CN111074235A - Air inlet device, air inlet method and semiconductor processing equipment - Google Patents
Air inlet device, air inlet method and semiconductor processing equipment Download PDFInfo
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- CN111074235A CN111074235A CN201811223387.1A CN201811223387A CN111074235A CN 111074235 A CN111074235 A CN 111074235A CN 201811223387 A CN201811223387 A CN 201811223387A CN 111074235 A CN111074235 A CN 111074235A
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- reaction chamber
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- air inlet
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- 238000000034 method Methods 0.000 title claims abstract description 60
- 239000004065 semiconductor Substances 0.000 title claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 119
- 238000006243 chemical reaction Methods 0.000 claims abstract description 117
- 239000000758 substrate Substances 0.000 claims abstract description 28
- 239000007789 gas Substances 0.000 claims description 121
- 239000001301 oxygen Substances 0.000 claims description 39
- 229910052760 oxygen Inorganic materials 0.000 claims description 39
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 36
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 25
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 238000000605 extraction Methods 0.000 claims description 10
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000003446 ligand Substances 0.000 abstract description 11
- 230000008569 process Effects 0.000 description 41
- 239000010408 film Substances 0.000 description 33
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 description 22
- 150000002500 ions Chemical class 0.000 description 22
- 239000012159 carrier gas Substances 0.000 description 21
- 229910000449 hafnium oxide Inorganic materials 0.000 description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 16
- 229910052735 hafnium Inorganic materials 0.000 description 15
- 238000010926 purge Methods 0.000 description 15
- NPEOKFBCHNGLJD-UHFFFAOYSA-N ethyl(methyl)azanide;hafnium(4+) Chemical group [Hf+4].CC[N-]C.CC[N-]C.CC[N-]C.CC[N-]C NPEOKFBCHNGLJD-UHFFFAOYSA-N 0.000 description 13
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 12
- -1 hafnium ions Chemical class 0.000 description 12
- 239000010409 thin film Substances 0.000 description 8
- ZYLGGWPMIDHSEZ-UHFFFAOYSA-N dimethylazanide;hafnium(4+) Chemical compound [Hf+4].C[N-]C.C[N-]C.C[N-]C.C[N-]C ZYLGGWPMIDHSEZ-UHFFFAOYSA-N 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- CRHIBFCNJROORF-UHFFFAOYSA-N hafnium(4+);methylazanide Chemical compound [Hf+4].[NH-]C.[NH-]C.[NH-]C.[NH-]C CRHIBFCNJROORF-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000013110 organic ligand Substances 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 150000001450 anions Chemical class 0.000 description 2
- 238000000231 atomic layer deposition Methods 0.000 description 2
- VBCSQFQVDXIOJL-UHFFFAOYSA-N diethylazanide;hafnium(4+) Chemical compound [Hf+4].CC[N-]CC.CC[N-]CC.CC[N-]CC.CC[N-]CC VBCSQFQVDXIOJL-UHFFFAOYSA-N 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 125000002147 dimethylamino group Chemical group [H]C([H])([H])N(*)C([H])([H])[H] 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000005649 metathesis reaction Methods 0.000 description 1
- 125000000250 methylamino group Chemical group [H]N(*)C([H])([H])[H] 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Classifications
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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
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
-
- 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]
- C23C16/45527—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
- C23C16/45542—Plasma being used non-continuously during the ALD reactions
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Metallurgy (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- Plasma & Fusion (AREA)
- Electromagnetism (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
- Formation Of Insulating Films (AREA)
Abstract
The invention provides an air inlet device, an air inlet method and semiconductor processing equipment, which comprise a first air inlet pipeline for introducing a first precursor into a reaction chamber, and further comprise a plasma generator and a second air inlet pipeline, wherein the plasma generator is connected with the reaction chamber through the second air inlet pipeline and used for providing plasma for the reaction chamber, and the plasma can react with the first precursor and form a required film on the surface of a substrate. The gas inlet device, the gas inlet method and the semiconductor processing equipment provided by the invention can reduce ligand vacancies in the first precursor, thereby improving the density of the film and improving the quality and the electrical property of the film.
Description
Technical Field
The invention relates to the technical field of semiconductor processing, in particular to an air inlet device, an air inlet method and semiconductor processing equipment.
