Classifications

• • H—ELECTRICITY
  • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
  • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
  • H10P50/00—Etching of wafers, substrates or parts of devices
  • H10P50/20—Dry etching; Plasma etching; Reactive-ion etching
  • H10P50/28—Dry etching; Plasma etching; Reactive-ion etching of insulating materials
  • H10P50/282—Dry etching; Plasma etching; Reactive-ion etching of insulating materials of inorganic materials
  • H10P50/283—Dry etching; Plasma etching; Reactive-ion etching of insulating materials of inorganic materials by chemical means
• • H—ELECTRICITY
  • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
  • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
  • H10P50/00—Etching of wafers, substrates or parts of devices
  • H10P50/20—Dry etching; Plasma etching; Reactive-ion etching
  • H10P50/28—Dry etching; Plasma etching; Reactive-ion etching of insulating materials
  • H10P50/282—Dry etching; Plasma etching; Reactive-ion etching of insulating materials of inorganic materials
  • H10P50/283—Dry etching; Plasma etching; Reactive-ion etching of insulating materials of inorganic materials by chemical means
  • H10P50/285—Dry etching; Plasma etching; Reactive-ion etching of insulating materials of inorganic materials by chemical means of materials not containing Si, e.g. PZT or Al2O3
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
  • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
  • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
  • C23C16/40—Oxides
  • C23C16/403—Oxides of aluminium, magnesium or beryllium
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
  • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
  • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
  • C23C16/40—Oxides
  • C23C16/405—Oxides of refractory metals or yttrium
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
  • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
  • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
  • C23C16/45523—Pulsed gas flow or change of composition over time
  • C23C16/45525—Atomic layer deposition [ALD]
  • C23C16/45553—Atomic layer deposition [ALD] characterized by the use of precursors specially adapted for ALD
• • H—ELECTRICITY
  • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
  • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
  • H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
  • H10P14/60—Formation of materials, e.g. in the shape of layers or pillars of insulating materials
  • H10P14/63—Formation of materials, e.g. in the shape of layers or pillars of insulating materials characterised by the formation processes
  • H10P14/6326—Deposition processes
  • H10P14/6328—Deposition from the gas or vapour phase
  • H10P14/6334—Deposition from the gas or vapour phase using decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
  • H10P14/6339—Deposition from the gas or vapour phase using decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition deposition by cyclic CVD, e.g. ALD, ALE or pulsed CVD
• • H—ELECTRICITY
  • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
  • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
  • H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
  • H10P14/60—Formation of materials, e.g. in the shape of layers or pillars of insulating materials
  • H10P14/66—Formation of materials, e.g. in the shape of layers or pillars of insulating materials characterised by the type of materials
  • H10P14/662—Laminate layers, e.g. stacks of alternating high-k metal oxides
• • H—ELECTRICITY
  • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
  • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
  • H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
  • H10P14/60—Formation of materials, e.g. in the shape of layers or pillars of insulating materials
  • H10P14/69—Inorganic materials
  • H10P14/692—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses
  • H10P14/6938—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses the material containing at least one metal element, e.g. metal oxides, metal oxynitrides or metal oxycarbides
  • H10P14/6939—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses the material containing at least one metal element, e.g. metal oxides, metal oxynitrides or metal oxycarbides characterised by the metal
  • H10P14/69391—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses the material containing at least one metal element, e.g. metal oxides, metal oxynitrides or metal oxycarbides characterised by the metal the material containing aluminium, e.g. Al2O3
• • H—ELECTRICITY
  • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
  • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
  • H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
  • H10P14/60—Formation of materials, e.g. in the shape of layers or pillars of insulating materials
  • H10P14/69—Inorganic materials
  • H10P14/692—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses
  • H10P14/6938—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses the material containing at least one metal element, e.g. metal oxides, metal oxynitrides or metal oxycarbides
  • H10P14/6939—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses the material containing at least one metal element, e.g. metal oxides, metal oxynitrides or metal oxycarbides characterised by the metal
  • H10P14/69392—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses the material containing at least one metal element, e.g. metal oxides, metal oxynitrides or metal oxycarbides characterised by the metal the material containing hafnium, e.g. HfO2
• • H—ELECTRICITY
  • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
  • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
  • H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
  • H10P14/60—Formation of materials, e.g. in the shape of layers or pillars of insulating materials
  • H10P14/69—Inorganic materials
  • H10P14/692—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses
  • H10P14/6938—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses the material containing at least one metal element, e.g. metal oxides, metal oxynitrides or metal oxycarbides
  • H10P14/6939—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses the material containing at least one metal element, e.g. metal oxides, metal oxynitrides or metal oxycarbides characterised by the metal
  • H10P14/69395—Inorganic materials composed of oxides, glassy oxides or oxide-based glasses the material containing at least one metal element, e.g. metal oxides, metal oxynitrides or metal oxycarbides characterised by the metal the material containing zirconium, e.g. ZrO2

Definitions

• the present invention relates to the field of semiconductor manufacturing and semiconductor devices, and more particularly, to a method of using ultra-thin inorganic etch stop layers in semiconductor processing.
