WO2003090268A1 - Procede de traitement de substrat et procede de production de dispositifs a semi-conducteurs - Google Patents
Procede de traitement de substrat et procede de production de dispositifs a semi-conducteurs Download PDFInfo
- Publication number
- WO2003090268A1 WO2003090268A1 PCT/JP2003/005032 JP0305032W WO03090268A1 WO 2003090268 A1 WO2003090268 A1 WO 2003090268A1 JP 0305032 W JP0305032 W JP 0305032W WO 03090268 A1 WO03090268 A1 WO 03090268A1
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- WIPO (PCT)
- Prior art keywords
- silicon substrate
- substrate
- processing method
- ultraviolet light
- ultraviolet
- Prior art date
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 155
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 145
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Classifications
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
- H01L21/28008—Making conductor-insulator-semiconductor electrodes
- H01L21/28017—Making conductor-insulator-semiconductor electrodes the insulator being formed after the semiconductor body, the semiconductor being silicon
- H01L21/28158—Making the insulator
- H01L21/28167—Making the insulator on single crystalline silicon, e.g. using a liquid, i.e. chemical oxidation
- H01L21/28194—Making the insulator on single crystalline silicon, e.g. using a liquid, i.e. chemical oxidation by deposition, e.g. evaporation, ALD, CVD, sputtering, laser deposition
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
- H01L21/02043—Cleaning before device manufacture, i.e. Begin-Of-Line process
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- H01L21/02107—Forming insulating materials on a substrate
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- H01L21/02126—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon the material containing Si, O, and at least one of H, N, C, F, or other non-metal elements, e.g. SiOC, SiOC:H or SiONC
- H01L21/0214—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon the material containing Si, O, and at least one of H, N, C, F, or other non-metal elements, e.g. SiOC, SiOC:H or SiONC the material being a silicon oxynitride, e.g. SiON or SiON:H
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- H01L21/0223—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate
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- H01L21/02236—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate of the semiconductor substrate or a semiconductor layer group IV semiconductor
- H01L21/02238—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate of the semiconductor substrate or a semiconductor layer group IV semiconductor silicon in uncombined form, i.e. pure silicon
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- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
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- H01L21/28167—Making the insulator on single crystalline silicon, e.g. using a liquid, i.e. chemical oxidation
- H01L21/28202—Making the insulator on single crystalline silicon, e.g. using a liquid, i.e. chemical oxidation in a nitrogen-containing ambient, e.g. nitride deposition, growth, oxynitridation, NH3 nitridation, N2O oxidation, thermal nitridation, RTN, plasma nitridation, RPN
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- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/314—Inorganic layers
- H01L21/3143—Inorganic layers composed of alternated layers or of mixtures of nitrides and oxides or of oxinitrides, e.g. formation of oxinitride by oxidation of nitride layers
- H01L21/3144—Inorganic layers composed of alternated layers or of mixtures of nitrides and oxides or of oxinitrides, e.g. formation of oxinitride by oxidation of nitride layers on silicon
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- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
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- H01L21/314—Inorganic layers
- H01L21/316—Inorganic layers composed of oxides or glassy oxides or oxide based glass
- H01L21/3165—Inorganic layers composed of oxides or glassy oxides or oxide based glass formed by oxidation
- H01L21/31654—Inorganic layers composed of oxides or glassy oxides or oxide based glass formed by oxidation of semiconductor materials, e.g. the body itself
- H01L21/31658—Inorganic layers composed of oxides or glassy oxides or oxide based glass formed by oxidation of semiconductor materials, e.g. the body itself by thermal oxidation, e.g. of SiGe
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- H01L29/40—Electrodes ; Multistep manufacturing processes therefor
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- H01L29/49—Metal-insulator-semiconductor electrodes, e.g. gates of MOSFET
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- H01L29/66409—Unipolar field-effect transistors
- H01L29/66477—Unipolar field-effect transistors with an insulated gate, i.e. MISFET
- H01L29/66545—Unipolar field-effect transistors with an insulated gate, i.e. MISFET using a dummy, i.e. replacement gate in a process wherein at least a part of the final gate is self aligned to the dummy gate
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S438/00—Semiconductor device manufacturing: process
- Y10S438/906—Cleaning of wafer as interim step
Definitions
- the present invention relates to a semiconductor device, and more particularly, to a substrate processing method for forming a substantially very thin insulating film having excellent characteristics on a substrate, and a method of manufacturing a semiconductor device using the insulating film.
- the thickness of the gate insulating film is reduced as the gate length is reduced due to the miniaturization. Need to be reduced according to the scaling law.
- the thickness of the gate insulating film must be set to l to 2 nm or less when using a conventional silicon thermal oxide film. In such a very thin gate insulating film, the problem that the tunnel current increases and the gate leakage current increases as a result cannot be avoided.
- Forming a high dielectric film directly on a silicon substrate is preferable in order to reduce the silicon oxide equivalent effective thickness of the insulating film.
- the metal element diffuses from the high-dielectric film into the silicon substrate, and the scattering of carriers in the channel region occurs. Problems arise.
- an extremely thin base having a thickness of 1 nm or less, preferably 0.8 nm or less is provided between the high-dielectric gate oxide film and the silicon substrate. It is preferable to interpose an oxide film. Such a very thin base oxide film must uniformly cover the surface of the silicon substrate and is required not to form defects such as interface states.
