Member for semiconductor manufacturing apparatus
The semiconductor manufacturing equipment member with a spinel-containing surface layer and tungsten carbide-titanium nitride skeleton addresses conductivity variations, achieving uniform and stable electrical performance.
Patent Information
- Application Number
- PCT/JP2025/001940
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2024-05-27
- Filing Date
- 2025-01-22
- Publication Date
- 2025-12-04
AI Technical Summary
Conventional semiconductor manufacturing equipment components experience local variations in electrical conductivity, leading to inconsistent performance.
A semiconductor manufacturing equipment member with a ceramic base and conductor that includes a surface layer containing spinel and a skeleton composed of tungsten carbide and titanium nitride, designed to stabilize electrical conductivity and reduce variations.
The configuration enhances uniformity and stability of electrical conductivity, ensuring consistent performance and efficient voltage application across the conductor.
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Figure JP2025001940_04122025_PF_FP_ABST
Abstract
Description
Semiconductor manufacturing equipment components
[0001] The present invention relates to a member for a semiconductor manufacturing device.
[0002] Conventionally, semiconductor manufacturing equipment for manufacturing semiconductor devices includes various components according to their functions. Such semiconductor manufacturing equipment may use components for semiconductor manufacturing equipment that include a ceramic substrate and a conductor disposed within the ceramic substrate. For example, a substrate holder has been proposed as such a semiconductor manufacturing equipment component, in which the ceramic substrate is made from a 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).
[0003] Patent No. 5032444
[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 result in the failure to fully exhibit the desired function. A main object of the present invention is to provide a semiconductor manufacturing equipment member including a conductor with excellent uniformity in electrical conductivity.
[0005] [1] A semiconductor manufacturing equipment member according to an embodiment of the present invention includes a ceramic base and an electric conductor. The electric conductor is provided within the ceramic base. The ceramic base has a thermal expansion coefficient of 2.0×10 -6 / ℃~10.0×10 -6 / °C and a spinel. The conductor has a surface layer containing spinel and a skeleton located inside the surface layer. [2] In the semiconductor manufacturing equipment member described in [1] above, the skeleton may be composed of tungsten carbide and titanium nitride. [3] In the semiconductor manufacturing equipment member described in [2] above, the skeleton may contain tungsten carbide in an amount of 50 wt % to 99 wt %, and the skeleton may contain titanium nitride in an amount of 1 wt % to 50 wt %. [4] In the semiconductor manufacturing equipment member described in [1] above, the skeleton may be composed of molybdenum. [5] In the semiconductor manufacturing equipment member described in any one of [1] to [4] above, in a line analysis using an electron probe microanalyzer on a cross section of the ceramic base provided with the conductor cut in the thickness direction, the average Mg intensity of the surface layer may be three times or more 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 in a direction perpendicular to the thickness direction; the intensity of Mg characteristic X-rays on 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 an Mg characteristic X-ray spectrum for each measurement line; the maximum intensity of a peak located at the interface between the ceramic substrate and the conductor in the Mg characteristic X-ray spectrum is taken 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; the maximum intensity of a peak located inside the conductor in the Mg characteristic X-ray spectrum is taken 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 spinel content in the ceramic substrate may be 0.5 wt % to 55 wt %, and the titanium nitride content in the ceramic substrate may be 0.1 wt % to 1.0 wt %. [8] In the semiconductor manufacturing equipment member described in any of [1] to [7] above, the dimension of the conductor in the thickness direction of the ceramic substrate may be 10 μm to 50 μm. [9] In the semiconductor manufacturing equipment member described in any of [1] to [8] above, the conductor may be obtained by printing.
[10] The semiconductor manufacturing equipment member described in any of [1] to [9] above may include an electrode and / or a resistance heating element and a terminal portion as the conductor. The terminal portion is electrically connected to the electrode and / or the resistance heating element.
[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.