• ALD Atomic layer deposition
• ALE atomic layer etching
• ESL ultrathin etch stop layer
• a substrate processing method includes depositing a first film on a substrate, depositing a second film on the first film, and selectively etching the second film relative to the first film using an ALE process, where the etching self-terminates at an interface of the second film and the first film.
• a substrate processing method includes providing a substrate containing a first film on a substrate and a second film on the first film, initiating etching of the second film using an ALE process that selectively etches the second film relative to the first film, and removing the second film using the ALE process, where the etching self-terminates at an interface of the second film and the first film.
• the method further includes, following the removing, etching the first film using an additional ALE process, where the ALE process includes alternating gaseous exposures of a first reactant and a second reactant, and the additional ALE process includes alternating gaseous exposures of a third reactant and a fourth reactant, and where the ALE process and the additional ALE process are performed without plasma excitation of the first reactant, the second reactant, the third reactant, and the fourth reactant.
• the first film has a uniform thickness of approximately one monolayer.
• a substrate processing method includes depositing a ZrCh film on a substrate, depositing a AI2O3 film on the ZrCh film, initiating etching of the AI2O3 film using a thermal ALE process that selectively etches the AI2O3 film relative to the ZrCh film, and removing the AI2O3 film using the thermal ALE process, wherein the etching self-terminates at an interface of the AI2O3 film and the ZrCL film.
• the ZrCh film has a uniform thickness of approximately one monolayer.
• the thermal ALE process includes alternating gaseous exposures of HF and A1(CEE) 3.
• the method further includes, following the removing, etching the ZrCL film using an additional thermal ALE process that includes alternating gaseous exposures of HF and A1(CH 3 )2C1.
• FIGS. 1 A - IE schematically show a method of processing a layer structure according to an embodiment of the invention
• FIG. 2 shows a substrate mass change traced with a quartz crystal microbalance (QCM) during deposition/etch processes according to an embodiment of the invention
• FIG. 3 shows a substrate mass change traced with a QCM during deposition/etch processes according to embodiment of the invention
• FIG. 4 shows etch rate measured by QCM according to an embodiment of the invention
• FIG. 5 shows a substrate mass change traced with a QCM during an ALE process according to embodiment of the invention.
• FIG. 6 shows in tabular form examples of combinations of etch reactants and materials that may be used for selective ALE according to embodiments of the invention.
• an ESL is used in material stacks to stop an etch process at an interface of different materials or to protect an underlying material from etching.
• Embodiments of the invention describe the use of an ESL that may be only one monolayer (atomic layer) thick and may be deposited and later removed in-situ in one or more process chambers.
• the methods described herein can provide significant reduction in processing time and materials usage in semiconductor device manufacturing, and allow deposition/etch processes in nano-sized spaces and 3D features. Further, the methods can reduce problems associated with stress buildup during integration of multi-stacks of materials in semiconductor devices.
• ALE is an etching technique for removing thin layers of material using sequential and self-limiting reactions.
• Thermal ALE that is performed in the absence of plasma excitation, provides isotropic atomic-level etch control using sequential thermally driven reaction steps that are self-saturating and self-terminating.
• Thermal ALE etch mechanisms can include fluorination and ligand-exchange, conversion- etch, and oxidation and fluorination reactions. The etching accuracy can reach atomic-scale dimensions, and a large area of uniform substrate etching can be achieved.
• FIGS. 1 A - IE schematically show a method of processing a layer structure according to an embodiment of the invention.
• the method includes providing a substrate 1 containing a base material 100 (e.g., a Si wafer), and a bottom film 102 on the base material 100.
