Composite structures and semiconductor manufacturing apparatus equipped with composite structures
A composite structure with Y2SiO5 crystals and a specific peak ratio in X-ray diffraction enhances particle resistance in semiconductor manufacturing, addressing the challenge of high particle generation in fluorine plasma environments.
Patent Information
- Application Number
- JP2022028740
- Authority / Receiving Office
- JP · JP
- Patent Type
- Patents
- Current Assignee / Owner
- Filing Date
- 2022-02-26
- Publication Date
- 2026-08-25
- Estimated Expiration
- 2042-02-26
AI Technical Summary
Existing semiconductor manufacturing materials do not adequately address the need for high particle resistance in fluorine plasma environments, particularly with Y2SiO5-based materials lacking a clear relationship between plasma resistance and X-ray crystal diffraction peak ratios.
A composite structure comprising a base material with a ceramic coating of Y2SiO5 crystals, where the peak intensity ratio of (300) to (121) in X-ray diffraction is greater than 100%, enhancing particle resistance by setting specific lattice constants and indentation hardness.
The composite structure effectively suppresses fluoridation and etching in fluorine plasma environments, reducing particle generation and improving resistance, with improved lattice constants and hardness.
Smart Images

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Abstract
Description
Technical Field
[0001] The present invention relates to a composite structure excellent in low-particle generation, which is preferably used as a member for a semiconductor manufacturing apparatus, and a semiconductor manufacturing apparatus including the same.
Background Art
[0002] A technique of coating a ceramic on a substrate surface to impart a function to the substrate is known. For example, as a member for a semiconductor manufacturing apparatus used in a plasma irradiation environment such as a semiconductor manufacturing apparatus, a member having a film with high plasma resistance formed on its surface is used. For the film, for example, oxide ceramics such as alumina (Al2O3) and yttria (Y2O3), and fluorides such as yttrium fluoride (YF3) and yttrium oxyfluoride (YOF) are used.
[0003] It has also been proposed to use a Y2SiO5-based material as a member for which plasma resistance is required (Patent Documents 1 and 2). However, these prior arts do not disclose or suggest any relationship between the plasma resistance of the Y2SiO5-based material and a specific peak ratio of X-ray crystal diffraction.
[0004] With the miniaturization of semiconductors, higher levels of particle resistance are required for various members in semiconductor manufacturing apparatuses, and materials corresponding thereto are still required.
Prior Art Documents
Patent Documents
[0005]
Patent Document 1
Patent Document 2
Summary of the Invention
Problems to be Solved by the Invention
[0006] The present inventors have now discovered that fluoridation in a fluorine plasma environment can be suppressed in Y2SiO5-based materials by setting a specific peak ratio of X-ray crystal diffraction to a specific value. This invention is based on this discovery.
[0007] Therefore, the present invention aims to provide a composite structure with excellent particle resistance (low-particle generation). Furthermore, it aims to provide this composite structure as a component for semiconductor manufacturing equipment, and semiconductor manufacturing equipment using it. [Means for solving the problem]
[0008] Furthermore, the composite structure according to the present invention is a composite structure comprising a base material and a structure provided on the base material and having a surface, wherein the structure mainly contains Y2SiO5 crystals, and the peak intensity ratio (300) / (121), which is the ratio of the (300) peak to the (121) peak in the X-ray diffraction of the crystals, is greater than 100%.
[0009] Furthermore, the composite structure according to the present invention is intended for use in environments where particle resistance is required.
[0010] Furthermore, the semiconductor manufacturing apparatus according to the present invention is equipped with the composite structure according to the present invention described above. [Brief explanation of the drawing]
[0011] [Figure 1] This is a schematic cross-sectional view of a member having a structure according to the present invention. [Figure 2] Figures 2a to 2c are graphs showing the relationship between the lattice constant and the amount of fluoride in the structure according to the present invention. [Figure 3] Figure 3a is a graph showing the intensity of X-ray diffraction data for the structure according to the present invention, and Figure 3b is a graph showing the relationship between the peak intensity ratio and the amount of fluoride for the structure according to the present invention. [Figure 4]This graph shows the relationship between the indentation hardness and fluoride content of the structure according to the present invention. [Figure 5] These are SEM images of the surface of a structure according to the present invention, before and after standard plasma test 1 or 2. [Modes for carrying out the invention]
[0012] composite structure The basic structure of the composite structure according to the present invention will be explained with reference to Figure 1. Figure 1 is a schematic cross-sectional view of the composite structure 10 according to the present invention. The composite structure 10 consists of a structure 20 provided on a base material 15, and the structure 20 has a surface 20a.