Background
With the development of semiconductor technology, the feature linewidth in the conventional silicon-based Complementary Metal Oxide Semiconductor (CMOS) integration technology has been reduced from the original micrometer level to the nanometer level, and silicon dioxide as an excellent gate dielectric layer material cannot meet the requirements of semiconductor devices on dielectric layers, so that people look to dielectric layer materials with high dielectric constants. Due to hafnium oxide (HfO)2) The hafnium oxide has the characteristics of high dielectric constant, large forbidden bandwidth, moderate valence band and conduction band offset, good thermal stability and the like, so that the hafnium oxide becomes a good high-dielectric-constant material for replacing a silicon dioxide dielectric layer. And the film prepared by the atomic layer deposition technology has the advantages of controllable thickness height, excellent uniformity, high step coverage rate and the like. Therefore, with the trend of feature line width reduction, the ald hafnium oxide process is receiving more and more attention.
In the existing atomic layer deposition hafnium oxide process, tetrakis (dimethylamino) hafnium (TDMAH) is generally used as the hafnium source, and water (H) is used2O) as an oxygen source, first introducing water into the reaction chamber to adsorb it on the substrate surface, and then introducing tetrakis (dimethylamino) hafnium into the reaction chamber to react with the water adsorbed on the substrate surface, thereby combining the hafnium source organic ligand with the oxygen in the water to deposit hafnium oxide on the substrate surface.
However, in the process of depositing hafnium oxide by reacting hafnium tetra (dimethylamino) and water, part of the hafnium source organic ligands cannot fully react with water due to steric hindrance, so that the hafnium source organic ligands cannot be combined with oxygen in water, a large number of oxygen vacancies are generated, the density of the film is reduced, and the electrical properties of the hafnium oxide film, such as leakage current density, breakdown voltage and the like, are affected.
Disclosure of Invention
The invention aims to at least solve one of the technical problems in the prior art, and provides a gas inlet device, a gas inlet method and semiconductor processing equipment, which can reduce ligand vacancies in a first precursor, thereby improving the compactness of a film and improving the quality and the electrical property of the film.
The gas inlet device comprises a first gas inlet pipeline for introducing a first precursor into a reaction chamber, and further comprises a plasma generator and a second gas inlet pipeline, wherein the plasma generator is connected with the reaction chamber through the second gas inlet pipeline and is used for providing plasma to the reaction chamber, and the plasma can react with the first precursor and form a required thin film on the surface of a substrate.
Preferably, the apparatus further comprises a third gas inlet pipeline, and the third gas inlet pipeline is used for introducing the second precursor into the reaction chamber.
Preferably, the air extractor further comprises an air extracting device and an air extracting pipeline, and two ends of the air extracting pipeline are respectively connected with the air extracting device and the second air inlet pipeline; the air exhaust device is connected with the reaction chamber.
Preferably, the system further comprises a first precursor source bottle, a first connecting pipeline and a first source bottle air inlet pipeline, wherein the first precursor source bottle is connected with the reaction chamber through the first air inlet pipeline;
two ends of the first connecting pipeline are respectively connected with the first source bottle air inlet pipeline and the first air inlet pipeline;
and on-off valves are arranged on the first connecting pipeline, the first source bottle air inlet pipeline and the first air inlet pipeline.
Preferably, the system further comprises a second precursor source bottle, a second connecting pipeline and a second source bottle air inlet pipeline, wherein the second precursor source bottle is connected with the reaction chamber through the third air inlet pipeline;
two ends of the second connecting pipeline are respectively connected with the second source bottle air inlet pipeline and the third air inlet pipeline;
and on-off valves are arranged on the second connecting pipeline, the second source bottle air inlet pipeline and the third air inlet pipeline.
Preferably, the gas used to provide the plasma comprises one or more of oxygen, ozone and nitric oxide mixed with argon or nitrogen.
Preferably, on-off valves are arranged on the second air inlet pipeline and the air suction pipeline.
The invention also provides a gas inlet method, which adopts the gas inlet device to introduce the first precursor and the plasma into the reaction chamber and comprises the following steps:
introducing the first precursor into the reaction chamber through the first gas inlet pipeline;
and forming plasma through the plasma generator, and introducing the plasma into the reaction chamber through the second air inlet pipeline.
Preferably, the gas inlet device further comprises a third gas inlet pipeline, and the third gas inlet pipeline is connected with the reaction chamber;
before the step of introducing the first precursor into the reaction chamber through the first gas inlet pipe, the method further comprises the following steps: and introducing a second precursor into the reaction chamber through the third gas inlet pipeline.
The invention also provides semiconductor processing equipment which comprises a reaction chamber and the gas inlet device, so that the first precursor and the plasma are introduced into the reaction chamber.
The invention has the following beneficial effects:
the gas inlet device comprises a first gas inlet pipeline, a plasma generator and a second gas inlet pipeline, wherein the first gas inlet pipeline is used for introducing a first precursor into a reaction chamber, the plasma generator is used for forming plasma and is connected with the reaction chamber through the second gas inlet pipeline so as to provide the plasma for the reaction chamber, ions in the plasma and ions in the first precursor are mutually attracted and combined by virtue of the ions in the plasma with opposite charges, and the first precursor is fully reacted, so that ligand vacancies in the first precursor are reduced, the density of a required film formed on the surface of the substrate is improved, and the quality and the electrical performance of the film are improved.