[0007] 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. FIG. 2 is a schematic cross-sectional view of an electrostatic chuck according to another embodiment of the present invention. FIG. 3 is a Mg characteristic X-ray spectrum of the semiconductor manufacturing equipment heater of Example 1. FIG. 4 is a Mg characteristic X-ray spectrum of the semiconductor manufacturing equipment heater of Comparative Example 1. FIG. 5 is a schematic cross-sectional view of a semiconductor manufacturing equipment member according to yet another embodiment of the present invention. FIG. 6A is a schematic perspective view of an example of a terminal portion included in the semiconductor manufacturing equipment member of FIG. 5. FIG. 6B is a schematic plan view of the terminal portion of FIG. 6A. FIG. 7A is a schematic perspective view of a modified example of the terminal portion included in the semiconductor manufacturing equipment member of FIG. 5. FIG. 7B is a schematic plan view of the terminal portion of FIG. 7A. FIG. 8A is a schematic perspective view of another modified example of the terminal portion included in the semiconductor manufacturing equipment member of FIG. 5. FIG. 8B is a schematic plan view of the terminal portion of FIG. 8A.
[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 the Semiconductor Manufacturing Equipment Component Fig. 1 is a schematic cross-sectional view of a heater as a semiconductor manufacturing equipment component according to one embodiment of the present invention. The semiconductor manufacturing equipment component 100 is typically a component of semiconductor manufacturing equipment for manufacturing semiconductor devices. The semiconductor manufacturing equipment component 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 x 10 -6 / ℃~10.0×10 -6 / °C and a spinel. The conductor 2 is provided within 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 with respect to the surface layer 21. The inventors discovered that in a semiconductor manufacturing equipment member in which a conductor is provided within a ceramic substrate, if spinel is formed and unevenly distributed inside the conductor, variations in electrical conductivity occur in the conductor. Therefore, after extensive research into the location of spinel, they 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. Therefore, it is possible to improve the electrical conductivity of the conductor and suppress the variation in 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, surrounding the conductor 2. This configuration can stably suppress 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), hafnium (Hf), etc. 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 includes 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 suppress leakage of current flowing through the conductor's skeleton 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 TiN content in the skeleton 22 of the conductor 2, calculated as oxide, is, for example, 1.0 wt% to 50.0 wt%, preferably 1.0 wt% to 5.0 wt%. When the WC and / or TiN content in the skeleton of the conductor is 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 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 Mo content 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 concentrations in the surface layer 21 and skeleton 22 of the conductor 2 are 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 provided with the conductor 2 is cut in the thickness direction to form a cross section including the conductor 2. (2) Next, multiple measurement lines are set in the cross section, extending in the thickness direction of the ceramic substrate 1 and passing through the conductor 2. The multiple measurement lines are positioned at arbitrary intervals from each other in a direction perpendicular to the thickness direction of the ceramic substrate 1. The number of measurement lines is typically three. Each of the multiple 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 first end with respect to the conductor 2. (3) Next, the intensity of the characteristic X-rays of Mg is measured for each of the multiple measurement lines using the EPMA. Furthermore, 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 distance from the first end to the second end of the measurement line being the X-axis and the intensity of the Mg characteristic X-rays being the Y-axis, to create an 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 taken as the maximum 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 Mg intensity of the skeleton 22.
[0019] In the above line analysis using EPMA, the maximum Mg intensity of the skeleton 22 of the conductor 2 is typically smaller than the maximum Mg intensity of the surface layer 21 of the conductor 2. In the above line analysis using EPMA, the maximum Mg intensity of the skeleton 22 of the conductor 2 is, for example, 5,000 or less, preferably 3,000 or less, and more preferably 2,000 or less. On the other hand, in the above line analysis using EPMA, the maximum 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 Mg intensity of the surface layer 21 of the conductor 2 is, for example, 3,000 or more, preferably 4,000 or more. On the other hand, in the above line analysis using EPMA, the maximum Mg intensity of the surface layer 21 of the conductor 2 is, for example, 20,000 or less. When the maximum values of the Mg intensities of the surface layer and skeleton of the conductor are within such ranges, the electrical conductivity of the conductor can be further improved and conductivity variations in 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 value of the Mg intensity of the surface layers to the average value of the skeletons is such a value, the electrical conductivity of the conductor can be further improved and the variation in conductivity in the conductor can be more stably suppressed. On the other hand, the average value of the Mg intensity of the surface layers 21 is, for example, 13 times or less, or for example 12 times or less, the average value of the Mg intensity of the skeletons 22.
[0021] The thickness of the conductor 2 (the dimension in the thickness direction of the ceramic substrate 1) is, for example, 10 μm to 50 μm, and preferably 20 μm to 30 μm.
[0022] B. Details of the Semiconductor Manufacturing Equipment Members Hereinafter, each of the semiconductor manufacturing equipment members will be described in detail.
