US20170140902A1 - Corrosion-resistant components and methods of making - Google Patents

Corrosion-resistant components and methods of making Download PDF

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Publication number
US20170140902A1
US20170140902A1 US15/353,429 US201615353429A US2017140902A1 US 20170140902 A1 US20170140902 A1 US 20170140902A1 US 201615353429 A US201615353429 A US 201615353429A US 2017140902 A1 US2017140902 A1 US 2017140902A1
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Prior art keywords
corrosion
layer
resistant
rare earth
porous layer
Prior art date
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Abandoned
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US15/353,429
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English (en)
Inventor
Matthew Simpson
Ramesh Divakar
Alan Filer
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Coorstek Inc
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Coorstek Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Coorstek Inc filed Critical Coorstek Inc
Priority to US15/353,429 priority Critical patent/US20170140902A1/en
Priority to JP2019547068A priority patent/JP7054705B2/ja
Priority to EP19178123.6A priority patent/EP3560906B1/en
Priority to EP17729576.3A priority patent/EP3526177B1/en
Priority to KR1020197017241A priority patent/KR102384436B1/ko
Priority to CN201780070875.0A priority patent/CN109963825B/zh
Priority to PCT/US2017/032468 priority patent/WO2018093414A1/en
Priority to US15/593,888 priority patent/US11376822B2/en
Publication of US20170140902A1 publication Critical patent/US20170140902A1/en
Assigned to COORSTEK, INC. reassignment COORSTEK, INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: DIVAKAR, RAMESH, FILER, Alan, SIMPSON, MATTHEW
Priority to US17/382,735 priority patent/US20220013335A1/en
Assigned to JPMORGAN CHASE BANK, N.A. reassignment JPMORGAN CHASE BANK, N.A. SECURITY INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: COORSTEK, INC.
Abandoned legal-status Critical Current

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    • C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
    • C04B2237/32—Ceramic
    • C04B2237/36—Non-oxidic
    • C04B2237/366—Aluminium nitride
    • C—CHEMISTRY; METALLURGY
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
    • C04B2237/32—Ceramic
    • C04B2237/36—Non-oxidic
    • C04B2237/368—Silicon nitride
    • C—CHEMISTRY; METALLURGY
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
    • C04B2237/40—Metallic
    • C04B2237/403—Refractory metals
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
    • C04B2237/56—Using constraining layers before or during sintering
    • C04B2237/567—Using constraining layers before or during sintering made of metal
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    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
    • C04B2237/68—Forming laminates or joining articles wherein at least one substrate contains at least two different parts of macro-size, e.g. one ceramic substrate layer containing an embedded conductor or electrode
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    • C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
    • C04B2237/70—Forming laminates or joined articles comprising layers of a specific, unusual thickness
    • C04B2237/704—Forming laminates or joined articles comprising layers of a specific, unusual thickness of one or more of the ceramic layers or articles
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    • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
    • C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
    • C04B2237/70—Forming laminates or joined articles comprising layers of a specific, unusual thickness
    • C04B2237/708—Forming laminates or joined articles comprising layers of a specific, unusual thickness of one or more of the interlayers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/16—Vessels
    • H01J2237/166—Sealing means
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/32—Processing objects by plasma generation
    • H01J2237/33—Processing objects by plasma generation characterised by the type of processing
    • H01J2237/334—Etching
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/32—Processing objects by plasma generation
    • H01J2237/33—Processing objects by plasma generation characterised by the type of processing
    • H01J2237/334—Etching
    • H01J2237/3341—Reactive etching
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32009—Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
    • H01J37/32082—Radio frequency generated discharge
    • H01J37/321—Radio frequency generated discharge the radio frequency energy being inductively coupled to the plasma
    • H01J37/32119—Windows
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32431—Constructional details of the reactor
    • H01J37/32458—Vessel
    • H01J37/32522—Temperature
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32431—Constructional details of the reactor
    • H01J37/32798—Further details of plasma apparatus not provided for in groups H01J37/3244 - H01J37/32788; special provisions for cleaning or maintenance of the apparatus
    • H01J37/32853—Hygiene
    • H01J37/32862—In situ cleaning of vessels and/or internal parts

Definitions

  • the present disclosure relates generally to corrosion-resistant components for the processing of equipment, such as semiconductors, and to methods of making such corrosion-resistant components.
  • PVD Physical vapor deposition
  • CVD chemical vapor deposition
  • High rate deposition tends to produce fissures between grains.
  • Denser coatings made by CVD are characterized by a grain size that tends to be small, typically less than 100 nm.
  • Aerosol deposition has been used and it also suffers from cost limitations and an inability to make thick coatings that do not spall.
  • Thermal plasma spray is the most widely used coating technology in the semiconductor equipment industry, but it cannot produce rare-earth coatings with porosity less than 1%, and therefore is prone to the shedding of particles.
  • plasma spray coatings commonly contain a high density of microcracks (typically more than 100/mm 2 ), and this, together with the porosity, leads to the shedding of particles.
  • Ceramic lids are commonly interposed between induction coils and induction plasma used for etching in the semiconductor industry. Insulating rings surrounding the wafer chuck and other chamber parts in etch and deposition equipment need to be corrosion-resistant as well as stable, for the reasons outlined above.
  • Embodiments of the present disclosure include a corrosion-resistant component configured for use with a semiconductor processing reactor, the corrosion-resistant component comprising: a) a ceramic insulating substrate; and, b) a corrosion-resistant non-porous layer associated with the ceramic insulating substrate, the corrosion-resistant non-porous layer having a composition comprising at least 15% by weight of a rare earth compound based on total weight of the corrosion-resistant non-porous layer; and, the corrosion-resistant non-porous layer characterized by a microstructure substantially devoid of microcracks and fissures, and having an average grain size of at least about 100 nm and at most about 100 ⁇ m.
  • the ceramic insulating substrate is selected from the group consisting of aluminum oxide, aluminum nitride, silicon nitride, silicate-based materials and mixtures of two or more thereof.
  • the corrosion-resistant component according to either paragraph [0008] or [0009], wherein the rare earth compound is selected from the group consisting of yttrium oxide (Y2O3), yttrium silicates, yttrium fluorides, yttrium oxyfluorides, yttrium aluminates, nitrides, complex nitride compounds, and combinations of two or more thereof.
  • Y2O3 yttrium oxide
  • silicates yttrium fluorides
  • yttrium oxyfluorides yttrium aluminates
  • nitrides complex nitride compounds
  • the corrosion-resistant component according to any of paragraphs [0008]-[0010], wherein the corrosion-resistant non-porous layer is adhered to the ceramic insulating substrate, and the corrosion-resistant non-porous layer has: a porosity of at most 1%; an adhesion strength of at least 20 MPa; and, a thickness of at least 50 ⁇ m.
  • the corrosion-resistant component according to any of paragraphs [0008]-[0011], wherein the corrosion-resistant non-porous layer has: a porosity of at most 0.5%; an adhesion strength of at least 30 MPa; a thickness of at least 100 ⁇ m; and, an average grain size of at least about 300 nm and at most about 30 ⁇ m.
  • the corrosion-resistant component according to any of paragraphs [0008]-[0014], wherein the corrosion-resistant component is a lid configured for releasable engagement with a plasma etch reactor and has a loss tangent of less than 1 ⁇ 10 ⁇ 4 .
  • the corrosion-resistant component according to any of paragraphs [0008]-[0015], further comprising at least one interposing layer embedded in the ceramic insulating substrate, or layered between the ceramic insulating substrate and the corrosion-resistant non-porous layer.
  • the corrosion-resistant component according to any of paragraphs [0008]-[0016], wherein the at least one interposing layer is selected from the group consisting of rare earth oxides, rare earth silicates, rare earth aluminates, and mixtures of two or more thereof.
  • the corrosion-resistant component according to any of paragraphs [0008]-[0020], wherein the at least one interposing layer is adhered to both the corrosion-resistant non-porous layer and to the ceramic insulating substrate, and the corrosion-resistant non-porous layer has: a porosity of at most 1%; an adhesion strength of at least 20 MPa; and, a thickness of at least 50 ⁇ m.
  • Embodiments of the present disclosure also include a green laminate configured for use with a semiconductor processing reactor, the green laminate comprising: a first layer of green sinterable material selected from the group consisting of aluminum oxide, aluminum nitride, silicon nitride, silicate-based materials, and mixtures of two or more thereof; a second layer of green sinterable material selected from the group consisting of yttrium oxide (Y 2 O 3 ), yttrium silicates, yttrium fluorides, yttrium oxyfluorides, yttrium aluminates, nitrides, complex nitride compounds, and combinations of two or more thereof; and, wherein upon heat treatment of the green laminate, the second layer has a porosity of at most 1% and an average grain size of at least about 100 nm and at most about 100 ⁇ m.
