WO2010092757A1 - 原子層成長装置および薄膜形成方法 - Google Patents
原子層成長装置および薄膜形成方法 Download PDFInfo
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- WO2010092757A1 WO2010092757A1 PCT/JP2010/000482 JP2010000482W WO2010092757A1 WO 2010092757 A1 WO2010092757 A1 WO 2010092757A1 JP 2010000482 W JP2010000482 W JP 2010000482W WO 2010092757 A1 WO2010092757 A1 WO 2010092757A1
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- plasma
- emission intensity
- substrate
- thin film
- gas
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- 239000010409 thin film Substances 0.000 title claims description 42
- 238000000034 method Methods 0.000 title claims description 22
- 239000007789 gas Substances 0.000 claims abstract description 87
- 239000000758 substrate Substances 0.000 claims abstract description 59
- 230000001590 oxidative effect Effects 0.000 claims abstract description 32
- 229910052751 metal Inorganic materials 0.000 claims abstract description 30
- 239000002184 metal Substances 0.000 claims abstract description 30
- 239000001257 hydrogen Substances 0.000 claims abstract description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 18
- 238000005121 nitriding Methods 0.000 claims abstract description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000010408 film Substances 0.000 claims description 74
- 230000015572 biosynthetic process Effects 0.000 claims description 28
- 238000001514 detection method Methods 0.000 claims description 23
- 125000002524 organometallic group Chemical group 0.000 claims description 7
- 230000005540 biological transmission Effects 0.000 claims description 4
- 230000006698 induction Effects 0.000 claims 2
- 238000000231 atomic layer deposition Methods 0.000 description 20
- 238000007254 oxidation reaction Methods 0.000 description 12
- 239000001301 oxygen Substances 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- YZCKVEUIGOORGS-IGMARMGPSA-N Protium Chemical class [1H] YZCKVEUIGOORGS-IGMARMGPSA-N 0.000 description 6
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- 150000004767 nitrides Chemical class 0.000 description 5
- 238000005259 measurement Methods 0.000 description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 230000005404 monopole Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000000644 propagated effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 description 1
- 230000002123 temporal effect Effects 0.000 description 1
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- H01J37/32—Gas-filled discharge tubes
- H01J37/32917—Plasma diagnostics
- H01J37/32935—Monitoring and controlling tubes by information coming from the object and/or discharge
- H01J37/32972—Spectral analysis
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- 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]
- C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations
- C23C16/45536—Use of plasma, radiation or electromagnetic fields
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- 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]
- C23C16/45544—Atomic layer deposition [ALD] characterized by the apparatus
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- 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
- C23C16/52—Controlling or regulating the coating process
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- 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
- H01J37/32917—Plasma diagnostics
- H01J37/32935—Monitoring and controlling tubes by information coming from the object and/or discharge
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- 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
- H01J37/32917—Plasma diagnostics
- H01J37/3299—Feedback systems
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—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
- H01L21/02112—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
- H01L21/02172—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 at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides
- H01L21/02175—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 at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides characterised by the metal
- H01L21/02178—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 at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides characterised by the metal the material containing aluminium, e.g. Al2O3
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
- H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
- H01L21/02274—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition in the presence of a plasma [PECVD]
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
- H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
- H01L21/0228—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition deposition by cyclic CVD, e.g. ALD, ALE, pulsed CVD
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
- H01L22/10—Measuring as part of the manufacturing process
- H01L22/12—Measuring as part of the manufacturing process for structural parameters, e.g. thickness, line width, refractive index, temperature, warp, bond strength, defects, optical inspection, electrical measurement of structural dimensions, metallurgic measurement of diffusions
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- H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
- H01L22/20—Sequence of activities consisting of a plurality of measurements, corrections, marking or sorting steps
- H01L22/26—Acting in response to an ongoing measurement without interruption of processing, e.g. endpoint detection, in-situ thickness measurement
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02367—Substrates
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- H01L21/02104—Forming layers
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- H01L21/02612—Formation types
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Definitions
- the present invention relates to an atomic layer growth apparatus and a thin film forming method for forming a thin film by generating plasma using an oxidizing gas or a nitriding gas on a substrate on which an organic metal component containing hydrogen is adsorbed.