[0023] B-1. Ceramic substrate The ceramic substrate 1 can have any appropriate shape depending on the application of the heater for semiconductor manufacturing equipment. A typical shape of the ceramic substrate 1 is a plate shape. The ceramic substrate 1 preferably has a disk shape. The thickness of the ceramic substrate 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 a ceramic material and spinel with a thermal expansion coefficient of 2.0 × 10 -6 / ℃~10.0×10 -6 / °C ceramic materials include, for example, aluminum nitride (AlN), alumina (Al 2 O 3 Such ceramic materials may 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 substrate 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. Adjacent AlN crystal grains among the plurality of AlN crystal grains are typically bonded together. The average grain size of the plurality of AlN crystal grains is, for example, 1 μm to 5 μm, preferably 1 μm to 3 μm.
[0028] The AlN content in the ceramic substrate 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 substrate 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 AlN content in the ceramic substrate is within this range, high thermal conductivity, high toughness, and high dielectric strength can be achieved. The content of the constituent 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 is typically present at the grain boundaries between AlN crystal grains, or is formed by a reaction between 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 %, and even more preferably 1.2 wt % or less. When the content of spinel in the ceramic substrate is within this range, the volume resistivity of the ceramic substrate can be stably improved at high temperatures.
[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 crystalline 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 substrate 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 substrate 1, calculated as oxide, is, for example, 1.0 wt % or less, preferably 0.8 wt % or less. When the content of TiN in the ceramic substrate 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 substrate is suppressed, which is preferable.
[0032] The ceramic substrate 1 may further include another crystalline phase other than the AlN crystalline phase, the spinel crystalline phase, and the TiN crystalline phase. Examples of the other crystalline phase include α-aluminum oxide (α-alumina). The content of the other crystalline phase in the ceramic substrate 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 substrate 1 is typically 0 wt %. When the content of the other crystalline phase in the ceramic substrate is within this range, the volume resistivity of the ceramic substrate can be sufficiently ensured in the high temperature range.
[0033] Such a ceramic base 1 has a relatively high volume resistivity in a high temperature range. The volume resistivity of the ceramic base 1 at 600° C. is, for example, 1.0×10 9 Ω cm or more, preferably 1.2 × 10 9 Ω cm or more, more preferably 2.0 × 10 9 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 On the other hand, the volume resistivity of the ceramic substrate 1 at 600°C is, for example, 1.0 × 10 12Ω cm or less, for example, 1.5 × 10 11 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 substrate 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 in accordance with, for example, 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, 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. Electrical conductor The electrical 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 electrical conductor 2 provided on the ceramic substrate 1. A plurality of electrical conductors 2 may be provided on the ceramic substrate 1. In this case, the plurality of electrical 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 electrical conductor 2 include electrodes such as ESC electrodes and RF electrodes; resistance heating elements; and terminal portions.
[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 appropriate shape. Examples of the resistance heating element 2a include a coil shape, a zigzag shape, and 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 an ESC electrode 2b as the conductor 2. In the illustrated example, the ESC electrode 2b is spaced apart from the resistance heating element 2a in the thickness direction of the ceramic base 1 and is located between the mounting surface 1a and the resistance heating element 2a. When a DC voltage is applied to the ESC electrode 2b with the semiconductor substrate 8 mounted on the mounting surface 1a, the ESC electrode 2b is charged with either a positive or negative charge depending on 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 of the semiconductor substrate 8. As a result, a Johnsen-Rahbek (JR) force is generated between the semiconductor substrate 8 and the ESC electrode 2b, and the semiconductor substrate 8 is chucked to the ceramic base 1. Although not illustrated, the semiconductor manufacturing equipment member 100 may include multiple ESC electrodes 2b.
[0041] The ESC electrode 2b may function as an RF electrode (i.e., a radio frequency electrode) for plasma processing. That is, the ESC electrode 2b preferably functions as an RF / ESC electrode. Examples of plasma processing include film formation processing and etching processing. When such plasma processing is performed on the semiconductor substrate 8 on the mounting surface 1a, an upper electrode is disposed on the opposite side of the semiconductor substrate 8 from the ESC electrode 2b. In this state, when radio frequency power is supplied to the ESC electrode 2b, a processing gas can be excited in the space between the ceramic base 1 and the upper electrode to generate plasma. The plasma processing is performed on the semiconductor substrate 8 by the plasma.