- a thin gut oxide film is generally formed by rapid thermal oxidation (RTO) treatment of a silicon substrate.
- RTO rapid thermal oxidation
- a thermal oxide film is formed to a desired thickness of 1 nm or less, it is necessary to lower the processing temperature during film formation.
- a thermal oxide film formed at such a low temperature tends to contain defects such as interface states, and is not suitable as a base oxide film of a high-dielectric gate oxide film.
- UV-O UV-excited oxygen radical
- FIG. 22 shows a schematic configuration of a conventional UV-O 2 radical substrate processing apparatus 10.
- the substrate processing apparatus 100 has a processing container 101 that holds the processing substrate 102 under a reduced pressure environment, and the substrate to be processed 10 0 2 is held on a holding table 101A having a heater 101a. Further, a shield head 101B is provided in the processing container 101 so as to face the substrate 22 on the holding table 101A, and the shield head 1B is provided. 0 1 oxygen gas to B, 0 2, N 2 0 , NO or oxidizing gas made from these mixtures are supplied.
- the glass head 101B is made of a material that is transparent to ultraviolet light such as quartz, and the processing vessel 101 is provided with a window 101C for transmitting ultraviolet light such as quartz. It is formed so as to expose the substrate to be processed 102 on the holding table 101A. Further, an ultraviolet light source 103 movable along the surface of the window 101C is formed outside the window 101C.
- a silicon substrate is introduced into the processing vessel 101 in Fig. 21 as the substrate to be processed 102, and the inside of the processing chamber 101 is exhausted.
- an oxidizing gas such as oxygen is introduced.
- the ultraviolet light source 103 is driven to form active radicals O * in the oxidizing gas.
- Such UV-activated radicals oxidize the exposed surface of the silicon substrate 102, and as a result, a very thin oxide film of about 0.4 to 0.8 nm is formed on the surface of the silicon substrate 102. It is formed.
- the oxide film can be formed to a uniform thickness by moving the ultraviolet light source 103 along the optical window 101 C. .
- the base oxide film under the high dielectric gate insulating film is very thin needed, using UV-o 2 radical substrate processing apparatus, 0.
- a base oxide film with a thickness of about 8 nm has been realized.
- a metal oxide film with a small interatomic valency so-called “low rigidity”
- high rigidity the interface between the silicon substrate and the metal oxide film becomes mechanically unstable and may cause defects.
- forming the oxynitride film as the base oxide film of the high dielectric gate insulating film composes the silicon substrate with the metal element or oxygen in the high dielectric gate insulating film.
- a more specific object of the present invention is to provide a substrate processing method capable of directly forming a very thin oxynitride film on a silicon substrate stably with good reproducibility while eliminating the influence of organic contamination. It is in.
- the substrate processing method of the present invention is characterized in that it has a step of removing carbon from the surface of a silicon substrate by irradiating the surface of the silicon substrate with ultraviolet light in an atmosphere of an essentially ultraviolet inert gas.
- the carbon removal step is performed while the silicon substrate to be irradiated with ultraviolet rays is heated from normal temperature.
- the method is characterized in that ultraviolet irradiation for the carbon removing step is performed under a reduced pressure atmosphere.
- the ultraviolet inert gas is nitrogen gas.
- the silicon substrate irradiated with ultraviolet rays is heated from room temperature, and the maximum temperature is 450 ° C.
- the ultraviolet light irradiating the surface of the silicon substrate has a wavelength of 150 to 270 nm.
- the light source of the ultraviolet light for irradiating the surface of the silicon substrate may be a derivative barrier discharge tube, a mercury lamp or a deuterium lamp.
- Another substrate processing method according to the present invention is the substrate processing method, wherein carbon is removed from the surface of the silicon substrate in the absence of oxygen; Forming an oxynitride film on the plate surface.
- an example of the step of forming an oxynitride film on the surface of the silicon substrate may include a step of irradiating an ultraviolet ray in the presence of nitrogen and oxygen.
- Still another substrate processing method includes a step of removing carbon from the surface of a silicon substrate by irradiating the surface of the silicon substrate with ultraviolet light in an atmosphere of an essentially ultraviolet inert gas; A step of forming an oxynitride film by irradiating ultraviolet rays in an atmosphere of an essentially ultraviolet inert gas.
- the step of forming the oxynitride film is a step of irradiating an ultraviolet ray in the presence of nitrogen and oxygen.
- Still another substrate processing method includes a step of removing carbon from the surface of a silicon substrate by irradiating the surface of the silicon substrate with ultraviolet light in an atmosphere of an essentially ultraviolet inert gas; And a step of exciting the NO gas with ultraviolet light to form an oxynitride film on the surface of the silicon substrate.
- the ultraviolet light has a wavelength of 145 to 192 nm.
- it is preferable that the ultraviolet light has a wavelength of about 170 nm.
- the ultraviolet light ultraviolet light formed by a dielectric barrier discharge tube in which xenon is sealed.
- the carbon removal step is preferably performed at a substrate temperature not exceeding 450 ° C.
- the oxynitride film forming step is preferably performed at a substrate temperature in the range of 450 to 550 ° C.
- the oxynitride film forming step is preferably performed in a time of 200 seconds or less.