  • Y 2 O 3 yttrium oxide
  • yttrium silicates yttrium fluorides
  • the second layer has a porosity of at most 0.5% and an average grain size of at least about 300 nm and at most about 30 ⁇ m.
  • Embodiments of the present disclosure also include an assembly configured for use in fabricating semiconductor chips, the assembly comprising: a reactor; and, a corrosion-resistant component including: a ceramic insulating substrate; and, a corrosion-resistant non-porous layer associated with the ceramic insulating substrate, the corrosion-resistant non-porous layer of a composition comprising at least 15% by weight of a rare earth compound based on total weight of the corrosion-resistant non-porous layer and is characterized by a microstructure substantially devoid of microcracks and fissures, and having: a thickness of at least 50 ⁇ m; a porosity of at most 1%; and, an average grain size of at least 100 nm and at most 100 ⁇ m.
  • the ceramic insulating substrate is selected from the group consisting of aluminum oxide, aluminum nitride, silicon nitride, silicate-based materials and mixtures of two or more thereof.
  • the rare earth compound is selected from the group consisting of yttrium oxide (Y 2 O 3 ), yttrium silicates, yttrium fluorides, yttrium oxyfluorides, yttrium aluminates, nitrides, complex nitride compounds, and combinations of two or more thereof.
  • the corrosion-resistant non-porous layer has: a thickness of at least 100 ⁇ m; a porosity of at most 0.5%; an adhesion strength of at least 30 MPa; and, an average grain size of at least about 300 nm and at most about 30 ⁇ m.
  • the at least one interposing layer is selected from the group consisting of rare earth oxides, rare earth silicates, rare earth aluminates, and mixtures of two or more thereof.
  • the at least one interposing layer is selected from the group consisting of ytterbium oxide (Yb 2 O 3 ), molybdenum (Mo), tungsten (W), molybdenum disilicide (MoSi 2 ), tungsten carbide (WC), tungsten disilicide (WSi 2 ), and mixtures of two or more thereof.
  • the reactor is a plasma etch reactor configured for plasma etching and the corrosion-resistant component is a lid configured for releasable engagement with the plasma etch reactor; and, wherein the lid has a loss tangent of less than 1 ⁇ 10 ⁇ 4 .
  • the reactor is a deposition reactor configured for in-situ cleaning with halogen gases and the corrosion-resistant component is a heater.
  • the reactor is a deposition reactor configured for in-situ cleaning with halogen gases and the corrosion-resistant component is a showerhead.
  • the substrate further includes at least one interposing conductive layer embedded therein, the conductive layer having a sheet resistivity of at most 10 Megaohm-cm and a coefficient thermal expansion difference of at most 4 ⁇ 10 ⁇ 6 /K relative to the coefficients of thermal expansion for the ceramic insulating substrate and the corrosion-resistant non-porous layer.
  • Embodiments of the present disclosure also include a corrosion-resistant component configured for use with a semiconductor processing reactor, the corrosion-resistant component comprising: a) a ceramic insulating substrate; and, b) a corrosion-resistant non-porous layer associated with the ceramic insulating substrate, the corrosion-resistant non-porous layer having a composition comprising at least 15% by weight of a rare earth compound based on total weight of the corrosion-resistant non-porous layer; and, the corrosion-resistant non-porous layer characterized by a microstructure devoid of microcracks and fissures, and having an average grain size of at least 100 nm and at most 100 ⁇ m.
  • the ceramic insulating substrate is selected from the group consisting of aluminum oxide, aluminum nitride, silicon nitride, silicate-based materials and mixtures of two or more thereof.
  • the corrosion-resistant component according to either paragraph [0041] or [0042], wherein the rare earth compound is selected from the group consisting of yttrium oxide (Y2O3), yttrium silicates, yttrium fluorides, yttrium oxyfluorides, yttrium aluminates, nitrides, complex nitride compounds, and combinations of two or more thereof.
  • Y2O3 yttrium oxide
  • silicates yttrium fluorides
  • yttrium oxyfluorides yttrium aluminates
  • nitrides complex nitride compounds
  • the corrosion-resistant component according to any of paragraphs [0041]-[0043], wherein the corrosion-resistant non-porous layer is adhered to the ceramic insulating substrate, and the corrosion-resistant non-porous layer has: a porosity of at most 1%; an adhesion strength of at least 20 MPa; and, a thickness of at least 50 ⁇ m.
  • the corrosion-resistant component according to any of paragraphs [0041]-[0044], wherein the corrosion-resistant non-porous layer has: a porosity of at most 0.5%; an adhesion strength of at least 30 MPa; a thickness of at least 100 ⁇ m; and, an average grain size of at least 300 nm and at most 30 ⁇ m.
  • the corrosion-resistant component according to any of paragraphs [0041]-[0047], wherein the corrosion-resistant component is a lid configured for releasable engagement with a plasma etch reactor and has a loss tangent of less than 1 ⁇ 10 ⁇ 4 .
  • the corrosion-resistant component according to any of paragraphs [0041]-[0053], wherein the at least one interposing layer is adhered to both the corrosion-resistant non-porous layer and to the ceramic insulating substrate, and the corrosion-resistant non-porous layer has: a porosity of at most 1%; an adhesion strength of at least 20 MPa; and, a thickness of at least 50 ⁇ m.
  • Embodiments of the present disclosure also include a green laminate configured for use with a semiconductor processing reactor, the green laminate comprising: a first layer of green sinterable material selected from the group consisting of aluminum oxide, aluminum nitride, silicon nitride, silicate-based materials, and mixtures of two or more thereof; a second layer of green sinterable material selected from the group consisting of yttrium oxide (Y 2 O 3 ), yttrium silicates, yttrium fluorides, yttrium oxyfluorides, yttrium aluminates, nitrides, complex nitride compounds, and combinations of two or more thereof; and, wherein upon heat treatment of the green laminate, the second layer has a porosity of at most 1% and an average grain size of at least 100 nm and at most 100 ⁇ m.
  • Y 2 O 3 yttrium oxide
  • yttrium silicates yttrium fluorides
  • the second layer has a porosity of at most 0.5% and an average grain size of at least 300 nm and at most 30 ⁇ m.
  • Embodiments of the present disclosure also include an assembly configured for use in fabricating semiconductor chips, the assembly comprising: a reactor; and, a corrosion-resistant component including: a ceramic insulating substrate; and, a corrosion-resistant non-porous layer associated with the ceramic insulating substrate, the corrosion-resistant non-porous layer of a composition comprising at least 15% by weight of a rare earth compound based on total weight of the corrosion-resistant non-porous layer and is characterized by a microstructure devoid of microcracks and fissures, and having: a thickness of at least 50 ⁇ m; a porosity of at most 1%; and, an average grain size of at least 100 nm and at most 100 ⁇ m.
  • the ceramic insulating substrate is selected from the group consisting of aluminum oxide, aluminum nitride, silicon nitride, silicate-based materials and mixtures of two or more thereof.
  • the rare earth compound is selected from the group consisting of yttrium oxide (Y 2 O 3 ), yttrium silicates, yttrium fluorides, yttrium oxyfluorides, yttrium aluminates, nitrides, complex nitride compounds, and combinations of two or more thereof.
  • the corrosion-resistant non-porous layer has: a thickness of at least 100 ⁇ m; a porosity of at most 0.5%; an adhesion strength of at least 30 MPa; and, an average grain size of at least 300 nm and at most 30 ⁇ m.
  • the at least one interposing layer is selected from the group consisting of rare earth oxides, rare earth silicates, rare earth aluminates, and mixtures of two or more thereof.
  • the at least one interposing layer is selected from the group consisting of ytterbium oxide (Yb 2 O 3 ), molybdenum (Mo), tungsten (W), molybdenum disilicide (MoSi 2 ), tungsten carbide (WC), tungsten disilicide (WSi 2 ), and mixtures of two or more thereof.
  • the reactor is a plasma etch reactor configured for plasma etching and the corrosion-resistant component is a lid configured for releasable engagement with the plasma etch reactor; and, wherein the lid has a loss tangent of less than 1 ⁇ 10 ⁇ 4 .
  • the reactor is a deposition reactor configured for in-situ cleaning with halogen gases and the corrosion-resistant component is a heater.
  • the reactor is a deposition reactor configured for in-situ cleaning with halogen gases and the corrosion-resistant component is a showerhead.
  • the substrate further includes at least one interposing conductive layer embedded therein, the conductive layer having a sheet resistivity of at most 10 Megaohm-cm and a coefficient thermal expansion difference of at most 4 ⁇ 10 ⁇ 6 /K relative to the coefficients of thermal expansion for the ceramic insulating substrate and the corrosion-resistant non-porous layer.