- ALD Advanced Layer Deposition
- a thin film is formed in units of atomic layers on a substrate.
- ALD atomic layer Deposition
- two kinds of gases mainly composed of elements constituting a film to be formed are alternately supplied onto a film formation target substrate, and a thin film is formed on the substrate in units of atomic layers.
- the formation of the atomic unit thin film is repeated a plurality of times to form a film having a desired thickness.
- a source gas made of TMA (Tri-Methyl Aluminum) and an oxidizing gas containing O are used.
- TMA Tri-Methyl Aluminum
- a nitriding gas is used instead of the oxidizing gas.
- the thin film formed by the ALD method has both high step coverage and film thickness controllability compared to a thin film formed by a general CVD (Chemical Vapor Deposition) method. Practical application to the formation of an insulating film called “gate” is expected. In addition, since an insulating film can be formed at a low temperature of about 300 ° C., application to the formation of a gate insulating film of a thin film transistor in a display device such as a liquid crystal display using a glass substrate is expected.
- Patent Document 1 describes plasma ALD of a tantalum nitride film.
- the generation time of the H 2 plasma pulse used for the reduction is set to 2000 to 4000 msec (see the document [0064]).
- the thickness and characteristics of the thin film such as the oxide film or the nitride film (dense density, withstand voltage)
- the refractive index) often varies in accordance with the density distribution of the generated plasma.
- the present invention can form a thin film so that the thickness and characteristics of the thin film such as an oxide film or a nitride film become uniform, and can efficiently form this thin film.
- An object is to provide an atomic layer growth apparatus and a thin film forming method.
- One embodiment of the present invention is an atomic layer growth apparatus for forming a thin film.
- the device is A substrate in which a plasma generation source that generates plasma by supplying high-frequency power using an oxidizing gas or a nitriding gas, and a substrate on which an organic metal component containing hydrogen is adsorbed are placed at a position facing the plasma generation source
- a film forming container in which a stage is disposed A light emission intensity detecting unit for detecting light emission intensity of a predetermined wavelength of light emitted on the substrate by the generation of the plasma through an observation window provided in the film forming container;
- a power control unit that stops the supply of high-frequency power from the plasma generation source when the value of the light emission intensity detected by the light emission intensity detection unit is equal to or less than a predetermined value.
- another embodiment of the present invention is a thin film forming method for forming a thin film.
- the method is Introducing an organometallic gas containing hydrogen into a film formation container to adsorb the organometallic component containing hydrogen on a substrate; Introducing an oxidizing gas or a nitriding gas into the film formation container to generate plasma, and oxidizing or nitriding the organometallic component adsorbed on the substrate; Detecting the emission intensity of a predetermined wavelength of light emitted on the substrate when the plasma is generated, through an observation window provided in the film formation container; Stopping the generation of plasma when the detected value of the emission intensity is equal to or lower than a predetermined value.
- the emission intensity of a predetermined wavelength of the light emitted on the substrate is detected through an observation window provided in the film formation container, and the detected emission intensity value is equal to or less than the predetermined value.
- the supply of high frequency power to the plasma generation source is stopped.
- the thin film is not formed unevenly corresponding to the generation density distribution of the plasma. That is, a thin film can be formed and the thin film can be efficiently formed so that the thickness and characteristics of the thin film are uniform.
- FIG. 1 It is the schematic showing the structure of the ALD apparatus which is one Example of the atomic layer growth apparatus of this invention. It is a figure explaining the antenna array and electric power feeding unit in the ALD apparatus shown in FIG. (A) is a graph which shows an example of the time change of the light intensity detected by a photon detection sensor, (b) is a graph which shows an example of the time change of reflected power.
- FIG. 1 is a schematic diagram showing the configuration of an ALD apparatus which is an embodiment of an atomic layer growth apparatus of the present invention.
- FIG. 2 is a diagram illustrating an antenna array and a power feeding unit in the ALD apparatus shown in FIG.