[0042] The ESC electrode 2b may have any appropriate shape. The ESC electrode 2b typically has a plate shape. In one embodiment, the ESC electrode 2b has a shape similar to the outer shape of the ceramic substrate 1 when viewed in the thickness direction of the ceramic substrate 1. In the illustrated example, the center of the ESC electrode 2b and the center of the ceramic substrate 1 substantially coincide with each other when viewed in the thickness direction of the ceramic substrate 1.
[0043] As described above, the ESC electrode 2b includes the surface layer 21 containing spinel and the skeleton 22 containing a conductive material. The conductive material constituting the skeleton 22 of the ESC electrode 2b is preferably a metal or an inorganic compound. Specific examples of metals include molybdenum, niobium, tantalum, and alloys thereof. Specific examples of inorganic compounds include molybdenum carbide. These conductive materials may be used alone or in combination.
[0044] C. Manufacturing Method of a Semiconductor Manufacturing Equipment Member Next, a manufacturing method of a semiconductor manufacturing equipment member according to one embodiment will be described. The manufacturing method of the semiconductor manufacturing equipment member 100 includes a mixing step of mixing raw material powders of the ceramic substrate 1, a forming step of preparing multiple molded bodies from the substrate raw material mixture obtained in the mixing step, an arrangement step of arranging a conductor precursor between the multiple molded bodies, and a firing step of firing the stack obtained in the arrangement step.
[0045] C-1. Mixing Step In the mixing step, the raw 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. 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 TiO 2 The raw material is further mixed. 2 The raw material is TiO as the main component. 2 Contains TiO 2 The raw material is typically in powder form. 2 The average particle size D50 of the raw material is, for example, 0.1 μm to 0.5 μm.
[0050] TiO 2 The amount of the 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 the AlN raw material. 2 The amount of the raw material added is, for example, 1.0 part by weight or less with respect to 100 parts by weight of the AlN raw material.
[0051] In one embodiment, in the mixing step, a binder is added to the substrate raw material mixture. Examples of binders include polyvinyl acetal resins, cellulose ether resins, (meth)acrylic resins, and paraffin wax. Note that (meth)acrylic resins include acrylic resins and / or methacrylic resins. Binders may be used alone or in combination. Among such 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, wet mixing is performed in the mixing step. Any appropriate organic solvent is used in the wet mixing. Examples of the organic solvent include alcohols, esters, and hydrocarbons. The organic solvents may be used alone or in combination. Among the organic solvents, alcohols are preferred. Examples of the 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. The mixing step is typically carried out at room temperature (23°C) and atmospheric pressure (0.1 MPa). The mixing time is set arbitrarily and appropriately. The mixing time is, for example, 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 Step In one embodiment, the manufacturing method of 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. Examples of the granulation method include spray granulation and tumble granulation, with spray granulation being preferred. This prepares a granulated product of the substrate raw material mixture (hereinafter referred to as raw material granules).
[0057] C-3. Molding Step 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 the molding method 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 In this way, a plurality of molded bodies having a desired shape are prepared. In one embodiment, two molded bodies having a disk shape are prepared.
[0059] C-4. Arrangement Step 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 molded body 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 preferably include a WC raw material and a TiN raw material.
[0061] The WC raw material contains WC as a main component. The WC raw material is typically in the form of a powder. 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 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 may be mixed into the conductor raw material slurry as needed. Examples of the binder include the same binders as those used in the mixing step described above, and preferably a (meth)acrylic resin.
[0065] The preparation of such a conductor raw material slurry is typically carried out using any appropriate mixing device. Examples of the mixing device include the same mixing device as that used in the mixing step described above. The environmental conditions for the preparation of 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] The conductor raw material slurry is then printed onto the sheet material by any suitable printing method, such as screen printing, letterpress printing, offset printing, or 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 preferred. 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, the precursor of the conductor 2 can be prepared by directly printing the conductor raw material slurry onto the first molded body. 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 then 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 then placed on the first molded body. 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 thin film formation methods include transfer printing, powder molding, and sputtering.
[0073] As a result, 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 produces a laminate having a structure of first compact / precursor of the conductor / second compact.
[0074] C-5. Firing Step Next, in the 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. Before the firing step, a degreasing step may be performed as necessary.