[0013] The structure 20 of the composite structure according to the present invention is a so-called ceramic coating. By applying a ceramic coating, various physical properties and characteristics can be imparted to the base material 15. In this specification, unless otherwise specified, the terms structure (or ceramic structure) and ceramic coating are used synonymously.
[0014] The composite structure 10 is installed, for example, inside the chamber of a semiconductor manufacturing apparatus having a chamber. The composite structure 10 may constitute the inner wall of the chamber. Inside the chamber, SF-based or CF-based fluorine gases are introduced to generate plasma, and the surface 20a of the structure 20 is exposed to the plasma atmosphere. Therefore, the structure 20 on the surface of the composite structure 10 is required to have particle resistance. Furthermore, the composite structure according to the present invention may be used as a component mounted outside the interior of a chamber. In this specification, the semiconductor manufacturing apparatus using the composite structure according to the present invention is used to include any semiconductor manufacturing apparatus (semiconductor processing apparatus) that performs processing such as annealing, etching, sputtering, and CVD.
[0015] Base material In the present invention, the substrate 15 is not particularly limited as long as it is used for its intended purpose, and is composed of, for example, alumina, quartz, anodized aluminum, metal, or glass, and is preferably composed of alumina. According to a preferred embodiment of the present invention, the arithmetic mean roughness Ra (JIS B0601: 2001) of the surface of the substrate 15 on which the structure 20 is formed is, for example, less than 5 micrometers (μm), preferably less than 1 μm, and more preferably less than 0.5 μm.
[0016] structure In the present invention, the structure contains Y2SiO5 crystals as a main component, and the lattice constants of the crystals satisfy at least one of a > 9.06, b > 6.93, and c > 6.70, and preferably the lattice constants satisfy at least one of a > 9.10, b > 6.94, c > 6.73.
[0017] In the present invention, the main component of the structure refers to a compound that is relatively more contained than other compounds contained in the structure 20 by quantitative or semi-quantitative analysis by X-ray diffraction (XRD) of the structure. For example, the main component is the compound most contained in the structure, and the ratio occupied by the main component in the structure is 70 wt% or more, preferably 90 wt% or more, and most preferably 100% by mass ratio.
[0018] In the present invention, components that the structure may contain in addition to Y2SiO5 include oxides such as scandium oxide, europium oxide, gadolinium oxide, erbium oxide, ytterbium oxide, and fluorides such as yttrium fluoride and yttrium oxyfluoride, and may contain two or more of these.
[0019] In the present invention, the structure is not limited to a single-layer structure and may be a multilayer structure. It is also possible to include a plurality of layers mainly composed of Y2SiO5 crystals with different compositions, and another layer, for example, a layer containing Y2O3, may be provided between the substrate and the structure.
[0020] Peak intensity ratio In the present invention, the peak intensity ratio (300) / (121), which is the ratio of the (300) peak to the (121) peak in the X-ray diffraction of the Y2SiO5 crystal, is set to be greater than 100%, and more preferably, the peak intensity ratio (300) / (121) is set to be greater than 110%.
[0021] The peak intensity ratio can be measured using XRD. A "Smart Lab / Rigaku" XRD instrument is used, and the XRD measurement conditions are as follows: characteristic X-ray is CuKα (λ=1.5418Å), tube voltage is 45kV, tube current is 200mA, sampling step is 0.01°, and scan speed is 10.0° / min. The peak intensity ratio (300) / (121) is calculated from the peak intensity at a diffraction angle 2θ=32.5°±0.4 (32.1°~32.9°) attributed to Miller index (hkl)=(121) and the peak intensity at a diffraction angle 2θ=31.1°±0.4° (30.7°~31.5°) attributed to Miller index (hkl)=(300). Since the structure in this invention is a novel structure with lattice constants a=9.0139 and c=6.6427 greater than those of the present invention, the peak positions (2θ) assigned to each Miller index (hlk) actually measured by XRD are shifted by 0.1 to 0.4° to the lower angle side compared to the theoretical peak positions (2θ) assigned to each Miller index (hkl).