- the ALD apparatus 10 shown in FIG. 1 forms a thin film using an organic metal source gas containing hydrogen such as TMA (Tri-Methyl Aluminum) and an oxidizing gas containing O. At that time, the ALD apparatus 10 alternately supplies an organic metal source gas and an oxidizing gas onto the substrate 42 to be formed. When supplying an oxidizing gas, the ALD apparatus 10 generates a plasma using an oxidizing gas containing O to form a thin film of metal oxide on an atomic layer unit on the substrate in order to increase reaction activity. A thin film having a desired thickness is formed by repeating the above process for a plurality of cycles with the above process as one cycle. A nitriding gas can be used instead of the oxidizing gas. When TMA is used as an organic metal, an Al 2 O 3 thin film is formed on the substrate.
- TMA Tri-Methyl Aluminum
- the ALD apparatus 10 includes a power supply unit 11, a film forming container 12, gas supply units 14 and 15, and exhaust units 16 and 17 such as vacuum pumps.
- a power supply unit 11 a film forming container 12
- gas supply units 14 and 15 gas supply units 14 and 15, and exhaust units 16 and 17 such as vacuum pumps.
- exhaust units 16 and 17 such as vacuum pumps.
- the power supply unit 11 is a unit that supplies electric power (high-frequency signal) to each antenna element 26 of an antenna array (described later) provided in the film forming container 12.
- the power supply unit 11 includes a light detection sensor 11a, a control unit 11b, a reflected power measurement unit 11c, a power supply unit 34, and a distributor 36. As shown in FIG. 2, the distributor 36 supplies the high frequency signal generated by the power supply unit 34 to each antenna element 26. The length of the feed line from the distributor 13 to each antenna element 26 is the same.
- the gas supply unit 14 is connected via a supply pipe 18 to a supply hole 20 formed on one side wall (left wall in the figure) of the film forming container 12.
- the gas supply unit 14 supplies an organic metal gas having hydrogen as a source gas into the film forming container 12 in the horizontal direction through the supply pipe 18 and the supply hole 20.
- the gas supply unit 15 is connected to a supply hole 21 formed in the upper wall of the film forming container 12 through a supply pipe 19.
- the gas supply unit 15 supplies an oxidizing gas into the film forming container 12 in a direction perpendicular to the substrate via the supply pipe 19 and the supply hole 21.
- the supply of the source gas and the supply of the oxidizing gas are performed alternately.
- the gas supply unit 14 supplies an organic metal gas, which is a raw material gas, into the film forming container 12 via the supply pipe 18 and the supply hole 20, and the gas supply unit 15 supplies the supply pipe.
- the oxidizing gas is supplied into the film forming container 12 through the supply holes 19 and the supply holes 21.
- the gas supply unit 14 supplies the oxidizing gas into the film forming container 12 through the supply pipe 18 and the supply hole 20, and the gas supply unit 15 forms the film through the supply pipe 19 and the supply hole 21.
- An organic metal gas which is a raw material gas may be supplied into the container 12.
- the exhaust unit 16 is connected to an exhaust hole 24 formed in the right wall of the film forming container 12 through an exhaust pipe 22.
- the exhaust unit 16 exhausts the source gas and the oxidizing gas alternately supplied into the film forming container 12 through the exhaust hole 24 and the exhaust pipe 22 in the horizontal direction.
- the exhaust unit 17 evacuates the film formation container 12 in the vertical direction through the exhaust hole 25 and the exhaust pipe 23. The exhaust of the source gas and the exhaust of the oxidizing gas are performed alternately.
- an open / close valve for example, an electromagnetic valve
- an electromagnetic valve for controlling conduction between the gas supply units 14 and 15 and the film forming container 12
- an on-off valves for controlling the conduction between the exhaust parts 16 and 17 and the film formation container 12, respectively.
- the opening / closing valve of the supply pipe 18 is opened to supply the gas into the film forming chamber 28.
- the on-off valve of the supply pipe 19 is opened to supply the gas.
- the exhaust pipe 22 is opened and closed.
- the open / close valve of the exhaust pipe 23 is opened.
- the film formation container 12 has a metal hollow box shape and is grounded. Inside the film formation container 12, an antenna array comprising a metal plate shower head 29 having a plurality of holes of a predetermined diameter and a plurality of antenna elements 26 in order from the upper wall side to the lower wall side. A substrate stage 32 containing a heater 30 is disposed. The film forming container 12 and the shower head 29 are grounded. The antenna array is arranged so that a virtual plane on which the antenna elements 26 are arranged is parallel to the substrate stage 32.