  • Embodiments of the present disclosure include a method for preparing a corrosion-resistant component for use with a semiconductor processing reactor, comprising: laying up a thinner layer of a sinterable powder composition comprising at least 15% by weight based on total weight of the thinner layer of a rare earth compound, and a thicker layer of sinterable substrate material to form a pre-laminate; and, heat treating the pre-laminate to form a corrosion-resistant component including a corrosion-resistant non-porous outermost layer characterized by a microstructure devoid of microcracks and fissures, and having an average grain size of at least 100 nm and at most 100 ⁇ m.
  • heat treating is selected from the group consisting of hot pressing and hot isostatic pressing.
  • the sinterable substrate material is selected from the group consisting of aluminum oxide, aluminum nitride, silicate-based materials, and mixtures of two or more thereof.
  • the rare earth compound is selected from the group consisting of yttrium oxide (Y 2 O 3 ), yttrium silicates, yttrium fluorides, yttrium oxyfluorides, yttrium aluminates, nitrides, complex nitride compounds and combinations of two or more thereof.
  • the sinterable substrate material is aluminum nitride and the rare earth compound is a rare earth silicate.
  • the at least one additional sinterable powder composition comprises a compound or metal having a coefficient thermal expansion difference of at most 4 ⁇ 10 ⁇ 6 /K relative to the coefficients of thermal expansion for the ceramic insulating substrate and the corrosion-resistant non-porous outermost layer.
  • the at least one additional sinterable powder composition comprises a compound or metal selected from the group consisting of ytterbium oxide (Yb 2 O 3 ), molybdenum (Mo), tungsten (W), niobium (Nb), molybdenum disilicide (MoSi 2 ), tungsten carbide (WC), tungsten disilicide (WSi 2 ), titanium carbide (TiC), titanium nitride (TiN), and mixtures of two or more thereof.
  • Yb 2 O 3 ytterbium oxide
  • Mo molybdenum
  • Mo tungsten
  • Nb niobium
  • MoSi 2 molybdenum disilicide
  • WC tungsten carbide
  • TiC titanium carbide
  • TiN titanium nitride
  • the at least one additional sinterable powder composition further comprises an insulating material selected from the group consisting of alumina, aluminum nitride, aluminates, silicates and mixtures of two or more thereof.
  • the at least one additional sinterable powder composition further comprises insulating materials.
  • the semiconductor processing reactor is a deposition reactor configured for in-situ cleaning with halogen gases and the corrosion-resistant component is a heater.
  • the semiconductor processing reactor is a deposition reactor configured for in-situ cleaning with halogen gases and the corrosion-resistant component is a showerhead.
  • the sinterable substrate material further includes at least one interposing conductive layer embedded therein, the conductive layer having a sheet resistivity of at most 10 Megaohm-cm and a coefficient thermal expansion difference of at most 4 ⁇ 10 ⁇ 6 /K relative to the coefficients of thermal expansion for the ceramic insulating substrate and the corrosion-resistant non-porous outermost layer.
  • FIG. 1A illustrates a cross-sectional view of an embodiment, such as a lid, including a corrosion-resistant component according to an example aspect of the invention
  • FIG. 1B illustrates a cross-sectional view of an embodiment, such as a lid, including a corrosion-resistant component according to another example aspect of the invention
  • FIG. 2 illustrates an assembly for plasma etching of semiconductor chips, including a corrosion-resistant lid according to an example aspect of the invention
  • FIG. 3 illustrates a cross-sectional view of a corrosion-resistant wafer heater according to an example aspect of the invention.
  • FIG. 4 illustrates a chemical vapor deposition reactor assembly including a wafer heater and a showerhead, each including a corrosion-resistant non-porous layer, according to an example aspect of the invention.
  • a ceramic substrate and a corrosion-resistant layer comprising a rare earth compound are sintered together to form a dense corrosion-resistant laminate or corrosion-resistant component. This is to solve the problem of coatings (via plasma spray coating operation, for example) being applied to previously sintered substrates, wherein the coating subsequently suffers from problems such as spalling or shedding particles during use.
  • the heat treating of a thin rare earth compound layer on a suitable substrate material provides a corrosion-resistant component.
  • the rare earth compound is yttrium oxide and the substrate material is a ceramic, such as aluminum oxide.
  • the rare earth compound comprises a rare earth silicate such as yttrium silicate on an aluminum nitride substrate.
  • a corrosion-resistant layer including a rare earth compound is co-sintered with insulating substrate materials to form corrosion-resistant ceramic lids, for example, that are commonly interposed between induction coils and induction plasma used for etching.
  • corrosion-resistant components useful as insulating rings surrounding the wafer chuck and other chamber parts in etch and deposition reactors, such as wafer heaters and deposition showerheads also benefit from this technology.
  • Components, assemblies and methods of the present disclosure provide a way to meet the need for physically and chemically stable, corrosion-resistant layers and parts such as ceramic lids integral to the plasma reactors used in the semiconductor industry.
  • Al 2 O 3 aluminum oxide
  • Yttria is commonly understood to be yttrium oxide, substantially comprising Y 2 O 3
  • Ytterbia is commonly understood to be ytterbium oxide, substantially comprising Yb 2 O 3 .
  • the term “substantially” generally refers a purity of 90 wt %, preferably 91 wt % or 92 wt % or 93 wt % or 94 wt % or 95 wt % or 96 wt % or 97 wt % or 98 wt % or 99 wt % or about 100 wt %.
  • the term “about” generally refers to plus or minus 10% of the indicated number. For example, “about 10%” may indicate a range of 9% to 11%, and “about 20” may mean from 18-22. Other meanings of “about” may be apparent from the context, such as rounding off, so, for example “about 1” may also mean from 0.5 to 1.4.
  • the term “soak” (see Tables in the Examples) refers to the holding time at a particular temperature or pressure in a hot pressing cycle.
  • “Adhesion strength” is measured by the ASTM C633 method.
  • “Loss tangent” is the ratio of the imaginary part of the dielectric constant to the real part; it is directly proportional to the power absorbed by the component.
  • “Color” is described using the 1976 CIELAB color space: this reduces colors to a lightness/darkness variable L*, for which absolute black is 0 and complete white is 100, and other parameters a* and b* which describe the hue of the object.
  • “Porosity” is measured by image analysis of a polished section, polished according to the following scheme (polishing supplies provided by Struers, Inc.): (i) 60 ⁇ m diamond: as needed to flatten the surface; (ii) 15 ⁇ m diamond, fixed abrasive pad: 2 min; (iii) 9 ⁇ m diamond, Largo (plastic) pad: 8 min; (iv) 3 ⁇ m diamond, DAC (nylon) pad: 6 min; and, (v) 1 ⁇ m diamond, napped cloth: 3 min. “Grain size” is measured by the by ASTM-E112 method.
  • “Green” or “unsintered” ceramics as referred to herein include ceramic materials or powders which have not been densified via a high temperature thermal process.
  • “Sintered” or “Cosintered” refers to one or more ceramic materials that have been exposed to a high temperature thermal process to promote sintering.
  • “Sintering” is a thermal or heat treatment process to promote material transport and densification through the gradual elimination of porosity. The sintering process is used to produce materials with controlled microstructure and porosity.
  • “Coating” is a layer applied to a substrate, for example, a sintered substrate.
  • “Laminate” or “composite laminate” is an assembly of layers that are joined via a process such as sintering, for example.
  • “Component” is a part or product.
  • a reactor for semiconductor fabrication or semiconductor processing is useful for etching or deposition or both.
  • a reactor is referred to interchangeably herein as a semiconductor processing reactor, a semiconductor fabrication reactor, or simply as reactor.
  • Reactors are useful for plasma etching or deposition or both.
  • both the ceramic insulating substrate and the corrosion-resistant non-porous layer are resistant to a plasma etching treatment employed in semiconductor processing.
  • the corrosion-resistant component is a lid for a plasma etch reactor.
  • Reactors used for deposition periodically run an etching process for cleaning of the reactor.
  • the reactor is a deposition reactor configured for in-situ cleaning with halogen gases and the corrosion-resistant component is a heater.
  • the reactor is a deposition reactor configured for in-situ cleaning with halogen gases and the corrosion-resistant component is a showerhead.
  • Ceramics are inorganic, non-metallic materials known for their ability to withstand high temperatures. Ceramics include oxides, non-oxides and composites (combinations of oxides and non-oxides). Oxides include, in non-limiting examples, alumina, glass-ceramics, beryllia, mullite, ceria, and zirconia. In a preferred embodiment the ceramic oxide is alumina (Al 2 O 3 ). Non-oxides include carbides, borides, nitrides, and silicides. In another preferred embodiment, the non-oxide is a nitride, such as aluminum nitride (AlN). Ceramic oxides, non-oxides, and composites are useful as substrates.