According to the gas inlet method provided by the invention, with the aid of the gas inlet device provided by the invention, a first precursor is introduced into the reaction chamber through the first gas inlet pipeline; and forming plasma through a plasma generator, introducing the plasma into the reaction chamber through a second gas inlet pipe, and making the ions in the plasma and the ions in the first precursor mutually attract and combine by virtue of the ions in the plasma with opposite charges to the ions in the first precursor, so that the first precursor is fully reacted, thereby reducing ligand vacancies in the first precursor, further improving the density of a required film formed on the surface of the substrate, and improving the quality and the electrical property of the film.
The semiconductor processing equipment provided by the invention comprises a reaction chamber and the gas inlet device provided by the invention, and ions in the plasma and ions in the first precursor are mutually attracted and combined by virtue of the ions with opposite charges in the plasma and the ions in the first precursor, so that the first precursor is fully reacted, ligand vacancies in the first precursor are reduced, the density of a required film formed on the surface of a substrate is further improved, and the quality and the electrical property of the film are improved.
Drawings
FIG. 1 is a schematic structural diagram of a semiconductor processing apparatus according to the present invention;
FIG. 2 is a block flow diagram of an air induction method provided by the present invention;
FIG. 3 is another block flow diagram of the air induction method provided by the present invention;
description of reference numerals:
1-a reaction chamber; 2-a substrate; 31-a first intake line; 32-a first source bottle inlet line; 33-a first precursor source bottle; 34-a first connection line; 41-a plasma generator; 42-a second intake line; 51-an air extraction device; 52-a suction line; 61-third intake line; 62-a second source bottle inlet line; 63-a second precursor source bottle; 64-second connecting line.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the gas inlet device, the gas inlet method and the semiconductor processing equipment provided by the present invention are described in detail below with reference to the accompanying drawings.
The embodiment provides a gas inlet device, which comprises a plasma generator 41, a second gas inlet pipeline 42 and a first gas inlet pipeline 31 for introducing a first precursor into a reaction chamber 1, wherein the plasma generator 41 is connected with the reaction chamber 1 through the second gas inlet pipeline 42 and is used for providing plasma to the reaction chamber 1, and the plasma can react with the first precursor and form a desired thin film on the surface of a substrate 2.
In the air inlet device provided by the embodiment, the ions in the plasma and the ions in the first precursor are attracted and combined with each other by virtue of the ions in the plasma, which have opposite charges with respect to the ions in the first precursor, so that the first precursor is fully reacted, and therefore, ligand vacancies in the first precursor are reduced, the density of a required film formed on the surface of the substrate 2 is further improved, and the quality and the electrical property of the film are improved.
The gas inlet apparatus provided in this embodiment is described below by taking the process of preparing hafnium oxide thin film as an example, wherein the first precursor is tetra (methylethylamino) hafnium (TEMAH, Hf [ N (C)2H5CH3)2]4) The plasma generator 41 is used to form oxygen plasma, and the gas for supplying the oxygen plasma is a gas including one or more of oxygen, ozone, and nitric oxide, and mixed with argon gas or nitrogen gas. Before the process is started, the substrate 2 is placed in the reaction chamber 1, then the tetra (methylamino) hafnium is introduced into the reaction chamber 1 through the first air inlet pipeline 31 to be adsorbed on the surface of the substrate 2, then the gas which comprises one or more of oxygen, ozone and nitric oxide and is mixed with argon or nitrogen is introduced into the plasma generator, the plasma generator is ionized to form the oxygen plasma, the oxygen plasma is introduced into the reaction chamber 1 through the second air inlet pipeline 42 to be adsorbed on the surface of the substrate 2 to be subjected to the generation of the tetra (methylamino) hafniumReact to form a hafnium oxide thin film on the surface of the substrate 2.
Specifically, tetrakis (methylamino) hafnium (Hf [ N (C) ]2H5CH3)2]4) From hafnium ions (Hf)4+) With ligands ([ N (C) ]2H5CH3)2]-) The oxygen plasma contains oxygen ions (O)2-) Because the oxygen ions are anions with negative charges, the hafnium ions are oxygen ions with positive charges, and the hafnium ions can be more effectively replaced from the tetra (methylethylamino) hafnium through the mutual attraction between the anions and cations with opposite charges, namely, the tetra (methylethylamino) hafnium and the oxygen plasma have replacement reaction, so that more hafnium oxides are formed in unit area, namely, the density of the hafnium oxides is improved, namely, ligand vacancies in the tetra (methylethylamino) hafnium are reduced, further, the density of the required film formed on the surface of the substrate 2 is improved, and the quality and the electrical performance of the film are improved.