[0022] Lattice constant According to one preferred embodiment of the present invention, the Y2SiO5 crystals contained in the structure satisfy at least one of the following lattice constants: a>9.06, b>6.93, and c>6.70, preferably a>9.10, b>6.94, and c>6.73. This suppresses fluoridation of the structure and improves its particle resistance.
[0023] According to the ICDD card (reference code: 01-070-5613), the lattice constants of Y2SiO5 are a=9.01 (Å), b=6.93 (Å), and c=6.64 (Å). The present invention is characterized in that at least one of the lattice constants a, b, and c takes the above value which exceeds these values.
[0024] In this invention, the lattice constant is measured using XRD. For example, a "Smart Lab / Rigaku" XRD instrument is used, and the XRD measurement conditions are set to CuKα (λ=1.5418Å) as the characteristic X-ray, tube voltage 45kV, tube current 200mA, sampling step 0.01°, and scan speed 10.0° / min. For example, using the XRD analysis software "SmartLab Studio II / Rigaku", the obtained XRD diffraction pattern is identified as a monoclinic crystal with chemical formula Y2SiO5, as shown on ICDD card 01-070-5613. Subsequently, using the same XRD analysis software "SmartLab Studio II / Rigaku", the lattice constant is calculated by refining the lattice constant using the external standard method. Metallic Si is used as the external standard, and the following peaks are specified for use in calculating the lattice constant: the peak at a diffraction angle of 2θ = 16.4° attributed to Miller index (hkl) = (110), the peak at a diffraction angle of 2θ = 20.6° attributed to Miller index (hkl) = (200), the peak at a diffraction angle of 2θ = 31.1° attributed to Miller index (hkl) = (300), the peak at a diffraction angle of 2θ = 32.5° attributed to Miller index (hkl) = (121), the peak at a diffraction angle of 2θ = 33.7° attributed to Miller index (hkl) = (310), the peak at a diffraction angle of 2θ = 46.3° attributed to Miller index (hkl) = (321), and the peak at a diffraction angle of 2θ = 48.8° attributed to Miller index (hkl) = (123). Since the structure in this invention is a novel structure with lattice constants greater than a=9.0139 and c=6.6427, the peak positions (2θ) assigned to each Miller index (hlk) actually measured by XRD are shifted by 0.1 to 0.4° to the lower angle side compared to the theoretical peak positions (2θ) assigned to each Miller index (hkl). Otherwise, the measurement of lattice constants can be performed in accordance with JIS K0131.
[0025] Indentation hardness According to one preferred embodiment of the present invention, the material contains Y2SiO5 crystals as the main component and has an indentation hardness greater than 7.5 GPa. This improves particle resistance. The indentation hardness is more preferably 10 GPa or higher. The upper limit of the indentation hardness is not particularly limited and may be determined by the required characteristics, but for example, it is 18 GPa or less.
[0026] The indentation hardness of a structure is measured by the following method: a micro-indentation hardness test (nanoindentation) is performed on the surface of a structure containing Y2SiO5 crystals as the main component on a substrate. A Berkovich indenter is used, and the indentation depth is fixed at 200 nm. The indentation hardness (indentation hardness) H IT Measure the H on the surface. IT Select a surface that excludes scratches and dents as the measurement point. More preferably, the surface should be a polished smooth surface. The number of measurement points should be at least 25. The 25 or more measured points H IT The average value of these values shall be defined as the hardness in this invention. Other test and analytical methods, procedures for verifying the performance of the test equipment, and conditions required for standard reference samples shall conform to ISO 14577.
[0027] Etching rate and fluoride content The composite structure according to the present invention can suppress fluorination in a fluorine plasma environment and also suppress etching by plasma.
[0028] In a preferred embodiment of the present invention, the surface roughness Sa (determined in accordance with ISO 25178) of the structure after the standard plasma test 1 described below is preferably less than 0.06 μm, and more preferably less than 0.03 μm. This provides superior particle resistance.
[0029] In this invention, the tests involving exposure to fluorine-based plasma as defined below will be referred to as Standard Plasma Test 1 and 2, respectively.