- Oxynitride film forming step 1. 3 3 ⁇ 1. 3 3 3 X 1 0 _ 3 what to be executed in the process pressure in the range of P a is preferable.
- the natural oxide film on the surface of the silicon substrate is removed before the oxynitride film forming step.
- a method of manufacturing a semiconductor device includes the steps of: irradiating an ultraviolet ray to a silicon substrate surface in an essentially ultraviolet inert gas atmosphere to remove carbon from the surface; Supplying the NO gas, exciting the NO gas with ultraviolet light to form an oxynitride film on the surface of the silicon substrate, and forming a high dielectric film on the oxynitride film. And a step of forming a good electrode on the high dielectric film.
- the ultraviolet light preferably has a wavelength of 145 to 192 nm.
- the ultraviolet light has a wavelength of 1.72 nm.
- the ultraviolet light has a wavelength of 170 nm.
- ADVANTAGE OF THE INVENTION it becomes possible to eliminate the influence of the organic contamination on the silicon surface, and to perform the oxynitridation process. At this time, it is possible to eliminate the film thickness instability, nitrogen concentration instability, and nitrogen depth profile instability caused by organic contamination, and to form an oxynitride film stably and with good reproducibility. Will be possible.
- the present invention is a technique that can be further applied to the conventional oxide film formation.
- FIG. 1 is a vertical sectional view showing a configuration of a substrate processing apparatus used in the present invention. You.
- FIG. 2 is an atomic force microscope (AFM) image of a silicon substrate subjected to the substrate processing method according to the present embodiment.
- AFM atomic force microscope
- FIG. 3 is a plan view of a cluster type processing apparatus including the substrate processing apparatus according to the present embodiment.
- FIG. 4 shows the results obtained by performing XPS analysis on a silicon substrate sample subjected to the substrate processing method according to the present embodiment, and obtaining a photoelectron spectrum.
- Figure 5 is a graph showing the effect of various treatments on carbon removal from the silicon substrate surface.
- FIG. 6 is a graph showing the relationship between the film thickness and the oxidation time when the substrate processing method according to the present embodiment is performed.
- FIG. 7 is a diagram for explaining the film thickness determination by the XPS method used in the present invention.
- FIG. 8 is another diagram for explaining the film thickness determination by the XPS method used in the present invention.
- FIG. 9 is a diagram showing a stationary phenomenon that appears when the silicon substrate surface is oxidized by the substrate processing apparatus shown in FIG.
- FIGS. 10A and 10B are diagrams schematically showing the states of (A) and (B) of the oxidation treatment of the silicon substrate surface performed by the substrate processing apparatus of FIG.
- FIG. 11 shows (A) and (B) forces.
- the film thickness distribution when the oxide film formed on the silicon substrate surface is subjected to UV-NO nitridation treatment is shown.
- FIGS. 12A and 12B show the case where (A) and (B) show a film obtained by forming an oxynitride film directly on the surface of a silicon substrate by UV-NO nitridation in the first embodiment of the present invention. It is a figure showing thickness distribution.
- FIG. 13 shows the (A) and (B) forces S according to the first embodiment of the present invention.
- FIG. 3 is a diagram showing the kinetics of forming an oxynitride film on a silicon substrate surface by UV-NO nitridation.
- FIGS. 14A and 14B show the kinetics of formation of an oxynitride film on the silicon substrate surface by UV-NO nitridation according to the first embodiment of the present invention.
- FIGS. 15A and 15B show the kinetics of the formation of an oxynitride film on the surface of a silicon substrate by UV-NO nitridation according to the first embodiment of the present invention.
- FIG. 16 is a diagram showing potential curves in various excited states of the NO molecule.
- FIG. 17 is a diagram illustrating an example of an ultraviolet light source.
- FIGS. 18A to 18C are diagrams illustrating the steps of manufacturing a semiconductor device according to the second embodiment of the present invention.
- FIGS. 19 (D) and (E) are diagrams illustrating the steps of manufacturing a semiconductor device according to the second embodiment of the present invention.
- FIGS. 20A and 20B show film thickness distributions when an oxynitride film is directly formed on the surface of a silicon substrate by UV-NO nitridation in the second embodiment of the present invention.
- FIG. 21 shows the results of measuring the nitrogen concentration taken into the film by the NO gas treatment according to the first embodiment at XPS detection angles of 90 ° and 30 °, and measuring the detection angle of 90 ° by XPS. It is the graph which took the ratio (30 ° / 90 °) of the measurement of the detection angle of 30 °.
- FIG. 22 is a vertical sectional view showing the configuration of a conventional UV-O 2 oxidation treatment apparatus.
- FIG. 3 is a plan view of a cluster type processing apparatus 60 including the substrate processing apparatus 20 according to the present embodiment.
- the substrate processing apparatus 20 includes a processing container 21 having a holding table 21 A for holding a substrate 22 to be processed, and the processing table 21 includes the holding table 21.
- a shower head 21 B made of a material, such as quartz, that transmits ultraviolet light is disposed opposite to the substrate 22 on A.
- the processing vessel 21 is exhausted through an exhaust port 21C, while an oxygen gas or a NO gas is supplied to the shear head 21B from an external gas source.
- the processing vessel 21 is further exposed to ultraviolet light such as quartz so that the shield head 21 B and the substrate 22 to be processed thereunder are exposed above the shield head 21 B.