In practical application, the first precursor in the process of preparing the hafnium oxide film may also be tetrakis (dimethylamino) hafnium (TDMAH) or tetrakis (diethylamino) hafnium (TDEAH). The argon or nitrogen in the gas used to provide the oxygen plasma is primarily used to ignite in the plasma generator 41 to form one or more of oxygen, ozone and nitric oxide into an oxygen plasma.
In this embodiment, the gas inlet device further comprises a third gas inlet pipe 61, and the third gas inlet pipe 61 is used for introducing the second precursor into the reaction chamber 1. Specifically, the second precursor can also react with the first precursor to form a required film, and the second precursor is introduced into the reaction chamber 1 to act together with the plasma, so that the first precursor reacts more fully.
Still taking the process of preparing hafnium oxide film by using hafnium tetra (methylethylamino) as the first precursor as an example to explain the function of the third gas inlet pipe 61 in the gas inlet device, in the process, the second precursor is introduced into the reaction chamber 1 as the oxygen source through the third gas inlet pipe 61, so that the oxygen in the second precursor reacts with the hafnium in the first precursor and reacts with the effect of the plasmaSimilarly, in the process of reacting the first precursor with the plasma, the second precursor is added, so that the first precursor can react more fully, and the compact hafnium oxide film can be formed. Water (H) is added below2O) as a second precursor. Before introducing the hafnium tetra (methylethylamino) into the reaction chamber 1, introducing H into the reaction chamber 1 through a third gas inlet pipeline 612O, to H2O is adsorbed on the surface of the substrate 2, and then tetrakis (methylethylamino) hafnium is introduced into the reaction chamber 1 through the first gas inlet pipe 31, so that tetrakis (methylethylamino) hafnium and H adsorbed on the surface of the substrate 2 are reacted2O reacts to form hafnium oxide, and oxygen plasma is introduced into the reaction chamber 1 through the plasma generator 41 and the second gas inlet pipeline 42, and the oxygen plasma and H on the surface of the substrate 22And reacting the reacted tetra (methylethylamino) hafnium with O to form a compact hafnium oxide film.
In particular, in tetrakis (methylamino) hafnium (Hf [ N (C) ]2H5CH3)2]4) Due to the ligand [ N (C)2H5CH3)2]-Large, block H2Diffusion of O to Hf4+And [ N (C)2H5CH3)2]-A joint of (2), block H2O is subjected to a metathesis reaction with hafnium tetra (methylethylamino)2-Hf with negative and positive charges4+Combined while [ N (C2H5CH3)2]-And H2Positively charged holes in O combine to make H2And the O and the hafnium tetra (methylethylamino) are fully reacted to form a compact hafnium oxide film, so that the film quality is improved.
In practical application, the second precursor as the oxygen source may also adopt oxygen (O)2) And ozone (O)3) And the like. The number of first intake lines 31 and third intake lines 61 may be plural. In addition, a second precursor (H)2The order of introducing O) and hafnium tetra (methylethylamino) into the reaction chamber 1 may be first introducing hafnium tetra (methylethylamino) and then introducing H2O, but preference is given to using a first H feed2Mode of O due to H2O is more easily adsorbed uniformly on the surface of the substrate 2On the face.
In this embodiment, the gas inlet device further includes a gas extractor 51 and a gas extraction pipeline 52, two ends of the gas extraction pipeline 52 are respectively connected with the gas extractor 51 and the second gas inlet pipeline 42, the plasma generated by the plasma generator 41 can be extracted into the gas extractor 51 through the gas extraction pipeline 52 by the gas extractor 51, so that when the first precursor or the second precursor is introduced into the reaction chamber 1, the gas for forming the plasma is introduced into the plasma generator 41 to form stable plasma, and the plasma enters the gas extractor 51 through the gas extraction pipeline 52, thereby preventing the substrate 2 from reacting with the plasma when the substrate 2 is not saturated to adsorb the first precursor, which affects the film quality, and when the plasma needs to be introduced into the reaction chamber 1, the stable plasma can be introduced into the reaction chamber 1 through the second gas inlet pipeline 42, therefore, the plasma meeting the process requirement can be introduced into the reaction chamber 1 within a short time, and the plasma is uniformly distributed in the reaction chamber 1, so that the process time is shortened, and the film quality is improved.