[0030] Plasma exposure conditions For a structure containing Y2SiO5 crystals as the main component on a substrate, its surface is exposed to a plasma atmosphere using an inductively coupled reactive ion etching (ICP-RIE) apparatus. The plasma atmosphere formation conditions are as follows:
[0031] Standard plasma test 1: The process gas used is SF6100 sccm, and the power output consists of a 1500W coil output for the ICP and a 750W bias output.
[0032] Standard plasma test 2: The process gas is SF6100 sccm, the power output is 1500W for the ICP coil, and the bias output is OFF (0W). In other words, no high-frequency power is applied to the electrostatic chuck bias.
[0033] For both standard plasma tests 1 and 2, the chamber pressure is 0.5 Pa and the plasma exposure time is 1 hour. The semiconductor manufacturing equipment component is placed on a silicon wafer adsorbed by an electrostatic chuck provided in the inductively coupled reactive ion etching apparatus so that its surface is exposed to the plasma atmosphere formed under these conditions.
[0034] Crystallite size Furthermore, according to one aspect of the present invention, Y2SiO5 is a polycrystalline material. Its average crystallite size is preferably less than 50 nm, more preferably less than 30 nm, and most preferably less than 20 nm. The small average crystallite size allows for the reduction of particles generated by the plasma.
[0035] In this specification, "polycrystalline material" refers to a structure formed by the bonding and accumulation of crystalline particles. Preferably, the crystalline particles constitute a crystal substantially by themselves. The diameter of the crystalline particles is, for example, 5 nanometers (nm) or larger.
[0036] In this invention, crystallite size is measured, for example, by X-ray diffraction. The average crystallite size can be calculated using Scherrer's formula.
[0037] Manufacturing of composite structures The composite structure according to the present invention may be manufactured by various purposeful manufacturing methods, as long as a structure having the above-described lattice constant can be realized on a substrate. That is, it may be manufactured by a method that can form a structure containing Y2SiO5 as the main component and having the above-described lattice constant on a substrate, for example, the structure can be formed on the substrate by physical vapor deposition (PVD) or chemical vapor deposition (CVD). Examples of PVD methods include electron beam physical vapor deposition (EB-PVD), ion beam assisted deposition (IAD), electron beam ion assisted deposition (EB-IAD), ion plating, and sputtering. Examples of CVD methods include thermal CVD, plasma CVD (PECVD), organometallic CVD (MOCVD), mist CVD, laser CVD, and atomic layer deposition (ALD). Furthermore, according to another aspect of the present invention, it can be formed by arranging fine particles such as brittle material on the surface of a substrate and applying a mechanical impact force to the fine particles. Here, methods for "applying mechanical impact force" include using high-speed rotating, high-hardness brushes or rollers or pistons that move up and down at high speed, utilizing the compressive force produced by shock waves generated during an explosion, applying ultrasound or plasma, or a combination of these.
[0038] Furthermore, the composite structure according to the present invention can preferably be formed by the aerosol deposition method (AD method). The AD method involves injecting an aerosol, which is a mixture of fine particles containing brittle materials such as ceramics dispersed in a gas, from a nozzle toward a substrate. The fine particles collide with the substrate, such as metal, glass, ceramics, or plastic, at high speed. The impact of this collision causes deformation and fracture of the brittle material fine particles, thereby joining them together and directly forming a structure (ceramic coating) containing the constituent materials of the fine particles on the substrate, for example, as a layered or film-like structure. This method does not require heating or cooling means, and the structure can be formed at room temperature, and a structure with mechanical strength equal to or greater than that of a fired body can be obtained. In addition, by controlling the conditions for impacting the fine particles, as well as the shape and composition of the fine particles, it is possible to vary the density, mechanical strength, and electrical properties of the structure in various ways. By setting these conditions to realize the composite structure according to the present invention, that is, to achieve the lattice constant according to the present invention, the composite structure according to the present invention can be manufactured. For example, it can be manufactured by controlling the type and flow rate of the carrier gas, adjusting the particle size of the raw material particles, and controlling various conditions that combine these factors.