- An optical window 21D made of a material that transmits light is provided.
- a heater 21a for heating the substrate to be processed 22 is provided in the holding table 21A.
- an ultraviolet light exposure device 24 is disposed via a coupling portion 23 provided corresponding to the optical window 21 D.
- the ultraviolet light exposure apparatus 24 includes a quartz optical window 24A corresponding to the optical window 21D, and the substrate to be processed which emits ultraviolet light through the quartz optical window 24A and the optical window 21D.
- the robot 24C is movably held in a direction parallel to the optical window 24A.
- the ultraviolet light source 24B is a linear light source provided so as to extend substantially perpendicular to the moving direction.
- a linear light source in the present invention, for example, an excimer lamp having a wavelength of 170 nm is used.
- the ultraviolet light generated by the ultraviolet light source 24B is absorbed by oxygen in the air before being introduced into the processing vessel 21 through the optical window 21D.
- an inert gas such as N 2 is supplied to the coupling portion 23 from an external gas source (not shown) through a line 23 A, and the inert gas is The light flows into the space 24D in the ultraviolet light exposure device 24 through a gap formed in the mounting portion of the optical window 24A of the light exposure device 24.
- shielding plates 24F are provided on both side surfaces of the ultraviolet light source 24B in order to prevent oxygen in the atmosphere from being entrained and flowing in just below the ultraviolet light source 24B. Further, under the shielding plate 24F, the height formed between the optical window 24A facing the ultraviolet light source 24B and the shielding plate 24F is at most about 1 mm. in a narrow region, an inert gas such as N 2 is supplied via line 2 4 b.
- This region is also supplied with the inert gas from line 23A, so that oxygen absorbing ultraviolet light is effectively eliminated in this region.
- the inert gas that has passed through the area below the shielding plate 24F flows into the space 24D, and is further discharged to the outside through an exhaust port 24E formed in the ultraviolet light exposure device 24. Is done.
- the movement and running of the ultraviolet light source 24 B can be controlled by the robot 24 C in the ultraviolet light exposure apparatus 24.
- Oxynitride on the surface of 2 by UV-activated oxynitridation By controlling the amount of exposure to ultraviolet light when forming the film, the distribution of the film thickness can be controlled.
- the robot 24C is controlled by a control device 25 such as a computer.
- the control device 25 also controls the driving of the ultraviolet light source 24B.
- a silicon substrate is subjected to carbon removal processing.
- the substrate processing apparatus 20 shown in FIG. 1 is used, and the carbon removal processing is performed in the substrate processing apparatus 20 in the absence of oxygen.
- an oxygen-free environment is formed in the processing vessel 21 and then the carbon on the silicon substrate is removed. Is removed. That is, a silicon substrate as a substrate to be processed is placed on a holding table 21A in a processing container 21 of the substrate processing apparatus 20, and the silicon substrate is sealed after the processing container 21 is sealed. Heat and fill processing vessel 21 with reduced pressure nitrogen gas. In this state, the ultraviolet lamp is turned on and driven to remove carbon on the surface of the silicon substrate.
- a silicon substrate 22 to be processed is placed on a substrate holder 21A provided with a heater 2la at a normal temperature as shown in FIG.
- the air is exhausted from the exhaust port 21C, and the atmosphere is heated to the nitrogen gas atmosphere by the heater 21a while irradiating ultraviolet rays with the ultraviolet light source 24.
- the temperature of the silicon substrate introduced into the processing chamber at room temperature gradually increases toward the heater heating temperature.
- the carbon compound on the silicon substrate is easily reduced in molecular weight by the energy of ultraviolet irradiation, is scattered and vaporized by elevating the temperature of the substrate, is evacuated, and is easily removed. It is preferable that the actual temperature of the substrate when irradiated with ultraviolet rays in an N 2 atmosphere be 450 ° C. or less.
- a temperature of 450 ° C. or more is suitable. Higher temperatures are better for better film quality. Therefore, a processing temperature of 700 to 75 ° C. is preferable in consideration of device requirements.
- a substantially thin oxynitride film with good film quality can be formed densely and stably in a few seconds.
- the temperature of the carbon removing step and the temperature of the film forming step can be separately and precisely controlled using an infrared lamp or the like as a heating source of the silicon substrate, and the process can be advanced.
- the silicon substrate Before placing the silicon substrate inserted into the processing chamber at room temperature on the heated substrate holder, immediately away from the substrate holder at the insertion position of the substrate, under a reduced pressure nitrogen atmosphere, preferably at several tens of OmTorr ultraviolet rays Drive the irradiation device. Since the temperature rise of the substrate due to the radiation from the substrate holder and the heat transfer by the nitrogen gas is relatively slow, the carbon compound on the substrate surface is degraded to low molecular weight by ultraviolet rays before reaching 450 ° C, and under a reduced pressure atmosphere. It is easily scattered and evaporated. Thereafter, the silicon substrate is placed on the heated substrate holder, and a desired oxynitride film forming step is performed. It is important to keep the nitrogen pressure low to keep the heat transfer by the gas low and to help the diffusion of carbon compounds.
- the carbon removal effect is shown by the roughness of the silicon surface by high-temperature Ar anneal following the carbon removal process.
- Figures 2 (A)-(C) show natural oxidation by HF treatment (DHF cleaning treatment).