In practical applications, on-off valves may be disposed on both the second air inlet line 42 and the pumping line 52 to control the plasma to enter the reaction chamber 1 or the pumping device 51, and when the on-off valve disposed on the second air inlet line 42 is closed and the on-off valve disposed on the pumping line 52 is opened, the plasma enters the reaction chamber 1 through the second air inlet line 42; when the on-off valve provided on the second air intake line 42 is opened and the on-off valve provided on the exhaust line 52 is closed, the plasma enters the exhaust device 51.
In practical applications, the air extracting device 51 may be further connected to the reaction chamber 1 for extracting air from the reaction chamber 1 to extract residual air in the reaction chamber 1, so as to prevent the reaction chamber 1 from being contaminated and affecting the quality of the film.
In this embodiment, the gas inlet device further comprises a first precursor source bottle 33, a first connecting line 34 and a first source bottle gas inlet line 32, wherein the first precursor source bottle 33 is connected with the reaction chamber 1 through the first gas inlet line 31; both ends of the first connecting pipeline 34 are respectively connected with the first source bottle air inlet pipeline 32 and the first air inlet pipeline 31; on-off valves are provided on the first connecting line 34, the first source bottle inlet line 32 and the first inlet line 31.
In this embodiment, the on-off state among the first connecting line 34, the first source bottle gas inlet line 32, and the first gas inlet line 31 is controlled only by the on-off valve on the first connecting line 34, the on-off valve on the first source bottle gas inlet line 32 is used to control the on-off state between the first source bottle gas inlet line 32 and the first precursor source bottle 33, and the on-off valve on the first gas inlet line 31 is used to control the on-off state between the first gas inlet line 31 and the first precursor source bottle 33. When the second precursor or the plasma is introduced into the reaction chamber 1, the carrier gas is introduced into the first source bottle inlet line 32, the on-off valve on the first connecting line 34 is opened, the on-off valves on the first source bottle inlet line 32 and the first inlet line 31 are closed, the carrier gas can enter the reaction chamber 1 through the first connecting line 34 and the first inlet line 31, so that a stable carrier gas flow can be formed in the first source bottle inlet line 32, when the first precursor is required to be introduced into the reaction chamber 1, the on-off valve on the first connecting line 34 is closed, the on-off valves on the first source bottle inlet line 32 and the first inlet line 31 are opened, the stable carrier gas flow in the first source bottle inlet line 32 enters the first precursor source bottle 33 through the first source bottle inlet line 32, so that the first precursor can be stably carried into the reaction chamber 1 through the first inlet line 31, therefore, the first precursor meeting the process requirement can be introduced into the reaction chamber 1 within a short time, and the first precursor is uniformly distributed in the reaction chamber 1, so that the process time is shortened, and the quality of the film is improved.
However, the manner of arranging the on-off valves on the first source bottle inlet line 32 and the first inlet line 31 is not limited to this, and two on-off valves may be arranged on the first source bottle inlet line 32, one of the on-off valves being used to control the on-off between the first source bottle inlet line 32 and the first connecting line 34, and the other of the on-off valves being used to control the on-off between the first source bottle inlet line 32 and the first precursor source bottle 33, or two on-off valves may be arranged on the first inlet line 31, one of the on-off valves being used to control the on-off between the first inlet line 31 and the first connecting line 34, and the other one of the on-off valves being used to control the on-off between the first inlet line 31 and the first precursor source bottle 33.
In this embodiment, the gas inlet device further comprises a second precursor source bottle 63, a second connecting line 64 and a second source bottle gas inlet line 62, wherein the second precursor source bottle 63 is connected to the reaction chamber 1 through a third gas inlet line 61; the two ends of the second connecting pipeline 64 are respectively connected with the second source bottle air inlet pipeline 62 and the third air inlet pipeline 61; on-off valves are provided on the second connecting line 64, the second source cylinder inlet line 62 and the third inlet line 61.
In this embodiment, the on-off among the second connecting line 64, the second source bottle gas inlet line 62 and the third gas inlet line 61 is controlled by only the on-off valve on the second connecting line 64, the on-off valve on the second source bottle gas inlet line 62 is used for controlling the on-off between the second source bottle gas inlet line 62 and the second precursor source bottle 63, and the on-off valve on the third gas inlet line 61 is used for controlling the on-off between the third gas inlet line 61 and the second precursor source bottle 63. When the first precursor or the plasma is introduced into the reaction chamber 1, the carrier gas is introduced into the second source bottle inlet line 62, the on-off valve on the second connecting line 64 is opened, the on-off valves on the second source bottle inlet line 62 and the third inlet line 61 are closed, the carrier gas can enter the reaction chamber 1 through the second connecting line 64 and the third inlet line 61, so that a stable carrier gas flow can be formed in the second source bottle inlet line 62, when the second precursor is required to be introduced into the reaction chamber 1, the on-off valve on the second connecting line 64 is closed, the on-off valves on the second source bottle inlet line 62 and the third inlet line 61 are opened, so that the stable carrier gas flow in the second source bottle inlet line 62 enters the second source bottle 63 through the second source bottle inlet line 62, so that the second precursor can be stably carried into the reaction chamber 1 through the third inlet line 61, therefore, the second precursor meeting the process requirement can be introduced into the reaction chamber 1 within a short time, and the second precursor is uniformly distributed in the reaction chamber 1, so that the process time is shortened, and the quality of the film is improved.
