powder, and acrylic resin (binder) were placed in a ball mill and wet-mixed for 10 hours using an organic solvent to obtain a conductor raw material slurry.
[0109] The conductor raw material slurry was then applied in a predetermined pattern by screen printing onto a ceramic sheet serving as a sheet material, and then dried in the atmosphere at 70°C for 30 minutes. This resulted in the preparation of a precursor-holding sheet comprising a ceramic sheet and a conductor precursor formed on the ceramic sheet. The conductor precursor had a thickness of 50 μm. The ceramic sheet was made of aluminum nitride. The ceramic sheet had a thickness of 200 μm.
[0110] Next, the precursor-holding sheet was placed on the first compact so that the ceramic sheet was in contact with the first compact. Next, the second compact was placed on the opposite side of the conductive precursor from the first compact, thereby obtaining a laminate in which the precursor-holding sheet was sandwiched between the first compact and the second compact.
[0111] The laminate was then fired by hot pressing, more specifically, at 1800° C. for 2 hours in a nitrogen atmosphere. As a result, the first and second compacts were sintered and integrated, and the precursor of the conductor was fired to become a conductor and embedded in the ceramic substrate. At this time, atoms inside the compacts migrated (diffused), and a surface layer containing spinel was formed at the interface between the compacts and the precursor of the conductor. In this manner, a heater for semiconductor manufacturing equipment comprising a ceramic base and an electric conductor was manufactured.
[0112] <<Example 2>> A heater for semiconductor manufacturing equipment was manufactured in the same manner as in Example 1, except that the first molded body and the second molded body were replaced with the first molded sheet and the second molded sheet prepared as follows, respectively. The first and second molded sheets were each prepared by forming the base material slurry prepared in the same manner as in Example 1 into a sheet using a doctor blade molding machine. The thickness of each of the first and second molded sheets was 200 μm.
[0113] <<Example 3>> In the same manner as in Example 1, a first compact and a second compact were prepared. Also, a coil made of molybdenum (Mo) (hereinafter referred to as Mo coil) was prepared, and then the Mo coil was sandwiched between the first compact and the second compact to obtain a laminate. Thereafter, the laminate was fired in the same manner as in Example 1. As a result, the first compact and the second compact were sintered and integrated, a surface layer containing spinel was formed on the surface of the Mo coil, and the conductor having the surface layer and the skeleton was embedded in the ceramic substrate. In this manner, a heater for semiconductor manufacturing equipment comprising a ceramic base and an electric conductor was manufactured.
[0114] <<Comparative Example 1>> A first compact and a second compact were prepared in the same manner as in Example 1, except that in preparing the conductor raw material slurry, 4.0 parts by weight of Al2O3 powder was used instead of 4.0 parts by weight of TiN powder. Next, the first and second compacts were each sintered by hot pressing. More specifically, the first and second compacts were each sintered at 1800°C for 2 hours in a nitrogen atmosphere. This resulted in a first sintered body and a second sintered body.
[0115] Thereafter, a conductor raw material slurry prepared in the same manner as in Example 1 was applied to the first sintered body in a predetermined pattern by screen printing, and then dried in the atmosphere at 70°C for 30 minutes, thereby forming a conductor precursor directly on the first sintered body. Next, the second sintered body was placed on the opposite side of the conductor precursor from the first sintered body, thereby obtaining a laminate in which the conductor precursor was sandwiched between the first and second sintered bodies. Next, the laminate was fired in the same manner as in Example 1 to produce a heater for semiconductor manufacturing equipment.
[0116] [Table 1]
[0117] [Table 2]
[0118] <Evaluation> As shown in Table 1, in Examples 1 to 3, the conductor has a surface layer and a skeleton containing spinel, while in Comparative Example 1, the conductor has no surface layer and the spinel is dispersed throughout the conductor. As described above, it is clear that when a conductor includes a surface layer, the resistivity variation in the conductor can be significantly reduced. Since the resistivity variation and the conductivity variation in a conductor are correlated, it is clear that when the resistivity variation is small, the conductivity variation is also small, and the conductivity uniformity in the conductor is excellent. Furthermore, as shown in Table 2, in the Mg characteristic X-ray spectrum of Example 1, the maximum intensity of the peaks located in the surface layer (first and second interfaces) of the conductor was greater than the maximum intensity of the peaks located in the skeleton of the conductor. In other words, it was confirmed that the Mg concentration in the surface layer (first and second interfaces) of the conductor was greater than the Mg concentration in the skeleton of the conductor. [Industrial Applicability]
[0119] The semiconductor manufacturing equipment member according to the embodiment of the present invention is typically used in the manufacture of semiconductors, and can be particularly suitably used for susceptors, heaters, electrostatic chucks, ceramic conductors, lead-in terminals, shower heads, and the like. [Explanation of symbols]
[0120] 1. Ceramic substrate 2. Conductors 21 Surface layer 22 Skeleton 2a Resistance heating element 2b ESC electrode 2c terminal section 100 Semiconductor manufacturing equipment components
Claims
1. a ceramic substrate; A semiconductor manufacturing equipment member comprising: a conductor provided within the ceramic base, The ceramic substrate has a thermal expansion coefficient of 2.0×10 -6 / ℃~10.0×10 -6 / °C ceramic material and spinel, The conductor has a surface layer containing spinel and a skeleton located inside the surface layer.
2. 2. The semiconductor manufacturing equipment member according to claim 1, wherein the skeleton is made of tungsten carbide and titanium nitride.
3. the content of tungsten carbide in the skeleton is 50 wt % to 99 wt %; 3. The semiconductor manufacturing equipment member according to claim 2, wherein the content of titanium nitride in the skeleton is 1 wt % to 50 wt %.
4. 2. The semiconductor manufacturing equipment member according to claim 1, wherein the skeleton is made of molybdenum.
5. 5. The semiconductor manufacturing equipment member according to claim 1, wherein, in a line analysis using an electron probe microanalyzer on a cross section of the ceramic base material on which the conductor is provided, cut in the thickness direction, the average Mg intensity of the surface layer is three times or more the average Mg intensity of the skeleton.
6. 5. The semiconductor manufacturing equipment member according to claim 1, wherein the ceramic substrate further contains titanium nitride.
7. The content of spinel in the ceramic substrate is 0.5 wt % to 55 wt %; 7. The semiconductor manufacturing equipment member according to claim 6, wherein the content of titanium nitride in said ceramic base material is 0.1 wt % to 1.0 wt %.
8. 5. The semiconductor manufacturing equipment member according to claim 1, wherein the dimension of the conductor in the thickness direction of the ceramic base is 10 μm to 50 μm.
9. 5. The semiconductor manufacturing equipment member according to claim 1, wherein the conductor is obtained by printing.
10. The conductor includes: Electrodes and / or resistive heating elements; 5. The semiconductor manufacturing equipment member according to claim 1, further comprising: a terminal portion electrically connected to the electrode and / or the resistance heating element.
Citation Information
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