[0075] The firing temperature is, for example, 1600° C. to 1900° C., preferably 1650° C. to 1850° C. The firing time is, for example, 0.5 hours to 100 hours. The environmental pressure in the firing step is, for example, 100 kPa to 900 kPa.
[0076] Examples of the sintering method include hot pressing and hot isostatic pressing (HIP), with hot pressing being preferred. In hot pressing, the laminate is typically placed in a hot press die (e.g., a carbon jig), heated to the sintering temperature as described above, and pressed at a predetermined pressure. The pressure in hot pressing is, 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, in the firing process, the conductor precursor is sandwiched between two compacts. This allows atoms within the compact to migrate (diffuse) more smoothly than when the conductor precursor is sandwiched between two sintered bodies, allowing the spinel to concentrate at the interface between the ceramic substrate and the conductor precursor. This allows the conductor precursor to be stably formed, having a surface layer containing spinel and a skeleton located inside the surface layer. In particular, when the conductor precursor is held on a sheet material, the spinel-containing surface layer can be formed even more stably. When the conductor precursor is formed by printing, the conductor 2 becomes a conductor 2 obtained by printing (printed conductor). In this manner, a semiconductor manufacturing equipment member 100 including a ceramic base material and a conductor is prepared.
[0078] D. Uses of the Semiconductor Manufacturing Equipment Member The semiconductor manufacturing equipment member 100 can be used in any suitable semiconductor manufacturing equipment. Examples of uses of the semiconductor manufacturing equipment member 100 include heaters, susceptors, electrostatic chucks, ceramic conductors, lead-in terminals, 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 an ESC electrode 2 b in addition to the resistance heating element 2 a.
[0080] The heater 101 is a heater for use in a semiconductor manufacturing device, and includes a semiconductor manufacturing device member 100 (ceramic substrate 1 and conductor 2), a ceramic shaft 5, a first power feed rod 6, and a second power feed rod 7.
[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 supply rod 7 is electrically connected to the ESC electrode 2 b. In the illustrated example, the second power supply rod 7 passes through the internal space of the ceramic shaft 5 and is electrically connected to the ESC electrode 2 b. The second power supply rod 7 is made of any appropriate conductive material. A voltage can be applied to the ESC electrode 2 b via the second power supply rod 7.
[0086] 2, in another embodiment, the 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 an ESC electrode 2b. In the illustrated example, the conductor 2 further includes a resistance heating element 2a in addition to the ESC electrode 2b.
[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 substrate 1 and is in contact with the electrode and / or resistance heating element in the thickness direction of the ceramic substrate 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 substrate 1. In the illustrated example, the ceramic substrate 1 has a recess 15. The recess 15 is recessed from the surface of the ceramic substrate 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 substrate 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 composed of WC and TiN. When the skeleton contains WC and TiN, cracking due to the difference in thermal expansion coefficient between the terminal portion and the ceramic substrate 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 also contains WC and TiN, they can be stably joined together, and delamination 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 2 c may be formed of a plurality of cylindrical members arranged concentrically, with a ceramic material similar to the ceramic substrate 1 typically disposed between the plurality of cylindrical members.
[0094] 7A and 7B , the terminal portion 2 c may be formed of a plurality of small pieces arranged in a staggered pattern, with the same ceramic material as the ceramic substrate 1 typically being disposed between the small pieces.
[0095] 8A and 8B , the terminal portion 2 c may be formed of a plurality of rod-shaped members spaced apart from one another, with the same ceramic material as the ceramic substrate 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 components constituting the terminal portion 2c. Therefore, in the semiconductor manufacturing equipment member 100 including such a terminal portion 2c, cracks and residual stress due to differences in thermal expansion can be reduced.
[0097] To manufacture the semiconductor manufacturing equipment component 100 having the terminal portion 2c shown in Figures 6A to 8B, for example, a tablet 20 corresponding to the configuration of the terminal portion is prepared using the above-described substrate raw material mixture and the above-described conductive material raw material. A typical tablet preparation device is a 3D printer. Next, in the above-described 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 first compact / tablet / second compact structure. The laminate is then fired in the above-described firing step. In other words, the compacts and the tablet are fired simultaneously. Since the compacts and the tablet contain the substrate raw material mixture, the difference in their shrinkage rates can be reduced. Therefore, the occurrence of cracks can be suppressed and residual stress can be reduced in the manufactured semiconductor manufacturing equipment component. In this manner, the semiconductor manufacturing equipment component 100 having the terminal portion 2c is manufactured.