  • Oxides include, in non-limiting examples, alumina, glass-ceramics, beryllia, mullite, ceria, and zirconia. In a preferred embodiment the ceramic oxide is alumina (Al 2 O 3 ). Non-oxide
  • a corrosion-resistant layer including a rare-earth element or compound is advantageously joined with a ceramic substrate and/or other layers to provide a laminate, wherein the outermost layer is corrosion-resistant and non-porous.
  • rare-earth compounds include, but are not limited to trivalent rare earth oxides such as in an example embodiment, yttrium oxide (Y 2 O 3 ).
  • the rare earth compound is selected from the group consisting of yttrium oxide, yttrium silicates, yttrium fluorides, yttrium oxyfluorides, yttrium aluminates, nitrides, complex nitride compounds, and combinations of two or more thereof.
  • the rare earth compound is Y 3 Si 3 O 10 F.
  • the rare earth compound is a complex nitride compound such as YN.Si 3 N 4 or YN.AlN.Y 2 O 3 .2SiO 2 , for example.
  • Sintering aids are useful for example to minimize porosity, reduce grain size, and/or to enable less extreme processing conditions to be employed (for example, lower pressures in hot pressing) for sintering.
  • a sintering aid is added to the rare-earth compound.
  • the sintering aid added to the rare-earth compound is an oxide of tetravalent elements (e.g. Zr, Hf, Ce).
  • the amount of sintering aid added to the rare-earth compound is in the range from about 300 ppm to about 20% by weight based upon total weight of the rare-earth compound; in another example aspect from about 0.5% by weight to about 15% by weight based upon total weight of the rare-earth compound. In an example aspect, the amount of sintering aid added to the rare-earth compound is about 1% by weight, or about 2% by weight, or about 5% by weight, or about 10% by weight, or about 15% by weight. In an example aspect, the sintering aid added to the rare-earth compound is ZrO 2 or HfO 2 .
  • the rare-earth compound is yttria
  • ZrO 2 is used as a sintering aid in the amount of about 1% by weight based upon total weight of the rare-earth compound.
  • ZrO 2 is used as a sintering aid in the amount of about 15% by weight based upon total weight of the rare-earth compound.
  • about 1% by weight sintering aid is added to the rare-earth compound based upon total weight of the rare-earth compound.
  • Interposer layers can be placed between the substrate and the rare-earth compound containing corrosion-resistant layer in assembling the laminate.
  • at least one interposer layer between a yttria layer and an alumina substrate is useful in order to detect wear of the outermost corrosion-resistant layer.
  • Interposer layers may also advantageously include a rare-earth element or compound.
  • ytterbium oxide (Yb 2 O 3 ) is used as an interposer layer since its fluorescence at infrared (IR) wavelengths can be used to detect corrosion-resistant layer wear without producing a cosmetic color change of the material.
  • interposer layer(s) depends on function; typically interposer layers are at most about 2 mm in thickness.
  • interposer layers such as conductive layers or bonding layers function acceptably at thicknesses of less than 10 ⁇ m.
  • ceramic lids which are also referred to as ceramic windows or simply as lids or windows interchangeably herein, are commonly interposed between induction coils and induction plasma used for etching.
  • the electrical resistance of a metal layer could also serve to monitor the temperature of the lid, thus enabling feedback control over its temperature. Embedding or interposing the layers within the lid or component simplifies the assembly of the system and also improves shielding and the coupling of the heat to the lid.
  • the materials of the embedded layers can be considered close or acceptable if the difference in thermal expansion coefficients is at most 4 ⁇ 10 ⁇ 6 /K relative to the coefficients for the ceramic insulating substrate and the corrosion-resistant non-porous layer.
  • the at least one interposing layer is chosen to be a material having a thermal expansion coefficient difference of at most at most 4 ⁇ 10 ⁇ 6 /K relative to the coefficients for the ceramic insulating substrate and the corrosion-resistant non-porous layer.
  • Thermal expansion mismatches can often be helped by making the layer a composite of several different materials, whose combined thermal expansion matches the expansion of the bulk of the part.
  • MoSi 2 is a particularly suitable conductive metal, because its thermal expansion is close to that of alumina, and it does not react with alumina at the high processing temperatures.
  • the corrosion-resistant component has a loss tangent of the component of at most 1 ⁇ 10 ⁇ 3 , preferably at most 1 ⁇ 10 ⁇ 4 .
  • a component having a loss tangent of at most 1 ⁇ 10 ⁇ 4 is substantially transparent to radio-frequency (RF) energy.
  • RF radio-frequency
  • Excessive carbon content in the parts tends to promote high loss tangent and therefore carbon content should be minimized. Free carbon contents in excess of 2000 ppm are undesirable.
  • the carbon content is at most 1500 ppm.
  • the carbon content is at most 1000 ppm.
  • the carbon content is at most 500 ppm.
  • the carbon content is at most 100 ppm.
  • the corrosion-resistant component has a CIE Lab color L* parameter of at least 50. In another example aspect, the corrosion-resistant component has a CIE Lab color L* parameter of at least 80.
  • First row transition elements such as V, Cr, Mn, Fe, Co, Ni, Cu, and Zn, for example, diffuse relatively quickly through silicon and can alter the electrical properties of devices.
  • the presence of Au and Ag can cause similar problems.
  • elements such as Li, Na, and K diffuse quickly through silica and can affect the charge density on device gates.
  • the corrosion-resistant component of the invention is substantially contaminant free. Total concentration of undesirable elements in the raw materials for making corrosion-resistant components is to be minimized. The total concentration of these undesirable elements should be substantially less than 1 at %. In an example aspect, the total concentration of undesirable elements in raw materials used in making of the corrosion-resistant components is at most 1 at %.
  • Layer thickness for the outermost layer may be tailored to the component and its application for use.
  • the outermost layer is the corrosion-resistant non-porous layer.
  • the outermost layer may be oriented toward the inside of a chamber or reactor, for example.
  • lids or windows which are typically larger than 500 mm in diameter, relatively thick layers are desired.
  • the as-fired profile of such a large component may depart by a millimeter or more from the desired profile; therefore, it is desirable for the as-fired thickness of the outermost layer to be substantially more than one millimeter thick, in order to ensure the presence of enough outermost material even after grinding. Thinner layers are more appropriately used on smaller parts, because departures from the true form are typically less.
  • One example aspect of the invention is directed to a corrosion-resistant component configured for use with a semiconductor processing reactor, the corrosion-resistant component comprising: a) a ceramic insulating substrate; and, b) a corrosion-resistant non-porous layer associated with the ceramic insulating substrate, the corrosion-resistant non-porous layer having a composition comprising at least 15% by weight of a rare earth compound based on total weight of the corrosion-resistant non-porous layer; and, the corrosion-resistant non-porous layer characterized by a microstructure substantially devoid of microcracks and fissures, and having an average grain size of at least about 100 nm and at most about 100 ⁇ m.
  • the corrosion-resistant non-porous layer associated with the ceramic insulating substrate is adhered to the substrate.
  • the corrosion-resistant non-porous layer is adhered directly to the substrate.
  • the corrosion-resistant non-porous layer is adhered indirectly to the substrate, for example with interposing layers therebetween.
  • the microstructure of the corrosion-resistant non-porous layer is important to the durability and performance of the component.
  • a component or laminate including a non-porous layer free of microcracks and fissures does not suffer deleterious effects such as particle shedding.
  • the corrosion-resistant non-porous layer is characterized by a microstructure devoid of microcracks and fissures.
  • the corrosion-resistant non-porous layer is characterized by a microstructure substantially devoid of microcracks and fissures.
  • the corrosion-resistant non-porous layer has microcracks and fissures of less than 50 per mm 2 , in an example aspect less than 10 per mm 2 , in another example aspect less than 5 per mm 2 , and in yet another example aspect less than 1 per mm 2 .
  • the corrosion-resistant non-porous layer is characterized by a microstructure having microcracks and fissures of at most 1 per mm 2 , as quantified by image analysis, for example, or other methods as known in the art. Whereas microcracks and fissures are deleterious to the microstructural integrity of the corrosion-resistant non-porous layer, second phases in the microstructure may conversely increase strength of the layer (refer to Example 10).
  • grain size of the corrosion-resistant non-porous layer is important to the performance of the component. Generally, corrosion occurs fastest at grain boundaries, thus materials with larger grain sizes corrode more slowly. In addition, if corrosion on boundaries is relatively rapid, entire grains can be dislodged by grain boundary corrosion. This is also referred to herein as particle loss or shedding.
  • the corrosion-resistant component includes a corrosion-resistant non-porous layer having an average grain size as measured by ASTM-E112 of at least 100 nm.