- the shower head 29 is, for example, a rectangular metal member. As shown in FIG. 1, the shower head 29 is attached to the inner wall surface of the film formation container 12 between the upper wall of the film formation container 12 and the antenna array in parallel with the substrate stage 32.
- the plurality of holes formed in the shower head 29 are provided intermittently (at predetermined intervals) at positions on both sides (left and right in the figure) of each of the plurality of antenna elements 26.
- the plurality of holes have an elongated shape along the longitudinal direction (direction perpendicular to the paper surface in the drawing) of each of the plurality of antenna elements 26.
- the oxidizing gas supplied from the gas supply unit 15 into the film forming chamber 28 is diffused into a space between the upper wall of the film forming chamber 28 and the upper surface of the shower head 29, and then a plurality of gases formed in the shower head 29 are formed. Through the holes, the film is introduced (supplied) into the space below the shower head 29 from the upper side to the lower side of the film forming container 12.
- the antenna array generates plasma using oxidizing gas.
- the antenna array is located in the space between the shower head 29 and the substrate stage 32 between the left wall where the supply hole 20 is formed and the right wall where the exhaust hole 24 is formed. , Provided parallel to the surface of the substrate stage 32.
- a plurality of antenna elements 26 constituting the antenna array are arranged in parallel at regular intervals. Each of the plurality of antenna elements 26 is provided so as to be shifted in the lateral direction (left and right direction in FIG. 1) of the film formation container 12 so as not to come directly below the plurality of holes of the shower head 29 that supplies the oxidizing gas. ing.
- a high-frequency signal (high-frequency power) in the VHF band (for example, 80 MHz) generated by the power supply unit 34 is supplied to the distributor 36, and the high-frequency signal is divided in the distributor 36.
- These high-frequency signals are supplied to the protruding bases of the plurality of antenna elements 26 via the impedance matching unit 38.
- the impedance matching unit 38 adjusts an impedance mismatch caused by a change in the load of the antenna element 26 during the generation of plasma.
- the antenna element 26 includes a conductive rod-shaped monopole antenna (antenna main body) 39 such as copper, aluminum, or platinum housed in a cylindrical member 40 made of a dielectric such as quartz or ceramic. Has been. By covering the antenna body 39 with a dielectric, the capacity and inductance of the antenna are adjusted, and a high-frequency signal can be efficiently propagated along the longitudinal direction of the antenna body 39. Thereby, the antenna element 26 can efficiently radiate electromagnetic waves to the surroundings.
- a conductive rod-shaped monopole antenna antenna main body 39 such as copper, aluminum, or platinum housed in a cylindrical member 40 made of a dielectric such as quartz or ceramic.
- Each of the antenna elements 26 extends in a direction orthogonal to the flow direction of the source gas supplied from the supply hole 20 toward the substrate stage 32, and is electrically insulated so as to protrude from the side wall of the film forming container 12. It is attached to do.
- each of the antenna elements 26 is arranged in parallel at a constant interval, for example, 50 mm, and is provided such that the feeding positions between the adjacent antenna elements 26 are side walls facing each other.
- Each of the antenna elements 26 is disposed in a direction parallel to the substrate placement surface of the substrate stage 32. Further, the arrangement direction of the plurality of antenna elements 26 is a direction parallel to the substrate placement surface of the substrate stage 32.
- the antenna element 26 is configured, for example, by providing an antenna main body having a diameter of about 6 mm in a dielectric cylindrical member having a diameter of about 12 mm.
- the pressure in the film formation container 12 is about 20 Pa
- the antenna length of the antenna element 26 is (2n + 1) / 4 times the wavelength of the high-frequency signal (n is 0 or positive).
- the standing wave of the high-frequency signal is generated under the condition equal to the integer), and the antenna element 26 enters the resonance state. Thereby, electromagnetic waves are radiated around the antenna element 26 to generate plasma.
- the substrate stage 32 has an area smaller than the cross section of the space surrounded by the inner wall surface of the film formation container 12.