[0039] In this specification, "fine particles" means particles with an average particle size of 5 micrometers (μm) or less, as identified by particle size distribution measurement or scanning electron microscopy, when the primary particles are dense particles. When the primary particles are porous particles that are easily broken by impact, it means particles with an average particle size of 50 μm or less.
[0040] Furthermore, in this specification, "aerosol" refers to a solid-gas mixed phase in which the aforementioned fine particles are dispersed in a gas (carrier gas) such as helium, nitrogen, argon, oxygen, dry air, or a mixture of these gases, and also includes cases where "aggregates" are present, but preferably refers to a state in which the fine particles are substantially dispersed individually. The gas pressure and temperature of the aerosol may be set arbitrarily considering the physical properties of the desired structure, but the concentration of fine particles in the gas is preferably in the range of 0.0003 mL / L to 5 mL / L at the time of injection from the discharge port, when the gas pressure is converted to 1 atmosphere and the temperature to 20 degrees Celsius.
[0041] The aerosol deposition process is typically carried out at room temperature, and structures can be formed at a temperature well below the melting point of the particulate material, i.e., below several hundred degrees Celsius. In this specification, "room temperature" means a temperature significantly lower than the sintering temperature of the ceramics, and substantially refers to a room temperature environment of 0 to 100°C. In this specification, "powder" refers to the state in which the aforementioned particulate matter has naturally aggregated. [Examples]
[0042] The present invention will be further described by the following examples, but the present invention is not limited to these examples.
[0043] As raw materials for the structures used in the examples, we prepared powders named F-1 and F-2, as shown in Table 1 below, using Y2O3 powder or Y2SiO5 powder.
[0044] Furthermore, the average particle size was measured as follows: Using the laser diffraction particle size distribution analyzer "LA-960 / HORIBA," the particles were appropriately dispersed using ultrasound, and then the particle size distribution was evaluated. The resulting median diameter D50 was used as the average particle size.
[0045] As shown in Table 1 below, multiple samples were prepared by varying the combination of these raw materials and film formation conditions (type and flow rate of carrier gas, etc.) to create structures on substrates. The particle resistance of the obtained samples was evaluated after standard plasma tests 1 and 2. In this example, the aerosol deposition method was used to prepare the samples.
[0046] [Table 1]
[0047] As shown in the table, nitrogen (N2) or helium (He) was used as the carrier gas. The aerosol was obtained by mixing the carrier gas with the raw material powder (raw material fine particles) in the aerosol generator. The obtained aerosol was sprayed from a nozzle connected to the aerosol generator towards the substrate placed inside the film-forming chamber due to the pressure difference. At this time, the air inside the film-forming chamber was exhausted to the outside by a vacuum pump.
[0048] sample Each of the structures obtained as described above contained a polycrystalline material of Y2O3 or Y2SiO5 as its main component, and the average crystallite size of the polycrystalline material was less than 30 nm in all cases, with the average crystallite size of sample 1 being 12 nm.
[0049] Crystallite size was measured using XRD. A "Smart Lab / Rigaku" XRD system was used. The XRD measurement conditions were: characteristic X-ray CuKα (λ=1.5418Å), tube voltage 45kV, tube current 200mA, sampling step 0.01°, and scan speed 10.0° / min. The average crystallite size was calculated using Scherrer's formula. A value of 0.94 was used for K in Scherrer's formula.
[0050] The main components of Y2SiO5 on the substrate were measured by XRD. A "Smart Lab / Rigaku" XRD system was used. The XRD measurement conditions were: characteristic X-ray CuKα (λ=1.5418Å), tube voltage 45kV, tube current 200mA, sampling step 0.01°, and scan speed 10.0° / min. The XRD analysis software "SmartLab Studio II / Rigaku" was used to calculate the main components, and the ratio of each crystalline phase was calculated by Rietveld analysis. For polycrystalline structures in the case of stacked structures, it is desirable to use measurement results from a depth region of less than 1μm from the outermost surface using thin-film XRD.
[0051] Test evaluation For samples 1-5 obtained as described above, the following lattice constants, peak intensity ratios, indentation hardness, etching rate, arithmetic mean height Sa after plasma irradiation, and fluoride content were measured. Standard plasma tests were also performed as follows.