However, the manner of arranging the on-off valves on the second source bottle air inlet line 62 and the third air inlet line 61 is not limited to this, and two on-off valves may be provided on the second source bottle air inlet line 62, one of which is used to control the on-off between the second source bottle air inlet line 62 and the second connecting line 64, and the other of which is used to control the on-off between the second source bottle air inlet line 62 and the second precursor source bottle 63, or two on-off valves may be provided on the third air inlet line 61, one of which is used to control the on-off between the third air inlet line 61 and the second connecting line 64, and the other of which is used to control the on-off between the third air inlet line 61 and the second precursor source bottle 63.
In this embodiment, the gas used to provide the plasma includes one or more of oxygen, ozone, and nitric oxide, mixed with argon or nitrogen.
In this embodiment, the carrier gas comprises nitrogen or an inert gas, preferably high purity nitrogen.
The embodiment further provides a gas inlet method, which adopts the gas inlet device to introduce the first precursor and the plasma into the reaction chamber 1, and comprises the following steps:
s1, introducing a first precursor into the reaction chamber 1 through the first air inlet pipe 31;
s2, forming plasma by the plasma generator 41, and introducing the plasma into the reaction chamber 1 through the second gas inlet pipe 42.
In the gas inlet method provided by this embodiment, with the aid of the gas inlet device provided by this embodiment, the first precursor is introduced into the reaction chamber 1 through the first gas inlet pipeline 31; plasma is formed through the plasma generator 41, and the plasma is introduced into the reaction chamber 1 through the second air inlet pipeline 42, so that the plasma and the first precursor form a required film in the reaction chamber 1, and ions in the plasma and ions in the first precursor are mutually attracted and combined by virtue of the ions in the plasma, which have opposite charges with the ions in the first precursor, so that the first precursor is fully reacted, thereby reducing ligand vacancies in the first precursor, further improving the density of the required film formed on the surface of the substrate 2, and improving the quality and the electrical property of the film.
In this embodiment, the air inlet means further comprise a third air inlet line 61, the third air inlet line 61 being connected to the reaction chamber 1; before the step of introducing the first precursor into the reaction chamber 1 through the first gas inlet line 31, the method further includes:
s3, introducing the second precursor into the reaction chamber 1 through the third gas inlet line 61.
Specifically, the second precursor can also react with the first precursor to form a required film, and the second precursor is introduced into the reaction chamber 1 to act together with the plasma, so that the first precursor reacts more fully.
The gas inlet apparatus provided in this embodiment is described below by taking the process of preparing hafnium oxide thin film as an example, wherein the first precursor is tetra (methylethylamino) hafnium (TEMAH, Hf [ N (C)2H5CH3)2]4) The second precursor is water (H)2O), a plasma generator 41 is used to form an oxygen plasma, and the carrier gas is preferably high purity nitrogen.
Before the process begins, firstly setting the reaction temperature to be 30-450 ℃, the reaction pressure to be 1 Torr-5 Torr and the gas flow of the high-purity nitrogen to be 20-2000 standard milliliters per minute (sccm) -2000 standard milliliters per minute, firstly introducing the high-purity nitrogen into the second source bottle air inlet pipeline 62, closing the on-off valve on the second connecting pipeline 64, opening the on-off valves on the second source bottle air inlet pipeline 62 and the third air inlet pipeline 61, and enabling the carrier gas to enter the second precursor source bottle 63 through the second source bottle air inlet pipeline 62 so as to enable the carrier gas to carry H2O enters the reaction chamber 1 through the third gas inlet line 61, so that H2O is adsorbed on the substrate 2 and generally carries H2The flow rate of the carrier gas of O is 20-2000 standard ml/min, and in practical application, the second precursor source bottle 63 may be heated to increase the content of water vapor in the second precursor source bottle 63, and the heating temperature is generally 20-150 ℃. Meanwhile, high-purity nitrogen is introduced into the first source bottle air inlet pipeline 32, the on-off valve on the first connecting pipeline 34 is opened, the on-off valves on the first source bottle air inlet pipeline 32 and the first air inlet pipeline 31 are closed, carrier gas is made to enter the reaction chamber 1 through the first connecting pipeline 34 and the first air inlet pipeline 31, gas for providing oxygen plasma with the gas flow rate of 20 standard milliliters per minute to 2000 standard milliliters per minute is introduced into the plasma generator 41, the on-off valve arranged on the second air inlet pipeline 42 is opened, the on-off valve arranged on the air suction pipeline 52 is closed, and the oxygen plasma is made to enter the air suction device 51 through the second air inlet pipeline 42 and the air suction pipeline 52, so that the oxygen plasma is stably formed in the second air inlet pipeline 42.