  • the corrosion-resistant non-porous layer is characterized as having an average grain size of at least 100 nm, or at least 150 nm, or at least 200 nm, or at least 300 nm, or at least 500 nm.
  • problems may develop with overly large grain sizes, for example, the size of flaws weakening the material scales as the grain size; therefore, grain sizes larger than 100 ⁇ m are also undesirable.
  • the corrosion-resistant non-porous layer is characterized as having an average grain size of at most 100 ⁇ m, or at most 30 ⁇ m, or at most 10 ⁇ m, or at most 1 ⁇ m, or at most 750 nm.
  • the average grain size of the corrosion-resistant non-porous layer is in the range of about 100 nm to about 100 ⁇ m, preferably about 200 nm to about 50 ⁇ m, more preferably about 300 nm to about 30 ⁇ m. In another example aspect, the average grain size of the corrosion-resistant non-porous layer is at least 300 nm and at most 30 ⁇ m.
  • the corrosion-resistant component includes a corrosion-resistant non-porous layer having: a) a porosity of ⁇ 2%, preferably ⁇ 1% or ⁇ 0.9% or ⁇ 0.8% or ⁇ 0.7% or ⁇ 0.6% or ⁇ 0.5% or ⁇ 0.4% or ⁇ 0.3% or ⁇ 0.2% or ⁇ 0.1%; and b) an adhesion strength of ⁇ 15 MPa, preferably ⁇ 20 MPa or ⁇ 25 MPa or ⁇ 30 MPa or ⁇ 35 MPa or ⁇ 40 MPa; and c) a layer thickness of ⁇ 50 ⁇ m, preferably ⁇ 100 ⁇ m or ⁇ 150 ⁇ m or ⁇ 200 ⁇ m or ⁇ 250 ⁇ m or ⁇ 300 ⁇ m.
  • Layer thickness may be tailored to the application of use or component specifications desired. Alternatively, the layer thickness can be in the range of about 50 to about 500 ⁇ m, preferably about 100 to about 400 ⁇ m, more preferably about 150 to about 300 ⁇ m.
  • the corrosion-resistant non-porous layer has: a porosity of at most 1%; an adhesion strength of at least 20 MPa; and, a layer thickness of at least 50 ⁇ m.
  • the corrosion-resistant non-porous layer has: a porosity of at most 0.5%; an adhesion strength of at least 30 MPa; and, a layer thickness of at least 100 ⁇ m.
  • FIGS. 1A and 1B illustrate cross-sectional schematic views of example aspects of corrosion-resistant components.
  • corrosion-resistant component 100 includes substrate 110 having corrosion-resistant non-porous layer 120 adjacent to the substrate 110 where layer 120 provides an outermost layer for the component. Layer 120 has thickness t 1 .
  • corrosion-resistant component 150 includes substrate 110 having interposing layer 130 situated between substrate 110 and corrosion-resistant non-porous layer 120 . Layer 130 has thickness t 2 .
  • both the substrate and the corrosion-resistant non-porous layer are resistant to the plasma etching conditions employed in semiconductor processing.
  • corrosion-resistant component 100 includes non-porous corrosion-resistant layer 120 comprising a rare earth compound.
  • layer 120 comprises a trivalent rare earth oxide.
  • the rare earth compound is selected from the group consisting of yttrium oxide (Y 2 O 3 ), yttrium silicates, yttrium fluorides, yttrium oxyfluorides, yttrium aluminates, nitrides, complex nitride compounds, and combinations of two or more thereof.
  • the rare earth compound is a complex nitride compound such as, for example, YN.Si 3 N 4 or YN.AlN.Y 2 O 3 .2SiO 2 .
  • the corrosion-resistant component includes ceramic insulating substrate 110 , as shown also in FIG. 1A , selected from the group consisting of aluminum oxide (“alumina”, also Al 2 O 3 ), aluminum nitride, silicon nitride, silicate-based materials and mixtures of two or more thereof.
  • the substrate may further include zirconia (ZrO 2 ).
  • the ceramic insulating substrate is aluminum oxide.
  • the ceramic insulating substrate consists essentially of aluminum oxide.
  • the ceramic insulating substrate is aluminum oxide and the rare earth compound is a trivalent rare earth oxide.
  • the ceramic insulating substrate is aluminum nitride and the corrosion-resistant non-porous layer is a rare earth silicate.
  • the corrosion-resistant non-porous layer is adhered to the ceramic insulating substrate, and the corrosion-resistant non-porous layer has: a porosity of at most 1%; an adhesion strength of at least 20 MPa; and, a thickness of at least 50 ⁇ m.
  • the corrosion-resistant non-porous layer is adhered to the ceramic insulating substrate, and the corrosion-resistant non-porous layer has: a porosity of at most 0.5%; an adhesion strength of at least 30 MPa; a thickness of at least 100 ⁇ m; and, an average grain size of at least about 300 nm and at most about 30 ⁇ m.
  • corrosion-resistant component 100 is a lid configured for releasable engagement with a plasma etch reactor.
  • the corrosion-resistant component or lid has a loss tangent of less than 1 ⁇ 10 ⁇ 4 .
  • ceramic insulating substrate 110 and corrosion-resistant non-porous layer 120 are substantially transparent to radio-frequency (RF) energy.
  • RF radio-frequency
  • corrosion-resistant component 150 includes at least one interposing layer 130 selected from the group consisting of rare earth oxides, rare earth silicates, rare earth aluminates, and mixtures of two or more thereof.
  • the at least one interposing layer 130 is ytterbium oxide (Yb 2 O 3 ).
  • the at least one interposing layer comprises conducting materials.
  • the at least one interposing layer further comprises insulating materials.
  • the at least one interposing layer is adhered to both the corrosion-resistant non-porous layer and to the ceramic insulating substrate, and the corrosion-resistant non-porous layer has: a porosity of at most 1%; an adhesion strength of at least 20 MPa; and, a thickness of at least 50 ⁇ m.
  • the at least one interposing layer is adhered to both the corrosion-resistant non-porous layer and to the ceramic insulating substrate, and the corrosion-resistant non-porous layer has: a porosity of at most 0.5%; an adhesion strength of at least 30 MPa; a thickness of at least 100 ⁇ m; and, an average grain size of at least about 300 nm and at most about 30 ⁇ m.
  • At least one interposing layer is either embedded in the ceramic insulating substrate 110 (see FIG. 3 , layers 340 , 360 ), or between and adhered to both the substrate and the corrosion-resistant non-porous layer 120 (see FIG. 1B ).
  • the interposing layer is selected from the group consisting of rare earth oxides, rare earth silicates, rare earth aluminates and mixtures of two or more thereof.
  • a rare earth oxide suitable as an at least one interposing layer is ytterbium oxide (Yb 2 O 3 ).
  • the interposing layer comprises conducting materials, which can optionally further comprise insulating materials.
  • Conducting metal layers are useful as actively driven electrodes or as a passive RF shield.
  • the insulating materials are generally selected from the group consisting of alumina, aluminum nitride, silicon nitride, aluminates, silicates, and mixtures of two or more thereof, although any material compatible with the processing of the part and the metals in the layer could be also used; the reasons to add materials to the conducting layer can include obtaining better thermal expansion match to the rest of the part and improving the adhesion between the layer and the rest of the part.
  • the layer will usually have large openings in it to allow RF energy to pass through.
  • an interposing layer such as a conductive layer is non-continuous.
  • the substrate and the corrosion-resistant non-porous layer are substantially transparent to radio-frequency (RF) energy.
  • a green laminate configured for use with a semiconductor processing reactor comprises a first layer of green sinterable material and a second layer of green sinterable material including a rare earth compound.
  • the first layer of green sinterable material is selected from the group consisting of aluminum oxide, aluminum nitride, silicon nitride, silicate-based materials, and mixtures of two or more thereof.
  • the second layer of green sinterable material comprises a trivalent rare earth oxide.
  • the second layer comprises a rare earth compound selected from the group consisting of yttrium oxide (Y 2 O 3 ), yttrium silicates, yttrium fluorides, yttrium oxyfluorides, yttrium aluminates, nitrides, complex nitride compounds, and combinations of two or more thereof.
  • the second layer upon heat treatment of the laminate, has a porosity of at most 1% and an average grain size of at least 100 nm and at most 100 ⁇ m.
  • the second layer upon heat treatment of the laminate, has a porosity of at most 0.5%.
  • the average grain size of the second layer is at least 300 nm and at most 30 ⁇ m.
  • the green laminate further includes at least one interposing layer between the first and second layers, wherein the interposing layer comprises green sinterable material selected from the group consisting of rare earth oxides, rare earth silicates, rare earth aluminates, and mixtures of two or more thereof.
  • the green laminate further includes at least one interposing layer wherein the at least one interposing layer comprises conducting materials.
  • the green laminate further includes at least one interposing layer wherein the at least one interposing layer comprises insulating materials.