- the substrate stage 32 is a rectangular metal plate, for example, and is moved up and down by a lifting mechanism such as a power cylinder (not shown).
- a substrate 42 on which a thin film is formed is placed on the substrate stage 32.
- the power supply unit 11 includes a light detection sensor 11a, a control unit 11b, a reflected power measurement unit 11c, a power supply unit 34, and a distributor 36.
- An observation window 33 is formed of a transparent member such as quartz on the side wall of the film forming container 12 above the substrate 42 placed on the substrate stage 32.
- the light detection sensor 11 a is provided at a portion corresponding to the observation window 33 outside the film formation container 12.
- a band-pass filter that transmits light of a predetermined wavelength is provided on the front surface of the light receiving surface of the light detection sensor 11a. Thereby, the light detection sensor 11a is configured to receive light of a specific wavelength and detect the light emission intensity.
- the signal output from the light detection sensor 11a is sent to the control unit 11b.
- the band-pass filter has at least a wavelength band of 655.3 to 657.3 nm as a transmission band in order to mainly detect emission of hydrogen radicals at 656.3 nm.
- the reason why the observation window 33 is provided in the film formation container 12 to detect light having a predetermined wavelength is as follows. That is, oxygen radicals dissociated and generated from the oxidizing gas in the plasma react with organometallic molecules having hydrogen atoms adsorbed on the substrate 42, and the generated hydrogen radicals are excited in the plasma and emit specific light. To do.
- the light detection sensor 11a detects the emitted light, and the detection result is used for controlling the generation of plasma.
- the light emission of the hydrogen radical occurs when the oxygen radical reacts with the organic metal component, so that the progress of the oxidation reaction of the metal can be known by detecting the light emission of the hydrogen radical and examining the change in the intensity of the light.
- the oxidation reaction ends, the oxidation no longer proceeds on the substrate even if oxygen radicals are supplied. For this reason, it is not necessary to continue the generation of plasma thereafter. Continuing the generation of plasma increases the possibility that the oxide film formed by the plasma will be damaged. Therefore, the power supply unit 11 can know the progress of the oxidation reaction by detecting the emission intensity of the hydrogen radical, and controls the generation of the plasma to end when the progress of the oxidation reaction ends.
- the reflected power measurement unit 11 c measures the reflected power reflected by the antenna element 26 by measuring the voltage and current of the high-frequency signal from the power supply unit 34. The measured reflected power is sent to the control unit 11b.
- the reason for measuring the reflected power is to know the start time of plasma generation by supplying high-frequency power. The generation of plasma does not immediately start with the supply of high-frequency power, but plasma is generated when the reflected power decreases due to resonance. At that time, the time until resonance varies. Accordingly, the power supply unit 11 knows the timing of starting the generation of the plasma, and starts detecting the value of the light emission intensity by the light detection sensor 11a on the basis of the time when the reflected power becomes equal to or lower than a preset value.
- the controller 11b determines the generation start time of such plasma, starts detection of the light emission intensity value by the light detection sensor 11a, and performs control to stop the supply of the high-frequency signal according to the detection result of the light emission intensity.
- the power supply unit 34 is a part that generates a high-frequency signal such as 80 MHz in accordance with an instruction from the control unit 11b.
- FIG. 3A is a graph illustrating an example of a temporal change in emission intensity detected by the light detection sensor 11a.
- supply of a high-frequency signal to the antenna element 26 is started, and then plasma is generated, and light emission by hydrogen radicals starts at T 1 second. That is, the oxidation reaction starts.
- the emission intensity reaches a peak (emission intensity Pmax at the peak)
- the emission intensity crosses a threshold value determined by ⁇ times the emission intensity Pmax ( ⁇ is a predetermined value greater than 0 and less than 1) for T 2 seconds.
- the reflected power is approximately T 1 seconds, and the reflected power is equal to or less than a preset value.
- the control unit 11b detects the light intensity of the light detection sensor 11a and supplies power to the power supply unit 34 with T 1 second as the start time of the oxidation reaction and T 2 seconds as the end time of the oxidation reaction.
- the plasma generation time is (T 2 -T 1 ) seconds.