[0052] Measurement of lattice constants The lattice constant of Y2SiO5 was evaluated using XRD according to the following procedure. A "Smart Lab / Rigaku" XRD instrument was used. The XRD measurement conditions were as follows: characteristic X-ray was CuKα (λ=1.5418Å), tube voltage 45kV, tube current 200mA, sampling step 0.01°, and scan speed 10.0° / min. Using the XRD analysis software "SmartLab Studio II / Rigaku", the obtained XRD diffraction pattern was identified as a monoclinic crystal of chemical formula Y2SiO5, as shown on ICDD card 01-070-5613. Subsequently, using the same XRD analysis software "SmartLab Studio II / Rigaku", the lattice constant was calculated by refining the lattice constant using the external standard method. Metallic Si was used as the external standard. Furthermore, the following peaks were specified as those used to calculate the lattice constant: the peak at a diffraction angle of 2θ = 16.4° attributed to Miller index (hkl) = (110), the peak at a diffraction angle of 2θ = 20.6° attributed to Miller index (hkl) = (200), the peak at a diffraction angle of 2θ = 31.1° attributed to Miller index (hkl) = (300), the peak at a diffraction angle of 2θ = 32.5° attributed to Miller index (hkl) = (121), the peak at a diffraction angle of 2θ = 33.7° attributed to Miller index (hkl) = (310), the peak at a diffraction angle of 2θ = 46.3° attributed to Miller index (hkl) = (321), and the peak at a diffraction angle of 2θ = 48.8° attributed to Miller index (hkl) = (12-3). Furthermore, since the structure in this invention is a novel structure with lattice constants greater than a=9.0139 and c=6.6427, the peak positions (2θ) assigned to each Miller index (hlk) actually measured by XRD are shifted by 0.1 to 0.4° to the lower angle side compared to the theoretical peak positions (2θ) assigned to each Miller index (hkl). In addition, the measurement of lattice constants conforms to JIS K0131.
[0053] Measurement of peak intensity ratio The peak intensity ratio of the structure was evaluated using XRD according to the following procedure. A "Smart Lab / Rigaku" XRD instrument was used. The XRD measurement conditions were as follows: characteristic X-ray was CuKα (λ=1.5418Å), tube voltage 45kV, tube current 200mA, sampling step 0.01°, and scan speed 10.0° / min. For monoclinic Y2SiO5, the peak intensity at the diffraction angle 2θ=32.5°±0.4 (32.1°~32.9°) attributed to Miller index (hkl)=(121) was denoted as α, and the peak intensity at the diffraction angle 2θ=31.1°±0.4° (30.7°~31.5°) attributed to Miller index (hkl)=(300) was denoted as β. The peak intensity ratio was calculated using γ=β / α. Furthermore, since the structure in this invention is a novel structure with lattice constants a=9.0139 and c=6.6427 greater than those of the present invention, the peak positions (2θ) assigned to each Miller index (hlk) actually measured by XRD are shifted by 0.1 to 0.4° to the lower angle side compared to the theoretical peak positions (2θ) assigned to each Miller index (hkl).
[0054] Measurement of indentation hardness The indentation hardness of structures on a substrate was evaluated using a nanoindentation test (micro-indentation) according to the following procedure. The "ENT-2100 / Elionix" nanoindenter was used. For the nanoindentation test, a Berkovich indenter was used, the test mode was set to a set indentation depth, and the indentation depth was set to 200 nm. Indentation hardness (HIT) was measured. HIT measurements were randomly placed on the surface of the structure, with at least 25 measurement points. The average value of the 25 or more measured HITs was used as the hardness.
[0055] Standard plasma testing Standard plasma tests 1 and 2 were performed on the above-mentioned samples under the conditions described above, and the particle resistance after these tests was evaluated using the following procedure. A "Muc-21 Rv-Aps-Se / Sumitomo Precision Products" ICP-RIE apparatus was used. For both standard plasma tests 1 and 2, the chamber pressure was 0.5 Pa and the plasma exposure time was 1 hour. The samples were placed on a silicon wafer adsorbed by an electrostatic chuck on an inductively coupled reactive ion etching apparatus so that their surface was exposed to the plasma atmosphere formed under these conditions.