  • the heat treatment for the green laminate is selected from the group consisting of hot pressing and hot isostatic pressing.
  • the heat treated or sintered laminate including interposing layer(s) has an adhesion strength of at least 15 MPa, or at least 20 MPa, or at least 25 MPa, or at least 30 MPa, or at least 35 MPa, or at least 40 MPa.
  • FIG. 2 illustrates an example aspect of an assembly configured for use in plasma etching semiconductor wafers.
  • Plasma etch reactor assembly 200 includes plasma etch reactor 250 . Alternating magnetic fields generated by induction coils 240 extend through lid 225 , creating electric fields inside reactor 250 directly under lid 225 , which in turn create the etch plasma.
  • Corrosion-resistant lid 225 is configured for releasable engagement with plasma etch reactor 250 .
  • Lid 225 includes a corrosion-resistant ceramic insulating substrate 210 having an inner surface and an outer surface; and, further includes corrosion-resistant non-porous layer 220 , which is adjacent to the inner surface of substrate 210 .
  • Corrosion-resistant non-porous layer 220 having inner and outer planar surfaces, is positioned so that the inner planar surface of layer 220 faces the interior of reactor 250 .
  • interposing layer(s) (example layer 130 as shown in FIG. 1B ) are situated between substrate 210 and corrosion-resistant non-porous layer 220 .
  • layer 220 comprising a rare earth compound, wherein the non-porous layer is adhered to the corrosion-resistant substrate and has 1) an adhesion strength of ⁇ 15 MPa, preferably ⁇ 20 MPa or ⁇ 25 MPa or ⁇ 30 MPa or ⁇ 35 MPa or ⁇ 40 MPa, 2) a thickness of ⁇ 50 ⁇ m, preferably ⁇ 100 ⁇ m or ⁇ 150 ⁇ m or ⁇ 200 ⁇ m or ⁇ 250 ⁇ m or ⁇ 300 ⁇ m; alternately a thickness in the range of about 50 to about 500 ⁇ m, preferably about 100 to about 400 ⁇ m, more preferably about 150 to about 300 ⁇ m, and 3) a porosity of preferably ⁇ 1% or ⁇ 0.9% or ⁇ 0.8% or ⁇ 0.7% or ⁇ 0.6% or ⁇ 0.5% or ⁇ 0.4% or ⁇ 0.3% or ⁇ 0.2% or ⁇ 0.1%.
  • layer 220 includes at least 15% by weight based on total weight of layer of a rare earth compound.
  • layer 220 includes an adhesion strength of at least 20 MPa; a porosity of at most 1%; a microstructure substantially devoid of microcracks and fissures and an average grain size of at least 100 nm and at most 100 ⁇ m; and, a layer thickness of at least 50 ⁇ m.
  • the grain size is at least 300 nm and at most 30 ⁇ m.
  • lid 225 of the assembly includes layer 220 , wherein the rare earth compound is selected from the group consisting of yttrium oxide (Y 2 O 3 ), yttrium silicates, yttrium fluorides, yttrium oxyfluorides, yttrium aluminates, nitrides, complex nitride compounds and combinations of two or more thereof.
  • the assembly includes the corrosion-resistant ceramic insulating substrate 210 , wherein the substrate is selected from the group consisting of aluminum oxide, aluminum nitride, silicon nitride, silicate-based materials and mixtures of two or more thereof.
  • the assembly further comprises an interposing layer embedded in the substrate, or an interposing layer between and adhered to both the corrosion-resistant substrate and the non-porous layer.
  • the interposing layer may serve one or more functions, for example, to promote adhesion between the non-porous layer and the substrate, to prevent an adverse reaction between the non-porous layer and the substrate, and/or to provide some electrical function for the assembly.
  • an interposing layer such as ytterbium oxide (Yb 2 O 3 ) can be beneficial.
  • the interposing layer is selected from the group consisting of ytterbium oxide (Yb 2 O 3 ), MoSi 2 , radio-frequency (RF) conducting materials and mixtures of two or more thereof.
  • the corrosion-resistant lid of the assembly is substantially transparent to radio-frequency (RF) energy.
  • the assembly, including the corrosion-resistant lid, is preferably resistant to the plasma etching treatment employed in semiconductor processing.
  • the corrosion-resistant substrate and the corrosion-resistant non-porous layer of corrosion-resistant lid of the assembly are resistant to the plasma etching treatment employed in semiconductor processing.
  • FIG. 3 illustrates a cross-sectional schematic view of wafer heater apparatus 300 as in an example aspect.
  • the wafer (not shown) sits on the outermost layer ( 320 ) of insulating ceramic disk 310 having heating elements 340 embedded therein and also, optionally, metal RF shield 360 .
  • insulating ceramic 310 from which these heaters are made, is aluminum nitride.
  • alumina or silicon nitride are useful as ceramic insulating substrate 310 .
  • the heater is sometimes cleaned with fluorine-containing gas.
  • insulating ceramic 310 includes corrosion-resistant non-porous layer 320 and optional interposing layer 330 therebetween.
  • Corrosion-resistant non-porous layer 320 includes an outer surface for holding the wafer (not shown). Of particular importance is that the region of the rare earth compound containing layer directly under the wafer, in other words corrosion-resistant non-porous layer 320 , be dense. Otherwise particles from the heater would tend to be shed onto the underside of the wafer.
  • shed particles could migrate to the top side of the wafer in a subsequent step, which would in turn result in defects in the patterns on the wafer.
  • the sides, bottom and coverage on the stalk or supporting disk 380 of the wafer heater are less critical, as there is no direct path for particles to migrate to the wafer.
  • a plasma spray coating suffices to prevent against contamination for these other regions.
  • FIG. 4 illustrates a chemical vapor deposition reactor assembly including a wafer heater according to an example aspect of the invention.
  • Chemical vapor deposition (CVD) reactor assembly 400 includes showerhead 410 and heater 440 . Reactive gases flow through showerhead 410 , which is protected by corrosion-resistant non-porous layer 420 , onto wafer 450 , where a deposit is formed. The temperature of the wafer is maintained and kept uniform by heater 440 , which may also have a non-porous corrosion-resistant layer on it (as shown in FIG. 3 ) to protect it during cleaning.
  • showerhead 410 may further include interposing or embedded layers, such as an electrode, within to assist the generation of a plasma to promote chemical reactions.
  • assembly 400 is configured for use in fabricating semiconductor chips.
  • Assembly 400 includes corrosion-resistant components (i) wafer heater 440 , shown in FIG. 3 as wafer heater 300 in more detail), and/or (ii) showerhead 410 .
  • the deposition reactor is configured for in-situ cleaning with halogen gases and a corrosion-resistant component.
  • Each corrosion-resistant component includes a ceramic insulating substrate; and, a corrosion-resistant non-porous layer of a composition comprising at least 15% by weight of a rare earth compound based on total weight of layer.
  • the rare earth compound is a trivalent oxide.
  • the rare earth compound is selected from the group consisting of yttrium oxide (Y 2 O 3 ), yttrium silicates, yttrium fluorides, yttrium oxyfluorides, yttrium aluminates, nitrides, complex nitride compounds and combinations of two or more thereof.
  • the rare earth compound is yttrium oxide (Y 2 O 3 ).
  • the ceramic insulating substrate is selected from the group consisting of aluminum oxide, aluminum nitride, silicon nitride, silicate-based materials, and mixtures of two or more thereof.
  • the corrosion-resistant component further includes at least interposing layer between the substrate and the corrosion-resistant non-porous layer.
  • the interposing layer is selected from the group consisting of ytterbium oxide (Yb 2 O 3 ), MoSi 2 , radio-frequency (RF) conducting materials and mixtures of two or more thereof.
  • the substrate further includes at least one additional interposing conductive layer embedded therein, the conductive layer having a sheet resistivity of at most 10 Megaohm-cm, which may also be written as 10 megohm-cm interchangeably herein.
  • an assembly configured for use in fabricating semiconductor chips, the assembly comprising a reactor and a corrosion-resistant component.
  • the corrosion-resistant component includes a ceramic insulating substrate and a corrosion-resistant non-porous layer associated with the ceramic insulating substrate.
  • the corrosion-resistant non-porous layer has a composition comprising at least 15% by weight of a rare earth compound based on total weight of the corrosion-resistant non-porous layer.
  • the corrosion-resistant non-porous layer is characterized by a microstructure substantially devoid of microcracks and fissures, and having: a thickness of at least 50 ⁇ m; a porosity of at most 1%; and, an average grain size of at least 100 nm and at most 100 ⁇ m.
  • the ceramic insulating substrate of the assembly is selected from the group consisting of aluminum oxide, aluminum nitride, silicon nitride, silicate-based materials and mixtures of two or more thereof.