• the substrate 1 may contain one or more additional films and materials and one or more simple or advanced patterned features.
• the method further includes depositing a first film 104 over the bottom film 102.
• the first film 104 may serve as an ESL.
• the first film 104 is a dielectric film.
• the first film 102 can include a metal oxide film with a general formula M x O y , where x and y are integers. Examples include ZrCh and AI2O3.
• the first film 104 can include ZrCh that may be uniformly deposited on the base material 100 using ALD processing.
• the first film 102 is not limited to metal oxides and may include or consist of other materials, for example oxides, nitrides, oxynitrides, and other materials found in semiconductor devices.
• the method further includes depositing a second film 106 on the first film 104, where the second film 106 contains a different material than the first film 104.
• the first film 104 may be used to stop a subsequent etch process at an interface of the second film 106 and the first film 104 or to protect the first film 102 from etching.
• the second film 106 is a dielectric film.
• the second film 106 can include a metal oxide film with a general formula M x O y , where x and y are integers. Examples include ZrCh, HfCh, and AI2O3. In one example, the second film 106 can include AI2O3 that may be uniformly deposited on the first film 104 using ALD processing. However, the second film 106 is not limited to metal oxides and may include or consist of other materials, for example oxides, nitrides, oxynitrides, and other materials found in semiconductor devices.
• the method further includes initiating etching of the second film 106 using an ALE process (e.g., a thermal ALE process) that selectively etches the second film 106 relative to the first film 104.
• the ALE process removes the second film 106 until the etching self- terminates at the interface of the second film 106 and the first film 104 due to the selective etching characteristics of the ALE process.
• FIG. ID schematically shows the substrate 1 when the second film 106 has been removed from the substrate 1. Thereafter, according to one embodiment, the first film 104 may be removed from the substrate 1, for example using an additional ALE process. This is schematically shown in FIG. ID.
• FIG. 2 shows a substrate mass change traced with a quartz crystal microbalance (QCM) during deposition/etch processes according to an embodiment of the invention.
• the mass trace 200 shows substrate mass gain/loss in ng/cm 2 on a QCM as a function of time, where mass gain and mass loss correspond to deposition and etch processes, respectively.
• the film structure included a bottom AI2O3 film, a ZrCL film on the bottom AI2O3 film, and a top AI2O3 film on the ZrCL film.
• the mass trace 200 is divided into three sections, where the first section 201 shows mass gain during ALD of the ZrCL film having a monolayer thickness on the bottom AI2O3 film, second section 202 shows mass gain during ALD of the top AI2O3 film on the ZrCL film, and third section 203 shows mass loss during etching and removal of the top AI2O3 film using an ALE process.
• the ALD of the ZrCL film was performed using alternating gaseous exposures of zirconium tetrachloride (ZrCL) and water (H2O), and the ALD of the top AI2O3 film was performed using alternating gas exposures of trimethyl aluminum (A1(CH3)3) and H2O.
• the ALE of the top AI2O3 film used alternating gas exposures of hydrogen fluoride (ELF) and A1(CEL)3, where each ALD cycle included AI2O3 surface fluorination using a HF exposure, followed by exposure to A1(CFE)3, which resulted in etching of the fluorinated surface layer (i.e., AIF3) through a ligand exchange reaction.
• Unbalanced ALE reactions for etching of the top AI2O3 film include:
• the etching of the top AI2O3 film proceeds until the top AI2O3 film is fully removed and then the ALE process self-terminates at the interface of the top AI2O3 film and the ZrCL film.
• the ALE process self-terminates because the ZrCL film is highly resistant to etching by the alternating gases exposures of HF and A1(CH3)3.
• the ZrCL film undergoes fluorination upon reaction with HF to form ZrF4
• the ligand exchange reaction with A1(CH3)3 is thermodynamically unfavorable under the ALE conditions and this disrupts and stops the etching process.
• Unbalanced ALE reactions for the ZrCL film include:
• etch resistance of the ZrCL film is clearly shown in section 203 of FIG. 2, where, during removal of the top AI2O3 film, the measured mass trace 200 asymptotically approaches the mass of the ZrCL film after a large number of ALE cycles.
• fluorination of ZrCL is observed as a mass gain in each ALE cycle, following the subsequent exposure of the fluorinated surface to Al(CH3)3(g>, no net change in mass is observed, indicating a passive surface toward an exchange reaction.