- the plasma generation time (T 2 -T 1 ) seconds is It is about several tens of milliseconds. This plasma generation time is extremely short compared to the plasma generation time fixed to several hundred milliseconds to several seconds as in the prior art.
- the ALD apparatus 10 forms a thin film having a desired thickness by repeatedly forming the oxidized thin film in units of atomic layers.
- the progress of the oxidation reaction can be known by the emission of hydrogen radicals using the light detection sensor 11a, the state where the oxidation reaction is completed can be known.
- the thin film formed on the substrate is not exposed to plasma unnecessarily for a long time, the film thickness and characteristics of the thin film become uniform compared to the conventional case. Furthermore, since unnecessary plasma generation time is eliminated, the thin film can be formed efficiently in a short time.
- an organic metal gas containing hydrogen is introduced from the gas supply unit 14 into the film formation container 12 to adsorb the organic metal component on the substrate 42. Thereafter, the ALD apparatus 10 introduces an oxidizing gas containing O into the film forming container 12 from the gas supply unit 15 and simultaneously supplies power to the antenna element 26 to generate plasma. Using the oxygen radicals generated thereby, the organic metal component adsorbed on the substrate is oxidized. When plasma is generated and an oxidation reaction occurs, hydrogen radicals are generated on the substrate. It emits light when this hydrogen radical is excited and stabilized. The light emission intensity is detected by the light detection sensor 11 a through the observation window 33 provided in the film formation container 12.
- the control unit 11b stops the supply of power from the power supply unit 34 so that the generation of plasma is stopped when the detected value of the emission intensity is equal to or less than a predetermined value. Note that when the organic metal gas and the oxidizing gas are alternately replaced and flowed, it is preferable that the gas in the film formation chamber 28 is accurately replaced by flowing an inert gas or the like when the gas is replaced.
- the reflected power is measured, and detection of the value of the emission intensity is started on the basis of the time when the reflected power becomes equal to or lower than a preset value.
- the emission intensity is detected using a bandpass filter including 655.3 to 657.3 nm as a transmission band.
- the metal oxide film is formed using an oxidizing gas
- the present invention can also be applied when a metal is nitrided using a nitriding gas instead of the oxidizing gas.