  • the rare earth compound of the assembly is selected from the group consisting of yttrium oxide (Y 2 O 3 ), yttrium silicates, yttrium fluorides, yttrium oxyfluorides, yttrium aluminates, nitrides, complex nitride compounds, and combinations of two or more thereof.
  • the corrosion-resistant non-porous layer of the assembly is adhered to the ceramic insulating substrate and has an adhesion strength of at least 20 MPa.
  • the corrosion-resistant non-porous layer has a thickness of at least 100 ⁇ m; a porosity of at most 0.5%; an adhesion strength of at least 30 MPa; and, an average grain size of at least about 300 nm and at most about 30 ⁇ m.
  • the assembly further comprises at least one interposing layer embedded in the ceramic insulating substrate, or layered between the ceramic insulating substrate and the corrosion-resistant non-porous layer.
  • the at least one interposing layer is selected from the group consisting of rare earth oxides, rare earth silicates, rare earth aluminates, and mixtures of two or more thereof.
  • the at least one interposing layer is ytterbium oxide (Yb 2 O 3 ).
  • the at least one interposing layer comprises conducting materials that have a good coefficient of thermal expansion match with the ceramic insulating substrate and the corrosion-resistant non-porous layer.
  • the at least one interposing layer is chosen to be a material having a thermal expansion coefficient difference of at most at most 4 ⁇ 10 ⁇ 6 /K relative to the coefficients for the ceramic insulating substrate and the corrosion-resistant non-porous layer.
  • the at least one interposing layer further comprises insulating materials.
  • the at least one interposing layer is selected from the group consisting of ytterbium oxide (Yb 2 O 3 ), molybdenum (Mo), tungsten (W), molybdenum disilicide (MoSi 2 ), tungsten carbide (WC), tungsten disilicide (WSi 2 ), and mixtures of two or more thereof.
  • the reactor is a plasma etch reactor configured for plasma etching and the corrosion-resistant component is a lid configured for releasable engagement with the plasma etch reactor; and, wherein the lid has a loss tangent of less than 1 ⁇ 10 ⁇ 4 and is substantially transparent to radio-frequency (RF) energy.
  • the reactor is a deposition reactor configured for in-situ cleaning with halogen gases and the corrosion-resistant component is a heater.
  • the ceramic insulating substrate further includes at least one interposing conductive layer embedded therein, the conductive layer having a sheet resistivity of at most 10 Megaohm-cm.
  • the reactor is a deposition reactor configured for in-situ cleaning with halogen gases and the corrosion-resistant component is a showerhead.
  • Another aspect is directed to a method for preparing a corrosion-resistant component for use with a reactor.
  • the method includes the steps as follows: a) laying up a thinner layer of a sinterable powder composition comprising at least 15% by weight based on total weight of the thinner layer of a rare earth compound, and a thicker layer of sinterable substrate material to form a pre-laminate (also referred to herein as ‘green laminate’); and, b) heat treating the pre-laminate to form a corrosion-resistant laminate.
  • pre-laminate also referred to herein as ‘green laminate’
  • heat treating is selected from the group consisting of hot pressing and hot isostatic pressing.
  • the sinterable substrate material is selected from the group consisting of aluminum oxide, aluminum nitride, silicon nitride, silicate-based materials, and mixtures of two or more thereof.
  • the rare earth compound is a tri-valent rare earth oxide.
  • the rare earth compound is selected from the group consisting of yttrium oxide (Y 2 O 3 ), yttrium silicates, yttrium fluorides, yttrium oxyfluorides, yttrium aluminates, nitrides, complex nitride compounds and combinations of two or more thereof.
  • the amount of rare earth compound is about 15 to 100 wt %, or about 20 to about 90 wt %, or about 25 to about 80 wt %.
  • the rare earth compound is Y 3 Si 3 O 10 F.
  • the sinterable substrate material is aluminum oxide and the rare earth compound is a trivalent rare earth oxide.
  • the sinterable substrate material is aluminum nitride and the corrosion-resistant non-porous layer is a rare earth silicate.
  • the corrosion-resistant component is a lid configured for releasable engagement with a plasma etch reactor.
  • the lid has a loss tangent of less than 1 ⁇ 10 ⁇ 3 . In another example aspect of the method, the lid has a loss tangent of less than 1 ⁇ 10 ⁇ 4 . In an example aspect of the method, the corrosion-resistant component is substantially transparent to radio-frequency (RF) energy.
  • RF radio-frequency
  • the method further comprises laying up at least one additional sinterable powder composition layer interposed between the rare earth compound thinner layer and the substrate material thicker layer, prior to heat treatment.
  • the at least one additional sinterable powder composition comprises a compound or metal selected from the group consisting of ytterbium oxide (Yb 2 O 3 ), molybdenum (Mo), tungsten (W), niobium (Nb), and compounds like molybdenum disilicide (MoSi 2 ), tungsten carbide (WC), tungsten disilicide (WSi 2 ), titanium carbide (TiC), titanium nitride (TiN), and other such conducting materials and compounds that show metallic behavior and have a good coefficient of thermal expansion match to the ceramic insulating substrate and the corrosion-resistant non-porous layer, and mixtures of two or more thereof.
  • the at least one additional sinterable powder composition is ytterbium oxide (Yb 2 O 3 ).
  • the method includes at least one additional sinterable powder composition comprises conducting materials.
  • the method includes at least one additional sinterable powder composition comprises conducting metals.
  • the method includes the at least one additional sinterable powder composition further comprises insulating materials.
  • the method includes the at least one additional sinterable powder composition further comprises an insulating material selected from the group consisting of alumina, aluminum nitride, silicon nitride, silicates, and mixtures of two or more thereof.
  • the semiconductor processing reactor is a deposition reactor configured for in-situ cleaning with halogen gases and the corrosion-resistant component is a heater.
  • the sinterable substrate material further includes at least one interposing conductive layer embedded therein, the conductive layer having a sheet resistivity of at most 10 Megaohm-cm.
  • the semiconductor processing reactor is a deposition reactor configured for in-situ cleaning with halogen gases and the corrosion-resistant component is a showerhead.
  • a total concentration of undesirable elements in raw materials used is at most 1 at %.
  • Two disks (S 1 and S 12 ) made from an alumina-yttria laminate were manufactured as follows. High purity chemically precipitated yttrium oxide powder from AMR Corp. was attrition milled in water to particle size d90 ⁇ 1 ⁇ m. The slurry was then freeze dried and sieved through a 150 ⁇ m mesh.
  • Spray dried alumina powder of approximate composition 0.25 wt % SiO 2 , 0.05 wt % Na 2 O, 0.12 wt % MgO, 0.12 wt % CaO, balance Al 2 O 3 was heated in air at 800° C. for 8 hours to remove binder from the spray dried powder.
  • This powder is referred to as CoorsTek 99512.
  • the alumina powder was cold pressed in a 6-inch diameter die to a pressure of 440 psi and a total thickness of about 1 inch.
  • a layer of the yttria powder described above was then added on top of the alumina and cold pressed to 440 psi again.
  • the yttria layer was about 2000 ⁇ m thick at this point.
  • the process was repeated except that a layer of ytterbium oxide (Yb 2 O 3 ) powder about 1000 ⁇ m was interposed between the yttria layer and the alumina layer.
  • Yb 2 O 3 ytterbium oxide
  • the cold pressed laminate was transferred to a hot press mold assembly, consisting of the stack arrangement depicted below in Table 1.
  • Gray dense yttria-alumina laminates emerged from the hot press operation.
  • the grain size of the alumina as measured by the ASTM-E112 method was 1.7 ⁇ m.
  • the carbon content was 640 ppm.
  • the loss tangent of Si measured at 5 GHz was 9.1 ⁇ 10 ⁇ 5 .
  • Porosity was measured by image analysis of a polished section, polished according to the following scheme (polishing supplies provided by Struers, Inc.):
  • the porosity of S 1 and S 12 were found to be 0.24% and 0.72% respectively.
  • the corrosion-resistant non-porous yttria layer was observed to substantially have no microcracks or fissures.
  • the ytterbium oxide layer thickness measured from the section was 520 ⁇ m.
  • Adhesion strength as measured by a variant of ASTM C633 was found to be 30 MPa.
  • adhesion strength is the force required to cause failure when tension is applied between the outermost layer and the substrate, irrespective of the presence or absence of interposing layers or of the location of the failure, provided that the failure is not confined exclusively to the substrate.
  • the outermost layer being adhered to the substrate may include instances wherein at least one interposing layer is included and/or a reaction layer inherently resulting from sintering exists between the outermost layer and the substrate.
  • a reaction layer having composition Y 3 Al 5 O 12 between the yttria layer and the alumina substrate was present. Darkness L* of the sample, measured on the yttria side with a Hunterlab MiniScan XE colorimeter using the CIE L*a*b* color scale, was 53.9.