• the etch process stops on the ZrCL film after fully etching and removing the top AI2O3 film, thereby demonstrating that the ZrCh film, although having only a monolayer thickness, acts as an ESL to effectively protect the underlying material (i.e., the bottom AI2O3 film) from etching.
• the etch blocking ability of the ZrCk film as an ESL can in theory be infinite as the ligand exchange reaction is thermodynamically unfavorable under the ALE conditions. This allows an ultra-thin ESL with a monolayer thickness to effectively block the ALE process by using a proper material as an ESL.
• FIG. 3 shows substrate mass change traced with a QCM during deposition/etch processes according to embodiment of the invention.
• the trace 300 shows mass gain during ALD of a ZrCh film using alternating gas exposures of ZrCL and H2O, and mass change during subsequent ALE processing of the ZrCh film using alternating gas exposures of HF and A1(CH 3 )3.
• the robustness of the ZrCh film as an ESL is clearly demonstrated and shows a 100% blocking efficiency of the ZrF4 surface of the ZrCE film, even after 100 cycles of the ESL process.
• FIG. 4 shows etch rate measured by QCM according to embodiment of the invention.
• the etch rate of an AI2O3 film in an ALE process as a function of different amounts of ZrCh pre-deposited on the AI2O3 film is shown in the figure.
• the ZrCh was deposited by ALD using alternating gas exposures of A1(CH3)3 and H2O, and the ALE process was performed using alternating gas exposures of HF and A1(CH3)3.
• the experimental data in solid circles 400 shows that increasing amount of ZrCL deposited on the AI2O3 film resulted in reduced amount of etching of the underlying AI2O3 film.
• the effective etch blocking of ZrCh at a thickness of approximately one monolayer shows that the first monolayer of ZrCh uniformly covers the AI2O3 film and that the ZrCL precursor is more reactive towards exposed AI2O3 surface sites than the ZrCh covering the AI2O3 film.
• FIG. 5 shows a substrate mass change traced with a QCM during an ALE process according to embodiment of the invention.
• a ZrCh film is not etched by thermal ALE processing that etches a AI2O3 film using alternating gas exposures of HF and A1(CH3)3, the ZrCh film may be etched and removed by replacing one or more of the gaseous etch reactants in the ALE processing.
• a ZrCh film was etched, as shown in trace 500, by thermal ALE processing using alternating gas exposures of HF and dimethyl aluminum chloride (DMAC, A1(03 ⁇ 4)2q). Replacing A1(03 ⁇ 4)3 with A1(03 ⁇ 4)2q renders the ligand exchange reaction thermodynamically favorable and thereby enables etching of the ZrCh film according the following unbalanced ALE reactions:
• FIG. 6 shows in tabular form examples of combinations of etch reactants and materials that may be used for selective ALE according to embodiments of the invention. The listed combinations are based on experimental and thermodynamic information.
• a ZrCh film may be used as an ESL for thermal ALE processing of AI2O3 and HfCh films using alternating gaseous exposures of HF and A1(CH 3 ) 3. Thereafter, if desired, the ZrCh film may be removed using alternating gaseous exposures of HF and A1(CH 3 )2C1, for example.
• an AI2O3 film may be used as an ESL for thermal ALE processing of ZrCh and HfCh films using alternating gaseous exposures of HF and SiCl 4. Thereafter, if desired, the AI2O3 film may be removed using alternating gaseous exposures of HF and A1(CH 3 ) 3 , for example.
• the ALD processing, the ALE processing, or both may be performed at a substrate temperature between about 100°C and about 400°C, between about 200°C and about 400°C, or between about 200°C and about 300°C. In one example, the ALD processing, the ALE processing, or both, may be performed at a substrate temperature between about 250°C and about 280°C.
• the ALD processing and the ALE processing may be performed at the same substrate temperature or at approximately the same substrate temperature. Those skilled in the art will readily appreciate that this allows for high substrate throughput when performing both the ALD processing and the ALE processing in the same process chamber, and when using different process chambers for the ALD processing and the ALE processing.
• two or more of the ALD processing, the ALE processing, and the additional ALE processing may be performed at that same substrate temperature or at approximately the same substrate temperature.
• the ALE processing and the additional ALE processing may be performed at the same substrate temperature or at approximately the same substrate temperature.

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