- the silicon substrate 22 from which the film has been removed is introduced into the substrate processing apparatus 20 of FIG. 1 as a substrate to be processed, and a nitrogen gas is supplied to the shower head 21 B, and the ultraviolet light source 24 B perform UV-N 2 processing by driving the or oxygen gas is supplied to the head 2 1 B to the shower performs UV-O 2 processing by driving the ultraviolet source 2 4 B, and et al Fig. 2 is an atomic force microscope (AFM) image showing the substrate surface when heat treatment was performed for 90 seconds at 1175 ° C and 106 Pa in an Ar atmosphere.
- AFM atomic force microscope
- FIG. 2 (A) is a comparative example, and shows a case where a silicon substrate 22 is subjected to a DHF cleaning process and then a flattening process is performed without being processed by the substrate processing apparatus 20.
- FIG. 2 (B) shows that the silicon substrate is placed in the substrate processing apparatus 20 under a pressure of about 2.66 Pa ( 2 ⁇ 10 to 12 Torr).
- the results obtained by introducing oxygen gas at a flow rate of 150 SCCM from the hard head 21B at a substrate temperature of C at a flow rate of 150 SCCM and driving the ultraviolet light source 24B for 5 minutes are shown.
- FIG. 2 (C) shows the result of performing the same process as in FIG. 2 (B) by introducing nitrogen gas instead of oxygen gas from the shower head 21B.
- the heat treatment was performed by a rapid heat treatment (RTP) including an infrared lamp heating device via a vacuum transfer path 61 through a substrate processing apparatus 20 as shown in FIG. This is performed in the substrate processing apparatus 20 having a cluster configuration connected to the chamber 62.
- RTP rapid heat treatment
- the substrate processing apparatus 20 further includes a substrate loading / unloading module 63 and a cooling module 64 coupled to the vacuum transfer path 61.
- FIGS. 2A and 2C a large number of island-shaped defects are formed on the substrate surface, whereas in FIG. 2C, It can be seen that no such defect exists.
- the surface of the silicon substrate 22 is slightly tilted in the [110] direction. Along with this slight tilt, it can be seen that the two domains that define the 2 ⁇ 1 atomic terrace and the 1 ⁇ 2 atomic terrace are alternately arranged, and a single atomic step is formed by a single atomic layer step.
- the silicon atoms on the surface of the reconstructed silicon (100) form dimer rows at the 2 XI atomic terrace and the IX 2 atomic terrace. Since the directions of the silicon atom dimers are orthogonal between adjacent terraces, the line of the step becomes straight or crunchy depending on whether the energy at the step end is small or large.
- the surface roughness was measured for the samples in Figs. 2 (A) and (B).
- the average surface roughness Rms was 2.09 nm and 1.27 nm, respectively, and the maximum irregularity amplitude PV was 16.1 l. nm and 11.7 nm.
- the average surface roughness Rms was slightly reduced to 0.113 nm, and the maximum unevenness amplitude PV was also reduced to 1.33 nm.
- Figure 4 Referring to (A), but a large peak of photoelectrons corresponding to C s orbital is due to hydrocarbon in the atmosphere adsorbed on the surface of the substrate during transport to the analysis device, partly in the peak overlapping, sea urchin i indicated by the arrow in the figure, Kemikarureshifu bets C ls peak caused by the presence of S i C bond is Mihaka. A similar chemical shift occurs in the spectrum of Fig. 4 (B), but the spectrum is sharp in Fig. 4 (C), which corresponds to the sample of Fig. 2 (C). It can be seen that no C bond has been formed.
- Figs. 2 (A) to 2 (C) above show that the surface roughness of the substrate surface rapidly increases when SiC defects are present on the silicon substrate surface. This is because the SiC defects pinned the movement of the silicon atoms on the silicon substrate surface, thereby hindering the movement of the silicon atoms along the surface. By removing the iC defects, the silicon atoms move freely under the temperature and pressure conditions used in normal semiconductor processes, indicating that atomic layer steps are formed.
- Figure 5 shows the results obtained by using GCM ass spectacles to remove carbon from the silicon substrate surface by various treatments. See Figure 5 However, when carbon removal treatment is not performed, about 1200 ng of organic matter adheres to the surface of the 8-inch silicon substrate, but it is removed to some extent by treatment with ozone, oxygen, or nitrogen. You can see that you can do it. Of these treatments, the treatment with nitrogen is the most effective, and it can be seen that the treatment for 15 seconds can reduce the amount of residual organic matter to about 350 ng, and the treatment for 30 seconds to about 200 ng. . Table 1 below shows the energies of various carbon bonds.
- a silicon oxide film is formed on the surface of the silicon substrate 22 using the UV radical substrate processing apparatus 20 of FIG. 1, and the substrate temperature is set to 450 ° C.
- the following shows the relationship between the film thickness and the oxidation time when oxygen gas is supplied to the head 21 B and the ultraviolet light irradiation intensity and the oxygen gas flow rate or the oxygen partial pressure are varied in various ways.
- the natural oxide film on the surface of the silicon substrate 22 was removed prior to the radical oxidation, and in some cases, the carbon compound remaining on the substrate surface was removed by a decomposition reaction using ultraviolet light.
- the substrate surface is flattened by performing a high-temperature heat treatment at about 950 ° C. in an Ar atmosphere.