  • the grain sizes of the alumina as measured by the ASTM-E112 method were 0.76 ⁇ m (S 4 ) and 0.92 ⁇ m (S 5 ).
  • the grain size of the yttria measured in the same way was found to be 0.4 ⁇ m.
  • the loss tangent of S 4 at 5 GHz was found to be 11 ⁇ 10 ⁇ 5 , and that of S 5 to be 15.7 ⁇ 10 ⁇ 5 .
  • the porosity of both samples was measured by the method described in Example 1.
  • S 4 had a porosity of 0.50% and S 5 of 0.69%. Substantially no microcracks or fissures were observed in the corrosion-resistant non-porous yttria layer. Adhesion strength as measured by ASTM C633 was found to be 20 MPa for S 4 and 26 MPa for S 5 .
  • a reaction layer between the yttria layer and alumina substrate was present. Darkness L* of the sample, measured on the yttria side with a Hunterlab MiniScan XE colorimeter using the CIE L*a*b* color scale, was 49.7 for S 4 and 66.1 for S 5 .
  • Example 2 Two yttria-alumina laminates were cold pressed as described in Example 2.
  • One laminate (S 6 ) used AHPA alumina powder from Sasol, and the other laminate (S 7 ) used Baikowski TCPLS DBM alumina powder from Baikowski-Malakoff. Each laminate was placed between sheets of Mo foil.
  • the cold-pressed disks were hot pressed with the same stack configuration as in Example 2.
  • the temperature and pressure cycles are shown in Tables 7 and 8.
  • the loss tangent of sample S 6 was measured to be 4 ⁇ 10 ⁇ 5 .
  • L* was found to be 75.4 for S 6 and 75.9 for S 7 .
  • Adhesion strength for S 6 was 24 MPa and 35 MPa for S 7 .
  • the laminate made from the AHPA powder including AlF 3 additions was cracked in several places on removal and a porous interface between the yttria layer and the alumina layer was observed.
  • the loss tangent of this sample (S 8 ) was 2'10 ⁇ 5 .
  • the loss tangent of S 9 was 4.6 ⁇ 10 ⁇ 5 .
  • L* was found to be 48.6 for S 8 and 76.0 for S 9 .
  • Adhesion strength for S 8 was less than 5 MPa and was 39 MPa for S 9 .
  • the cold-pressed disks were hot pressed with the same stackup as in Example 2.
  • the pressure and temperature cycles are the same as for example 4.
  • the loss tangent of S 10 was found to be 15 ⁇ 10 ⁇ 5 , and its porosity was measured to be 1%. Substantially no microcracks or fissures were observed in the corrosion-resistant non-porous yttria layer.
  • the as-hot-pressed layer thickness of Y 2 O 3 was 920 ⁇ m and the thickness of the Yb 2 O 3 layer was 530 ⁇ m after hot pressing. L* was found to be 49.7 for S 10 .
  • Adhesion strength for S 10 was 28 MPa.
  • the as-hot-pressed layer thickness of Y 2 O 3 was 700 ⁇ m and the thickness of the Yb 2 O 3 layer was 450 ⁇ m after hot pressing.
  • One yttria-alumina laminate (S 43 ) was cold pressed as described in Example 5, except that the yttria and ytterbia powders were supplied by PIDC.
  • the laminate used the APA powder from Sasol. Mo foil was placed on both sides of the laminate.
  • the cold-pressed disk was hot pressed with the same stackup as in Table 4 for Example 2.
  • the temperature and pressure cycles are shown in Tables 10 and 11.
  • the as-hot-pressed layer thickness of Y 2 O 3 for S 43 was 2950 ⁇ m and the thickness of the Yb 2 O 3 layer was 525 ⁇ m after hot pressing.
  • One yttria-alumina laminate (S 50 ) was cold pressed as described in Example 6.
  • the laminate used the APA powder from Sasol. Mo foil was placed on both sides of the laminate.
  • the yttria powder was mixed with 1 wt % ZrO 2 before use.
  • the cold-pressed disk was hot pressed with the same stackup as in Table 4 for Example 2.
  • the pressure and temperature cycles are the same as for Example 6.
  • the loss tangent of S 50 was found to be 2.39'10 ⁇ 5 .
  • the as-hot-pressed layer thickness of Y 2 O 3 was 720 ⁇ m and the thickness of the Yb 2 O 3 layer was 350 ⁇ m after hot pressing.
  • the grain size of the yttrium oxide layer was estimated to be about 2 ⁇ m.
  • Two yttria-alumina laminates were cold pressed as described in Example 7.
  • One laminate (S 54 ) used the APA powder by Sasol, along with PIDC yttria and a 40 ⁇ m thick ceramic tape of ytterbia, with the ytterbia powder also coming from PIDC.
  • the second laminate (S 55 ) used HPA alumina from Orbite Technologies, along with PIDC yttria and ytterbia. Both laminates had Mo foil on both faces.
  • the cold-pressed disks were hot pressed with the same stackup as in Table 4 for Example 2.
  • the pressure and temperature cycles are the same as for Example 6.
  • the loss tangent of S 54 was found to be 3.93 ⁇ 10 ⁇ 5 .
  • the as-hot-pressed layer thickness of Y 2 O 3 was 985 ⁇ m and the thickness of the Yb 2 O 3 layer was 40 ⁇ m after hot pressing.
  • the loss tangent was found to be 2.06 ⁇ 10 ⁇ 5 .
  • the as-hot-pressed layer thickness of Y 2 O 3 was 1000 ⁇ m and the thickness of the Yb 2 O 3 layer was 315 ⁇ m after hot pressing.
  • the grain size of the yttrium oxide layers for S 54 and S 55 were determined to be about 5 to 20 ⁇ m.
  • Two yttria-alumina laminates were cold pressed as described in Example 8.
  • One laminate (S 57 ) used the APA powder by Sasol, along with PIDC yttria mixed with 3 vol % yttrium oxyfluoride (YOF) and PIDC ytterbia.
  • the second laminate (S 58 ) APA powder by Sasol, PIDC ytterbia, and PIDC yttria mixed with 3 vol % Y 2 Si 2 O 7 . Both laminates had Mo foil on both faces.
  • the cold-pressed disks were hot pressed with the same stackup as in Table 4 for Example 2.
  • the pressure and temperature cycles are the same as for Example 6.
  • the loss tangent of S 57 was found to be 4.50 ⁇ 10 ⁇ 5 .
  • the as-hot-pressed layer thickness of Y 2 O 3 was 1085 ⁇ m and the thickness of the Yb 2 O 3 layer was 380 ⁇ m after hot pressing.
  • the grain size of the yttrium oxide layer for S 57 was determined to be about 50 ⁇ m.
  • the loss tangent was found to be 7.73 ⁇ 10 ⁇ 5 .
  • the as-hot-pressed layer thickness of Y 2 O 3 was 980 ⁇ m and the thickness of the Yb 2 O 3 layer was 425 ⁇ m after hot pressing.
  • the grain size of the yttrium oxide layer for S 58 was determined to be about 5 to 10 ⁇ m.
  • One laminate (S 49 ) was cold pressed as described in Example 6.
  • the laminate used the APA powder from Sasol as the alumina base and a blend of 77 wt % yttria, 15 wt % zirconia, and 8 wt % alumina as the top layer. Mo foil was placed on both sides of the laminate.
  • the cold-pressed disk was hot pressed with the same stackup as in Table 4 for Example 2.
  • the pressure and temperature cycles are the same as for Example 6.
  • the loss tangent of S 49 was found to be 13.3 ⁇ 10 ⁇ 5 .
  • the as-hot-pressed layer thickness of blended layer was 1215 ⁇ m.
  • Adhesion of the laminate was found to be 32 MPa.
  • the average grain size of the yttria-rich grains of the non-porous layer was estimated to be about 2 ⁇ m.
  • At least one second phase namely alumina-rich grains of the composition Y 4 Al 2 O 9 , was observed in the microstructure and this second phase is believed to contribute to increased strength of the layer.
  • the present disclosure in various aspects, embodiments, and configurations, includes components, methods, processes, systems and/or apparatus substantially as depicted and described herein, including various aspects, embodiments, configurations, subcombinations, and subsets thereof. Those of skill in the art will understand how to make and use the various aspects, aspects, embodiments, and configurations, after understanding the present disclosure.
  • the present disclosure in various aspects, embodiments, and configurations, includes providing devices and processes in the absence of items not depicted and/or described herein or in various aspects, embodiments, and configurations hereof, including in the absence of such items as may have been used in previous devices or processes, for example, for improving performance, achieving ease and/or reducing cost of implementation.

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US20170250057A1 (en) 2017-08-31
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