- the plasma can be generated using an inductively coupled or capacitively coupled generation source instead of the electromagnetic coupling type using an antenna as a plasma generation source. That is, there is no particular limitation as long as it is an apparatus that generates plasma.
- the atomic layer growth apparatus and the thin film formation method of the present invention have been described in detail.
- the atomic layer growth apparatus and the thin film formation method of the present invention are not limited to the above-described embodiments, and do not depart from the spirit of the present invention.
- various improvements and changes may be made.
- ALD apparatus 11 Feeding unit 11a Light detection sensor 11b Control part 11c Reflected power measurement part 12 Film-forming container 14,15 Gas supply part 16,17 Exhaust part 22,23 Supply pipe 24,25 Exhaust hole 26 Antenna element 28 Film Forming Room 29 Shower Head 30 Heater 32 Substrate Stage 38 Impedance Matching Device 39 Monopole Antenna 42 Substrate 40 Cylindrical Member
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Abstract
Description
例えば、下記特許文献1には、窒化タンタル膜のプラズマALDが記載されている。当該文献1では、還元のために用いるH2プラズマパルスの発生時間は、2000~4000m秒に固定されて設定されている(当該文献[0064]参照)。
当該装置は、
酸化ガスあるいは窒化ガスを用いて、高周波電力の供給によりプラズマを発生させるプラズマ発生源と、このプラズマ発生源に対向する位置に、水素を含む有機金属の成分を吸着した基板が載置される基板ステージとが配設された成膜容器と、
前記プラスマの発生によって前記基板上で発光する光の所定の波長の発光強度を、成膜容器に設けられた観測窓を通して検出する発光強度検出部と、
前記発光強度検出部で検出した発光強度の値が所定値以下になるとき、前記プラズマ発生源の高周波電力の供給を停止する電力制御部と、を有する。
当該方法は、
成膜容器内に水素を含む有機金属ガスを導入して、基板上に水素を含む前記有機金属の成分を吸着させるステップと、
前記成膜容器内に酸化ガスまたは窒化ガスを導入してプラズマを発生し、基板に吸着した前記有機金属の成分を酸化または窒化させるステップと、
前記プラズマを発生させたとき、前記基板上で発光する光の所定の波長の発光強度を、成膜容器に設けられた観測窓を通して検出するステップと、
検出した前記発光強度の値が所定値以下になるとき、プラズマの発生を停止するステップと、を有する。
図1は、本発明の原子層成長装置の一実施例であるALD装置の構成を表す概略図である。図2は、図1に示すALD装置におけるアンテナアレイと給電ユニットを説明する図である。
図2に示すように、分配器36は、電力供給部34で生成された高周波信号を各アンテナ素子26に供給する。分配器13から各アンテナ素子26にいたる給電線の長さは同じである。
なお、本実施形態では、ガス供給部14が、供給管18および供給孔20を介して、成膜容器12内に原料ガスである有機金属のガスを供給し、ガス供給部15が、供給管19および供給孔21を介して、成膜容器12内に酸化ガスを供給する。しかし、ガス供給部14が、供給管18および供給孔20を介して、成膜容器12内に酸化ガスを供給し、ガス供給部15が、供給管19および供給孔21を介して、成膜容器12内に原料ガスである有機金属のガスを供給してもよい。
また、アンテナ素子26のそれぞれは、基板ステージ32の基板載置面と平行な方向に配置される。さらに、複数のアンテナ素子26の配列方向は基板ステージ32の基板載置面と平行な方向である。
基板ステージ32は、成膜容器12の内壁面で囲まれる空間の断面よりも小さい面積を有する。基板ステージ32は、例えば矩形の金属板であり、図示されないパワーシリンダ等の昇降機構により上下に昇降される。基板ステージ32には、薄膜を形成する基板42が載置される。
基板ステージ32に載置された基板42の上方の、成膜容器12の側壁には、石英等の透明部材により観測窓33が設けられている。
光検出センサ11aは、成膜容器12の外側の、観測窓33に対応する部分に設けられている。光検出センサ11aの受光面の前面には、所定の波長の光を透過するバンドパスフィルタが設けられている。これにより、光検出センサ11aは、特定の波長の光を受光して発光強度を検出するように構成されている。光検出センサ11aで出力した信号は、制御部11bに送られる。バンドパスフィルタは、656.3nmの水素ラジカルの発光を主に検出するために、655.3~657.3nmの波長帯域を少なくとも透過帯域とする。