- the ultraviolet light source 24 B an excimer lamp having a wavelength of 172 nm was used.
- the UV irradiation intensity was set to 5% of the reference intensity (50 mWZcm 2 ) at the window surface of UV light source 24 B, and the process pressure was set to 665 mP.
- a 5 mTorr
- the relationship between the oxidation time and the oxide film thickness when the oxygen gas flow rate was set to 30 SCCM.
- the data in series 2 set the ultraviolet light intensity to zero and set the process pressure to 13 3 P a (1 Torr), shows the relationship between the oxidation time and the oxide film thickness when the oxygen gas flow rate is set to 3 SLM.
- the data in series 3 set the ultraviolet light intensity to zero, The relationship between the oxidation time and the oxide film thickness when the process pressure is set to 2.66 Pa (20 mTorr) and the oxygen gas flow rate is set to 150 SCCM is shown.
- the intensity is set to 100%, that is, the reference intensity
- the process pressure is set to 2.66 Pa (20 mTorr)
- the oxygen gas flow rate is set to 150 SCCM.
- oxide film thickness The data for series 5 was set at 20% of the reference intensity of ultraviolet light, the process pressure was 2.66 Pa (20 mTorr), and the oxygen gas flow rate was 150 SCCM. The relationship between the oxidized temperature and the oxide film pressure is shown.
- the data in series 6 shows that the ultraviolet light irradiation intensity is set to 20% of the reference irradiation intensity, and the process pressure is set to about 67 P a 5 Torr), and shows the relationship between the oxidation time and the oxide film thickness when the oxygen gas flow rate is set to 0.5 SLM.
- the relationship between the oxidation time and the oxide film thickness when the process pressure was set at 2.66 Pa (20 mTorr) and the oxygen gas flow rate was set at 150 SCC ⁇ was set to 5%.
- the thickness of the oxide film is determined by the XPS method. However, there is no unified method for obtaining the thickness of the oxide film extremely thin below 1 nm.
- I x + is the integrated intensity of the spectrum peak corresponding to the oxide film (I 1 + + I 2 + + I 3 + + I 4 + ). This corresponds to the peak seen in the energy region of 104 eV.
- I ° + corresponds to the integrated intensity of the spectrum peak due to the silicon substrate, which corresponds to the energy region near 100 eV.
- the oxide film to be formed has a uniform thickness because such a dwell time continues to some extent. That is, according to the present invention, an oxide film having a thickness of about 0.4 nm can be formed on a silicon substrate to a uniform thickness.
- FIGS. 10A and 10B schematically show a process of forming a thin oxide film on such a silicon substrate. It should be noted that in these figures, the structure on the silicon (100) substrate is greatly simplified.
- one oxygen layer is formed on the silicon substrate surface by bonding two oxygen atoms per silicon atom.
- the silicon atoms on the substrate surface are coordinated by two silicon atoms inside the substrate and two oxygen atoms on the substrate surface, forming a suboxide.
- the silicon atom at the top of the silicon substrate is coordinated by four oxygen atoms, and a stable Si 4 + state is obtained. For this reason, it is considered that oxidation rapidly proceeds in the state of FIG. 10 (A), and the oxidation stops in the state of FIG. 10 (B).
- the thickness of the oxide film in the state of FIG. 10 (B) is about 0.4 nm, which is in good agreement with the oxide film thickness in the stationary state observed in FIG.
- the lower peak seen in the energy range of 101 to 104 eV when the oxide film thickness is 0.1 nm or 0.2 nm is shown in FIG.
- the peak that appears in this energy region when the oxide film thickness exceeds 0.3 nm corresponds to the suboxide of 0 (A) and is due to Si 4 +. It is considered to represent
- Fig. 11 (A) shows that the oxide film thus formed on the silicon substrate to a thickness of 0.4 nm is continuously applied to the shower head in the substrate processing apparatus 20 of Fig. 1.
- the figure shows the film thickness distribution obtained by ellipsometry when oxynitriding by supplying NO gas to 21 B.
- Table 2 shows the results obtained by setting the detection angle to 90 ° using the XPS method described above, with the actual film thickness at the center and the periphery of the substrate shown in Fig. 11 (A). .
- NO gas is supplied to the above-mentioned shear head 21 B at a flow rate of 200 SCCM, and the internal pressure of the processing vessel 21 is set to 3.99 Pa (0.03 Torr). ), While driving the ultraviolet light source 24 B at the reference intensity for 3 minutes.
- the substrate temperature is set at 450 ° C.
- Figure 11 (B) shows the film thickness distribution after oxynitriding obtained by ellipsometry when an oxide film was formed to a thickness of 0.7 ⁇ m on the silicon substrate surface under the same conditions.
- Table 2 shows the actual film thickness obtained by setting the detection angle to 90 ° by the XPS method for the center portion and the peripheral portion of the substrate.
- Fig. 12 (A) shows the case where the Si substrate from which the natural oxide film was removed was directly subjected to UV radical-NO treatment in the substrate processing apparatus 20 of Fig. 1.
- the film thickness distribution obtained by ellipsometry for the film formed on the surface of the silicon substrate 22 was shown in Table 4.Table 4 shows the film obtained in this way at the center and the periphery of the substrate. The results of the film thickness obtained by setting the detection angle to 90 ° by the XPS method are shown.