H is generally introduced into the reaction chamber 1 for 10 milliseconds to 30 seconds2After O, saturated adsorption can be achieved in the reaction chamber 1, then the first purging process is carried out, the on-off valve on the second connecting pipeline 64 is opened, the on-off valve at the joint of the second source bottle air inlet pipeline 62 and the second precursor source bottle 63 is closed, and H is stopped to be introduced into the reaction chamber 12And enabling the carrier gas to simultaneously enter the reaction chamber 1 through the first source bottle air inlet pipeline 32, the first air inlet pipeline 31, the second source bottle air inlet pipeline 62 and the third air inlet pipeline 61 so as to purge the third air inlet pipeline 61 and the reaction chamber 1, wherein the purging time is generally 1 second-3 minutes.
After the first purging process, the on-off valve on the first connecting pipeline 34 is closed, the on-off valves on the first source bottle inlet pipeline 32 and the first inlet pipeline 31 are opened, and the carrier gas enters the first precursor source bottle 33 through the first source bottle inlet pipeline 32, so that the carrier gas carries the tetra (methylethylamino) hafnium into the reaction chamber 1 through the first inlet pipeline 31, and the tetra (methylethylamino) hafnium and the H adsorbed on the substrate 2 are mixed together2The O reaction produces hafnium oxide, typically with a carrier gas carrying tetrakis (methylethylamino) hafnium at a flow rate of 20-2000 standard milliliters per minute. In practical applications, the first precursor source bottle 33 may be heated, typically at a temperature of 20-150 ℃. At the same time, high purity nitrogen is continuously introduced into the second source cylinder inlet line 62, andopening the on-off valve on the second connecting pipeline 64, closing the on-off valves on the second source bottle air inlet pipeline 62 and the third air inlet pipeline 61, leading the carrier gas to enter the reaction chamber 1 through the second connecting pipeline 64 and the third air inlet pipeline 61, simultaneously leading gas for providing oxygen plasma with the gas flow rate of 20 standard milliliters per minute-2000 standard milliliters per minute to the plasma generator 41, closing the on-off valve arranged on the second air inlet pipeline 42, opening the on-off valve arranged on the air suction pipeline 52, leading the oxygen plasma to enter the air suction device 51 through the second air inlet pipeline 42 and the air suction pipeline 52, and leading the oxygen plasma to be stably formed in the second air inlet pipeline 42.
Normally, after the tetra (methylethylamino) hafnium is introduced into the reaction chamber 1 for 10 milliseconds to 30 seconds, the saturated adsorption in the reaction chamber 1 can be achieved, then, the second purging process is performed, the on-off valve on the first connecting pipeline 34 is opened, the on-off valves on the first source bottle air inlet pipeline 32 and the first air inlet pipeline 31 are closed, the introduction of the tetra (methylethylamino) hafnium into the reaction chamber 1 is stopped, and the carrier gas is introduced into the reaction chamber 1 through the first source bottle air inlet pipeline 32, the first air inlet pipeline 31, the second source bottle air inlet pipeline 62 and the third air inlet pipeline 61, so as to purge the third air inlet pipeline 61 and the reaction chamber 1, wherein the purging time is generally 1 second to 3 minutes.
After the second purging process, the on-off valve disposed on the second air inlet line 42 is opened, and the on-off valve disposed on the air exhaust line 52 is closed, so that the oxygen plasma generated by the plasma generator 41 enters the reaction chamber 1 through the second air inlet line 42, and the oxygen plasma can fully react with the first precursor after the oxygen plasma is introduced into the reaction chamber 1 for 1 millisecond to 3 minutes, thereby forming a dense hafnium oxide film.
And then, performing a third purging process, namely opening the on-off valve arranged on the second air inlet pipeline 42, closing the on-off valve arranged on the air suction pipeline 52, stopping introducing the oxygen plasma into the reaction chamber 1, and allowing the carrier gas to enter the reaction chamber 1 through the first source bottle air inlet pipeline 32, the first air inlet pipeline 31, the second source bottle air inlet pipeline 62 and the third air inlet pipeline 61 so as to purge the first air inlet pipeline 31, the third air inlet pipeline 61 and the reaction chamber 1, wherein the general purging time is 1 second to 3 minutes. Thus, the sequential cycle of preparing the hafnium oxide film is completed.