[0056] Etching rate The etching rate (e) of the structure after Standard Plasma Test 1 was calculated using the formula e = d / t, based on the step difference (d) between the plasma-unexposed and exposed regions measured with a scanning laser microscope (LEXT OLS-4000, Olympus Corporation) and the plasma exposure time (t). The plasma-unexposed region was formed by partially masking the structure surface with a polyimide film before Standard Plasma Test 1.
[0057] Arithmetic mean height Sa after plasma irradiation The surface roughness of the structure after standard plasma test 1 was evaluated using a laser microscope to determine the arithmetic mean height (Sa) as defined in ISO 25178. The laser microscope used was an "OLS4500 / Olympus Corporation" laser microscope. The objective lens used was an MPLAPON100XLEXT, and the cutoff value λc was set to 25 μm.
[0058] Fluoride amount After Standard Plasma Test 2, the atomic concentration (%) of fluorine (F) atoms was measured at 1-second intervals during sputtering time, from 5 seconds to 149 seconds, using X-ray photoelectron spectroscopy (XPS) for depth profiling with ion sputtering. A K-Alpha / Thermo Fisher Scientific XPS instrument was used. All obtained atomic concentrations (%) of fluorine (F) atoms at 1-second intervals from 5 seconds to 149 seconds were integrated to obtain the cumulative fluorination amount (%) on the structure surface. To eliminate the influence of carbon (C) contamination adhering to the surface, data from sputtering time 0 seconds to 5 seconds were not included.
[0059] The results of the above tests are shown in the table below. [Table 2]
[0060] The relationship between the lattice constant and the amount of fluoride is shown graphically in Figures 2a, 2b, and 2c. Figure 3a is a graph showing the intensity of the X-ray diffraction data, and the relationship between the peak intensity ratio and the amount of fluoride is shown graphically in Figure 3b. The relationship between the indentation hardness and the amount of fluoride is shown graphically in Figure 4.
[0061] SEM image SEM images of the structure surface after standard plasma tests 1 and 2 were taken as follows. Specifically, the corrosion state of the plasma-exposed surface was evaluated using a scanning electron microscope (SEM). The SEM used was a "SU-8220 / Hitachi, Ltd." The acceleration voltage was set to 3kV. The resulting images are shown in Figure 5.
[0062] Embodiments of the present invention have been described above. However, the present invention is not limited to these descriptions. Modifications made by those skilled in the art to the above-described embodiments are also included within the scope of the present invention, as long as they retain the features of the present invention. For example, the shape, dimensions, material, and arrangement of structures, base materials, etc., are not limited to those exemplified and can be modified as appropriate. Furthermore, the elements of each of the above-described embodiments can be combined to the extent technically feasible, and combinations thereof are also included within the scope of the present invention, as long as they retain the features of the present invention. [Explanation of symbols]
[0063] 10... Composite structures, 15... Base materials, 20... Structures, 20a... Surfaces of structures
Claims
1. A composite structure comprising a base material and a structure provided on the base material and having a surface, The aforementioned structure is Y 2 SiO 5 A composite structure comprising crystals as its main component, wherein the peak intensity ratio (300) / (121), which is the ratio of the (300) peak to the (121) peak in the X-ray diffraction of the Y2SiO5 crystal, is greater than 100%.
2. The composite structure according to claim 1, wherein the peak intensity ratio (300) / (121) is greater than 110%.
3. The aforementioned structure is Y 2 SiO 5 A composite structure according to claim 1 or 2, comprising 70 wt% or more of the above.
4. The aforementioned structure is Y 2 SiO 5 A composite structure according to claim 1 or 2, comprising 90 wt% or more of the above.
5. The aforementioned structure is substantially Y 2 SiO 5 A composite structure according to claim 1 or 2, comprising the above.
6. The Y of the structure 2 SiO 5 The composite structure according to any one of claims 1 to 5, wherein the average crystallite size of is 50 nm or less.
7. A composite structure according to any one of claims 1 to 6, wherein the surface roughness Sa (determined in accordance with ISO 25178) of the structure after standard plasma test 1 is less than 0.06 μm.
8. A composite structure according to any one of claims 1 to 7, used in an environment where particle resistance is required.
9. A composite structure according to claim 8, which is a component for semiconductor manufacturing equipment.
10. A semiconductor manufacturing apparatus comprising a composite structure according to any one of claims 1 to 8.
Citation Information
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