- NO gas was supplied to the shear head 21 B at a flow rate of 200 SCCM, and the internal pressure of the processing vessel 21 was increased. Is maintained at 3.99 Pa (0.05 Torr) as in the previous case, and the ultraviolet light source 24B is driven at the reference intensity for 3 minutes.
- the substrate temperature is set at 450 ° C.
- a film with almost uniform thickness is formed on the surface of the silicon substrate. It can be seen that the edge is also about 0.5 nm.
- FIG. 12 (B) shows that the oxynitriding treatment was performed by setting the NO gas flow rate to 1 SLM and applying a UV light source 24 B to the reference intensity under a pressure of 665 Pa (5 Torr).
- Fig. 3 shows the film thickness distribution by ellipsometry when driving for 1 minute at.
- Table 5 shows the results of the film thickness measurement by the XPS method performed at a detection angle of 90 ° at the central portion and the peripheral portion of the substrate with respect to the film thus obtained. [Table 5]
- Fig. 12 (B) it can be seen that the film thickness distribution of the film formed on the substrate surface is almost uniform in this case as well. It can be seen that the thickness is about 0.5 nm both at the periphery and at the periphery.
- Table 6 below shows the results of elemental analysis performed by the XPS method on the film obtained by the experiment in FIG. 12 (A).
- the detection angle was set to 90 ° the oxygen atom concentration was 67.23%, the nitrogen atom concentration was 11.18%, and the silicon atom concentration was 21% at the center of the substrate. It was confirmed that it was 59%. Also at the substrate periphery, it was confirmed that the oxygen atom concentration was 6.6.88%, the nitrogen atom concentration was 9.13%, and the silicon atom concentration was 24.23%.
- the film thus formed is an oxynitride film containing nitrogen. It was confirmed that there was.
- Table 7 shows the results of elemental analysis by the XPS method on the film obtained by the experiment of FIG. 12 (B). [Table 7]
- FIGS. 13 (A;) and (B) show that in the substrate processing apparatus 20 of FIG. 1, NO gas is supplied to the shower head 21 B at a flow rate of 200 SCCM, and the processing pressure is reduced. 3.
- the thickness of the nitride film and the nitrogen concentration in the film are shown, respectively.
- FIG. 13 (A) the thickness of the oxynitride film increases with time, but when it reaches a thickness of about 0.5 nm, it is first described with reference to FIGS. 6 and 9. It can be seen that the same stopping phenomenon of film growth as in the above-mentioned case occurs.
- FIG. 13 (A) also shows a case where the ultraviolet light source 24B was not driven during such a nitriding treatment.
- Fig. 13 (B) shows that the oxynitride film with a high nitrogen concentration is formed immediately after the start of the nitriding treatment, but the nitrogen concentration in the film decreases with time, and the film growth mechanism increases with time. It can be seen that the reaction gradually shifted to the main oxidation reaction. Approximately 200 seconds after the start of processing, the unevenness of the nitrogen concentration in the film thickness direction is eliminated are doing.
- FIGS. 14 (A;) and (B) are diagrams corresponding to FIGS. 13 (A;) and (B), respectively, wherein the oxynitriding process is performed using the drive power of the ultraviolet light source 24B as the reference.
- the results are shown for the case where the intensity is set to 20% of the intensity, and the same results as in Figs. 13 (A) and (B) are obtained. That is, the film growth halting phenomenon occurs when the thickness of the oxynitride film reaches about 0.5 nm, and an oxynitride film having a high nitrogen concentration is formed at the beginning of the film growth, and the nitrogen atom Is concentrated near the interface between the oxynitride film and the silicon substrate.
- Figures 15 (A) and (B) show the film thickness and processing time when the same oxynitriding treatment of the silicon substrate surface was performed with the substrate temperature set to 550 ° C. , And the relationship between the distribution of nitrogen concentration in the film and the processing time.
- Fig. 15 (B) the concentration of nitrogen atoms incorporated in the film is shown when the detection angle in XPS analysis is set to 90 ° or 30 °. 13 (B) or FIG. 14 (B), which means that the formed oxynitride film has a composition closer to that of an oxide film. This is probably due to the fact that the substrate temperature during the oxynitriding process was set at 550 ° C., so that the oxidizing action by the oxygen remaining in the processing vessel 21 was promoted.
- the formed oxynitride film has a composition closer to the oxide film, so that the film growth stops, and the oxide film thickness stopping phenomenon described in FIGS. 6 and 9 occurs. It is considered that this occurs at a film thickness of about 0.46 nm, which is closer to 0.4 nm.
- the thickness of the oxynitride film is obtained by using the above-described equation (1) and the parameters associated therewith.
- this is an equation derived for the oxide film.
- the oxide film formed by the present invention is considered to have a thickness controlled to about two atomic layers.
- Figure 16 shows the potential curves for various excited states of the NO molecule.
- S. Chang / R. M. Hobson / Sumi Takakawa / Zu Kaneda “Atomic and molecular processes of ionized gas,” Tokyo Denki University Press [1982].
- atomic oxygen and atomic nitrogen can be generated by reducing NO molecules at a light wavelength of 145 nm or less.
- the light wavelength is shorter than the above-mentioned 1450 nm, radical oxygen (O ⁇ D ) starts to be excited, and it is considered that the oxidation reaction is mainly performed during the substrate processing.