すなわち、プラズマ中で酸化ガスから解離生成した酸素ラジカルが、基板42上に吸着した水素原子を有する有機金属分子と反応し、その際に生成する水素ラジカルがプラズマ中で励起され特定の光を放出する。光検出センサ11aはこの放出した光を検出し、この検出結果がプラズマの発生の制御に用いられる。
電力供給部34は、制御部11bの指示に応じて、例えば、80MHz等の高周波信号を生成する部分である。
制御部11bは、このようなとき、T1秒を酸化反応の開始時期とし、T2秒を酸化反応の終了時期として、光検出センサ11aの光強度の検出および電力供給部34の電力の供給を制御する。
上記例において、プラズマ発生時間は(T2-T1)秒であり、例えばαを1/e(eは、自然対数の底)としたとき、プラズマ発生時間(T2-T1) 秒は略数10m秒である。このプラズマ発生時間は、従来のような数100m秒~数秒に固定されたプラズマ発生時間に比べて極めて短い。
上記実施形態では、光検出センサ11aを用いて酸化反応の進行を、水素ラジカルの発光により知ることができるので、酸化反応が終了した状態を知ることができる。また、基板に形成された薄膜は、プラズマに不必要に長時間晒されないので、薄膜の膜厚および特性が従来に比べて均一になる。さらに、不必要なプラズマ発生時間がなくなるので薄膜の形成を短時間に効率よく行うことができる。
プラズマが発生し、酸化反応が発生したとき、基板上で水素ラジカルが発生する。この水素ラジカルが励起され安定化するとき発光する。この光の発光強度が、成膜容器12に設けられた観測窓33を介して光検出センサ11aで検出される。制御部11bは、検出した発光強度の値が所定値以下になるとき、プラズマの発生を停止するように、電力供給部34からの電力の供給を停止する。なお、有機金属のガスおよび酸化ガスを交互に置換して流すとき、ガスの置換時、不活性ガス等を流すことにより成膜室28内のガスを正確に入れ替えるようにするとよい。
さらに、プラズマの発生は、プラズマ発生源としてアンテナを用いる電磁波結合型の替わりに、誘導結合型あるいは容量結合型の発生源を用いて行うこともできる。すなわち、プラズマを発生させる装置であれば特に制限されない。
11 給電ユニット
11a 光検出センサ
11b 制御部
11c 反射電力計測部
12 成膜容器
14,15 ガス供給部
16,17 排気部
22,23 供給管
24,25 排気孔
26 アンテナ素子
28 成膜室
29 シャワーヘッド
30 ヒータ
32 基板ステージ
38 インピーダンス整合器
39 モノポールアンテナ
42 基板
40 円筒部材
Claims (8)
- 薄膜を形成する原子層成長装置であって、
酸化ガスあるいは窒化ガスを用いて、高周波電力の供給によりプラズマを発生させるプラズマ発生源と、このプラズマ発生源に対向する位置に、水素を含む有機金属の成分を吸着した基板が載置される基板ステージとが配設された成膜容器と、
前記プラスマの発生によって前記基板上で発光する光の所定の波長の発光強度を、成膜容器に設けられた観測窓を通して検出する発光強度検出部と、
前記発光強度検出部で検出した発光強度の値が所定値以下になるとき、前記プラズマ発生源の高周波電力の供給を停止する電力制御部と、を有することを特徴とする原子層成長装置。 - 前記電力制御部は、前記プラズマ発生源に供給する高周波電力の反射電力を計測し、反射電力が予め設定された値以下になった時点を基準として、前記発光強度の値の検出を開始する、請求項1に記載の原子層成長装置。
- 前記発光強度検出部は、655.3~657.3nmを透過帯域として含むバンドパスフィルタを用いて発光強度を検出する、請求項1または2に記載の原子層成長装置。
- 前記プラズマ発生源は、アンテナ、誘導電極、または平行平板電極である、請求項1~3のいずれか1項に記載の原子層成長装置。
- 薄膜を形成する薄膜形成方法であって、
成膜容器内に水素を含む有機金属ガスを導入して、基板上に水素を含む前記有機金属の成分を吸着させるステップと、
前記成膜容器内に酸化ガスまたは窒化ガスを導入してプラズマを発生し、基板に吸着した前記有機金属の成分を酸化または窒化させるステップと、
前記プラズマを発生させたとき、前記基板上で発光する光の所定の波長の発光強度を、成膜容器に設けられた観測窓を通して検出するステップと、
検出した前記発光強度の値が所定値以下になるとき、プラズマの発生を停止するステップと、を有することを特徴とする薄膜形成方法。 - 前記発光強度を検出するとき、プラズマを発生させるプラズマ発生源に高周波電力を供給するときの反射電力を計測し、この反射電力が予め設定された値以下になった時点を基準として、前記発光強度の値の検出を開始する、請求項5に記載の薄膜形成方法。
- 前記発光強度を検出するとき、655.3~657.3nmを透過帯域として含むバンドパスフィルタを用いて発光強度を検出する、請求項5または6に記載の薄膜形成方法。
- 前記プラズマの発生は、アンテナ、誘導電極、または平行平板電極のプラズマ発生源を用いて行う、請求項5~7のいずれか1項に記載の薄膜形成方法。
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JP2010186885A (ja) | 2010-08-26 |
KR101314582B1 (ko) | 2013-10-07 |
EP2398042A4 (en) | 2015-08-12 |
EP2398042A1 (en) | 2011-12-21 |
US20110293854A1 (en) | 2011-12-01 |
TWI512132B (zh) | 2015-12-11 |
KR20110116043A (ko) | 2011-10-24 |
JP4575984B2 (ja) | 2010-11-04 |
EP2398042B1 (en) | 2016-10-12 |
TW201035361A (en) | 2010-10-01 |
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