[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 the conductor by 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. The thickness of the test pieces was 3 mm. The cross section of the test piece along the thickness direction of the ceramic substrate was polished to a mirror finish by lapping as the measurement surface. The measurement surface contained the conductor. The polished surface was then analyzed by EPMA to obtain an elemental mapping image. This identified the elemental composition of the surface layer and skeleton of the conductor. 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 by EPMA A test specimen was prepared in the same manner as in (1) Identification of the Elemental Composition of the Conductor by EPMA. Next, three measurement lines extending along the thickness direction of the ceramic substrate and passing through the conductor were determined on the measurement surface of the test specimen. 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 by EPMA under the following conditions to measure the intensities of the characteristic X-rays of Mg and Al in each measurement line. <Measurement conditions> Apparatus: JXA-8530FPlus manufactured by JEOL Ltd. Acceleration voltage: 15 kV Probe 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 value of the Mg intensity of the conductor was calculated from the Mg intensities of the conductor for the three measurement lines. Furthermore, the maximum intensity of the peak 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) in the Mg characteristic X-ray spectrum for each measurement line was taken as the Mg intensity of the surface layer. The average value of the Mg intensity of the surface layer was calculated from the Mg intensities of the surface layer for the three measurement lines. Furthermore, this Mg intensity measurement using EPMA was performed twice to measure the Mg intensity of different cross sections of the ceramic substrate provided with the conductor. The results are shown in Table 2.
[0104] (3) Measurement of the resistivity of the 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 ) was calculated. The dimension between the end faces where the conductor was 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 faces of the test piece using conductive paste. Thereafter, a current ranging from 0 mA to 150 mA was supplied to the conductor in the test piece at room temperature (25°C) and normal pressure (0.1 MPa), and the minute voltage value V (mV) generated was measured. The resistance R (Ω) of the conductor was calculated from the relationship between the current value I and the voltage value V. The resistivity ρ (Ω cm) of the conductor was then calculated based on 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 Resistivity Variation of Conductor The resistivity of the conductor of the heater for semiconductor manufacturing equipment manufactured in the examples and comparative examples was measured by the tester four-terminal method. More specifically, the resistance value of each of a plurality of arbitrary locations (specifically, four locations) on the same surface of the conductor was measured by the tester four-terminal method. Next, the resistivity of each location of the conductor was calculated from the measured resistance value of each location of the conductor 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 value of the resistivities at multiple points of the conductor, and γ represents the variation in resistivity.)
[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 TiO 2 0.5 parts by weight of raw material powder (average particle size D50: 0.3 μm) was added to a ball mill, and then an 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. The particle size of the raw material granules was 80 μm.
[0107] The raw material granules were then subjected to uniaxial pressing 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 charged into a ball mill and wet-mixed for 10 hours using an organic solvent, thereby obtaining 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 at 70°C for 30 minutes in the atmosphere. This resulted in the preparation of a precursor-holding sheet comprising a ceramic sheet and a conductor precursor formed on the ceramic sheet. The thickness of the conductor precursor was 50 μm. The ceramic sheet was made of aluminum nitride. The thickness of the ceramic sheet was 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 first compact with respect to the conductor precursor. This resulted in a laminate in which the precursor-holding sheet was sandwiched between the first compact and the second compact.
[0111] Next, the laminate was fired by hot pressing. More specifically, the laminate was fired 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 compact migrated (diffused), and a surface layer containing spinel was formed at the interface between the compact and the precursor of the conductor. In this way, a heater for semiconductor manufacturing equipment was manufactured, comprising a ceramic substrate and a conductor.
[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 changed to first molded sheets and second molded sheets prepared as follows, respectively. The first molded sheet and the second molded sheet were each prepared by forming a base material slurry prepared in the same manner as in Example 1 into a sheet shape using a doctor blade molding machine. The thickness of each of the first molded sheet and the second molded sheet was 200 μm.