- the ultraviolet light source 24B is required to be 192-145 nm. It is preferable to use a light source that can generate ultraviolet light of a range of wavelengths.
- a light source 24 B can be turned on and off at any time.
- excimer lamps with wavelengths of 300 nm, 222 nm, 170 nm, 146 nm, and 126 nm as ultraviolet light sources with sharp spectra are commercially available. Available. Of these lamps, the lamps that satisfy the above conditions are limited to those with a wavelength of 1 72 nm and 1 46 nm.
- the excimer lamp with a wavelength of 146 nm has a half-width of about 13 nm, so that a part of the spectrum is less than 145 nm, and the lamp state and individual differences This does not necessarily mean that oxygen radicals will not be excited. For this reason, when a commercially available excimer lamp is used as the ultraviolet light source 24B in the substrate processing apparatus 20 of FIG. 1, it is preferable to use a wavelength of 172 nm.
- FIG. 17 shows a schematic diagram of such an excimer lamp (dielectric barrier discharge tube) 41 for generating ultraviolet light of 172 nm (Japanese Patent Application Laid-Open No. 7-196303 or See Japanese Patent Application Laid-Open No. 8-858861).
- the excimer lamp 41 has a double cylindrical container including an inner tube 42 and an outer tube 43, and is provided between the inner quartz tube 42 and the outer quartz tube 43.
- the space 47 is filled with Xe gas at a pressure of 33.25 kPa (250 Torr). Further, an aluminum thin-film electrode 45 is formed on the inner side surface of the inner quartz tube 42, and a mesh electrode 44 is formed outside the outer quartz tube 43.
- a getter chamber 48 is formed at an axial end of the space 47, and a getter 46 is provided in the getter chamber 48.
- the excimer lamp 41 can control lighting and extinguishing by itself by applying an AC voltage between the electrode 44 and the electrode 45 by a power source 50.
- Such excimer lamps include, for example, a model UER20-172 sold by Shio Denki Co., Ltd., and a certain laser model HES17 sold by Hoyashott Co., Ltd. 0 3 S's can be used.
- the ultraviolet light source is not limited to the above-described excimer lamp, and it is also possible to use a low-pressure mercury lamp or an excimer laser in some cases.
- FIG. 20 (A) and (B) show the ratio between the measurement and the measurement at the detection angle of 30 ° (30 ° / 90 °).
- the silicon substrate held in the cassette chamber (63 in Fig. 3) that was evacuated passed through the transfer chamber (61) and the reaction chamber (20 ), And oxynitriding with UV-NO is performed.
- the cassette chamber which is evacuated is equipped with a mechanism for raising and lowering the cassette, the organic components emitted from these mechanical systems are likely to cause silicon substrate contamination due to long-term retention.
- the nitrogen concentration tends to increase when a wafer formed immediately after the silicon substrate is loaded is compared with a wafer formed by holding the cassette room for 3 to 24 hours.
- the ratio (30 ° Z 90 °) showed a decreasing tendency.
- Such a change in the film formation characteristics due to the holding in the cassette chamber greatly affects the device manufacturing process.
- nitrogen tends to be present inside the film, and segregation and segregation occur at the interface.
- UV after also performing preprocessing as UV-N 2 is also the plot of Figure 2 0 wafers were forcibly contaminated by holding for 24 hours - than those subjected to processing oxynitride NO, the concentration , Ratio (30 ° no 90 °) It can be seen that both were recovered to values close to the values plotted on the silicon substrate without holding time. This is presumed to be because the process was performed with the adsorbed organic molecules removed.
- FIGS. 18 (A) to 19 (E) show a manufacturing process of a semiconductor device according to a third embodiment of the present invention.
- a silicon substrate 31 with diffusion regions 31a and 31b formed by ion-implanting impurity elements is used to make holes in insulating layers 35 and 36.
- the exposed surface 31 C of the silicon substrate 31 from which the native oxide film has been removed, which is exposed by the substrate 37, has a wavelength of 17 2 under the conditions described above in the substrate processing apparatus 20 of FIG.
- FIG. 18 (B) the surface of the silicon substrate 31 is subjected to the film-deposition phenomena as described above, so that the film thickness is reduced. Is formed to a thickness of about 0.5 nm.
- a metal electrode layer 34 is deposited on the high dielectric film 33 thus formed in the step of FIG. 19 (D), and this is etched in the step of FIG. 19 (E).
- a metal gate electrode 34 G is formed by the treatment.
- the UV-NO oxynitriding step of FIG. 18 (A) is preferably performed at a temperature not exceeding 550 ° C., and the processing pressure at that time is 1.33 to: L.3. preferably set to 3 X 1 0- 3 P a.
- nitride film can be formed, and the stable film formation shown in the formation of an oxynitride film can be similarly performed in the form of an oxide film.
Description
Claims
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AU2003235305A AU2003235305A1 (en) | 2002-04-19 | 2003-04-21 | Method of treating substrate and process for producing semiconductor device |
US10/967,284 US7129185B2 (en) | 2002-04-19 | 2004-10-19 | Substrate processing method and a computer readable storage medium storing a program for controlling same |
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AU2003235305A1 (en) | 2003-11-03 |
US7129185B2 (en) | 2006-10-31 |
US20050079720A1 (en) | 2005-04-14 |
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