And after the third purging process, performing a judging process, wherein whether the cycle number reaches the set cycle number or not needs to be judged, if so, ending the process, and if not, performing the process cycle again.
The judging process can be further divided into a first judging process and a second judging process, wherein the first judging process is performed after the second purging process, if the first judging process reaches the set cycle number, the oxygen plasma is introduced into the reaction chamber 1, the third purging process is performed, after the third purging process, the second judging process is performed, if the second judging process reaches the set cycle number, the process is ended, and if the set cycle number is not reached, the process is restarted from the step S3; if the first determination process does not reach the set number of cycles, the process is restarted from step S3 until the set number of cycles is reached in the first determination process, which is typically 2-10 cycles.
The embodiment also provides semiconductor processing equipment which comprises a reaction chamber 1 and the gas inlet device, wherein the first precursor and the plasma are introduced into the reaction chamber 1, so that a required thin film is formed on the surface of the substrate 2.
In the semiconductor processing apparatus provided by this embodiment, the ions in the plasma and the ions in the first precursor are attracted and combined with each other by the ions in the plasma having opposite charges to each other, so that the first precursor is fully reacted, and therefore, ligand vacancies in the first precursor are reduced, the density of the desired thin film formed on the surface of the substrate 2 is further improved, and the quality and the electrical property of the thin film are improved.
It will be understood that the above embodiments are merely exemplary embodiments taken to illustrate the principles of the present invention, which is not limited thereto. It will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the spirit and substance of the invention, and these modifications and improvements are also considered to be within the scope of the invention.
Claims (10)
1. The gas inlet device comprises a first gas inlet pipeline for introducing a first precursor into a reaction chamber, and is characterized by further comprising a plasma generator and a second gas inlet pipeline, wherein the plasma generator is connected with the reaction chamber through the second gas inlet pipeline and used for providing plasma for the reaction chamber, and the plasma can react with the first precursor and form a required film on the surface of a substrate.
2. The gas inlet apparatus of claim 1, further comprising a third gas inlet line for introducing a second precursor into the reaction chamber.
3. The air inlet device according to claim 1, further comprising an air extraction device and an air extraction pipeline, wherein two ends of the air extraction pipeline are respectively connected with the air extraction device and the second air inlet pipeline; the air exhaust device is connected with the reaction chamber.
4. The gas inlet arrangement of claim 1, further comprising a first precursor source bottle, a first connecting line, and a first source bottle gas inlet line, the first precursor source bottle being connected to the reaction chamber through the first gas inlet line;
two ends of the first connecting pipeline are respectively connected with the first source bottle air inlet pipeline and the first air inlet pipeline;
and on-off valves are arranged on the first connecting pipeline, the first source bottle air inlet pipeline and the first air inlet pipeline.
5. The gas inlet arrangement of claim 2, further comprising a second precursor source bottle, a second connecting line, and a second source bottle gas inlet line, the second precursor source bottle being connected to the reaction chamber through the third gas inlet line;
two ends of the second connecting pipeline are respectively connected with the second source bottle air inlet pipeline and the third air inlet pipeline;
and on-off valves are arranged on the second connecting pipeline, the second source bottle air inlet pipeline and the third air inlet pipeline.
6. The gas inlet device according to claim 1, wherein the gas for providing the plasma comprises a gas of one or more of oxygen, ozone and nitric oxide mixed with argon or nitrogen.
7. An air intake device according to claim 3, wherein on-off valves are provided on both the second air intake line and the air extraction line.
8. A method for introducing gas, wherein the gas inlet device of any one of claims 1 to 7 is used for introducing the first precursor and the plasma into the reaction chamber, and the method comprises the following steps:
introducing the first precursor into the reaction chamber through the first gas inlet pipeline;
and forming plasma through the plasma generator, and introducing the plasma into the reaction chamber through the second air inlet pipeline.
9. The method of claim 8, wherein the gas inlet device further comprises a third gas inlet line, the third gas inlet line being connected to the reaction chamber;
before the step of introducing the first precursor into the reaction chamber through the first gas inlet pipe, the method further comprises the following steps: and introducing a second precursor into the reaction chamber through the third gas inlet pipeline.
10. A semiconductor processing apparatus comprising a reaction chamber and the gas inlet apparatus of any one of claims 1 to 7 to introduce the first precursor and the plasma into the reaction chamber.
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| CN115369382A (en) * | 2022-08-24 | 2022-11-22 | 厦门韫茂科技有限公司 | Gas path device and gas inlet method for atomic layer deposition process |
| CN115679288A (en) * | 2022-11-08 | 2023-02-03 | 江苏微导纳米科技股份有限公司 | Coating apparatus and control method thereof |
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