[0113] Example 3: A first compact and a second compact were prepared in the same manner as in Example 1. A coil (hereinafter referred to as a Mo coil) made of molybdenum (Mo) was also prepared. The Mo coil was then sandwiched between the first compact and the second compact to obtain a laminate. The laminate was then fired in the same manner as in Example 1. As a result, the first compact and the second compact were sintered and integrated, and a surface layer containing spinel was formed on the surface of the Mo coil, and a conductor having a surface layer and a skeleton was embedded in the ceramic substrate. In this manner, a heater for semiconductor manufacturing equipment was manufactured, comprising a ceramic substrate and a conductor.
[0114] <<Comparative Example 1>> In preparing the conductor raw material slurry, 4.0 parts by weight of TiN powder was replaced with Al 2 O 3 A first compact and a second compact were prepared in the same manner as in Example 1, except that 4.0 parts by weight of the powder was used. Next, each of the first compact and the second compact was preliminarily sintered by hot pressing. More specifically, each of the first compact and the second compact was 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. This resulted in a conductor precursor being formed directly on the first sintered body. Next, a second sintered body was placed on the opposite side of the conductor precursor from the first sintered body. This resulted in a laminate in which the conductor precursor was sandwiched between the first sintered body and the second sintered body. Next, the laminate was fired in the same manner as in Example 1, and a heater for semiconductor manufacturing equipment was manufactured.
[0116]
[0117]
[0118] <Evaluation> As shown in Table 1, in Examples 1 to 3, the conductors had a surface layer containing spinel and a skeleton, while in Comparative Example 1, the conductor did not have a surface layer, and spinel was dispersed throughout the conductor. Thus, it can be seen that when a conductor includes a surface layer, the resistivity variation in the conductor can be significantly reduced. Since resistivity variation and conductivity variation in a conductor are correlated, it can be seen that small resistivity variation also small conductivity variation, and the conductor has excellent conductivity uniformity. Furthermore, as shown in Table 2, in Example 1, in the Mg characteristic X-ray spectrum, the maximum intensity of the peaks located in the surface layer (first interface and second interface) of the conductor was greater than the maximum intensity of the peak located in the skeleton of the conductor. In other words, it was confirmed that the Mg concentration in the surface layer (first interface and second interface) of the conductor was greater than the Mg concentration in the skeleton of the conductor.
[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.
[0120] REFERENCE SIGNS LIST 1 ceramic substrate 2 conductor 21 surface layer 22 skeleton 2a resistance heating element 2b ESC electrode 2c terminal portion 100 member for semiconductor manufacturing equipment
Claims
1. A semiconductor manufacturing device member comprising a ceramic substrate and a conductor provided within the ceramic substrate, wherein the ceramic substrate has a thermal expansion coefficient of 2.0 x 10 -6 / ℃~10.0×10 -6 / °C and a spinel, wherein the conductor has a surface layer containing the spinel and a skeleton located inside the surface layer.
2. The semiconductor manufacturing equipment member according to claim 1, wherein the skeleton is composed of tungsten carbide and titanium nitride.
3. A semiconductor manufacturing equipment member according to claim 2, wherein the tungsten carbide content in said skeleton is 50 wt % to 99 wt %, and the titanium nitride content in said skeleton is 1 wt % to 50 wt %.
4. The semiconductor manufacturing equipment member according to claim 1, wherein the skeleton is made of molybdenum.
5. A semiconductor manufacturing equipment component according to any one of claims 1 to 4, wherein, in a line analysis using an electron probe microanalyzer on a cross section of the ceramic substrate on which the conductor is provided, cut in the thickness direction, the average Mg intensity of the surface layer is at least three times the average Mg intensity of the skeleton.
6. A semiconductor manufacturing equipment member according to any one of claims 1 to 4, wherein the ceramic substrate further contains titanium nitride.
7. A semiconductor manufacturing equipment member according to claim 6, wherein the content of spinel in said ceramic base is 0.5 wt% to 55 wt%, and the content of titanium nitride in said ceramic base is 0.1 wt% to 1.0 wt%.
8. A semiconductor manufacturing equipment member according to any one of claims 1 to 4, wherein the dimension of the conductor in the thickness direction of the ceramic base is 10 μm to 50 μm.
9. A semiconductor manufacturing equipment member according to any one of claims 1 to 4, wherein the conductor is obtained by printing.
10. A semiconductor manufacturing equipment member according to any one of claims 1 to 4, comprising, as the conductor, an electrode and / or a resistance heating element, and a terminal portion electrically connected to the electrode and / or the resistance heating element.
Citation Information
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