CN111074235B - 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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- CN111074235B CN111074235B CN201811223387.1A CN201811223387A CN111074235B CN 111074235 B CN111074235 B CN 111074235B CN 201811223387 A CN201811223387 A CN 201811223387A CN 111074235 B CN111074235 B CN 111074235B
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- 238000000034 method Methods 0.000 title claims abstract description 59
- 239000004065 semiconductor Substances 0.000 title claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 133
- 238000006243 chemical reaction Methods 0.000 claims abstract description 123
- 239000007789 gas Substances 0.000 claims description 41
- 229910052760 oxygen Inorganic materials 0.000 claims description 39
- 239000001301 oxygen Substances 0.000 claims description 38
- 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 26
- 239000012159 carrier gas Substances 0.000 claims description 24
- 229910000449 hafnium oxide Inorganic materials 0.000 claims description 21
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 claims description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims description 13
- 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
- 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
- 238000000605 extraction Methods 0.000 claims description 4
- 210000002381 plasma Anatomy 0.000 claims 14
- 239000000758 substrate Substances 0.000 abstract description 26
- 239000003446 ligand Substances 0.000 abstract description 11
- 239000010408 film Substances 0.000 description 34
- 150000002500 ions Chemical class 0.000 description 24
- NPEOKFBCHNGLJD-UHFFFAOYSA-N ethyl(methyl)azanide;hafnium(4+) Chemical compound [Hf+4].CC[N-]C.CC[N-]C.CC[N-]C.CC[N-]C NPEOKFBCHNGLJD-UHFFFAOYSA-N 0.000 description 17
- 238000010926 purge Methods 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 229910052735 hafnium Inorganic materials 0.000 description 8
- CRHIBFCNJROORF-UHFFFAOYSA-N hafnium(4+);methylazanide Chemical group [Hf+4].[NH-]C.[NH-]C.[NH-]C.[NH-]C CRHIBFCNJROORF-UHFFFAOYSA-N 0.000 description 6
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 5
- -1 hafnium ions Chemical class 0.000 description 5
- 239000010409 thin film Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 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 4
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(iv) oxide Chemical compound O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 description 4
- 150000001450 anions Chemical class 0.000 description 3
- 238000000231 atomic layer deposition Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000013110 organic ligand Substances 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 238000000151 deposition Methods 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
- 238000004378 air conditioning Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process 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
- 238000010586 diagram Methods 0.000 description 1
- 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 1
- 238000006073 displacement reaction Methods 0.000 description 1
- SMQFETZVGKJCSL-UHFFFAOYSA-N ethylazanide;hafnium(4+) Chemical compound [Hf+4].CC[NH-].CC[NH-].CC[NH-].CC[NH-] SMQFETZVGKJCSL-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification 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
Classifications
-
- 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
Landscapes
- 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 is 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 air inlet device, the air inlet method and the semiconductor processing equipment provided by the invention can reduce the ligand vacancy in the first precursor, thereby improving the film density and the film quality and the electrical property.
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 characteristic line width in the traditional silicon-based Complementary Metal Oxide Semiconductor (CMOS) integrated technology has been reduced from the original micron level to the nanometer level, and silicon dioxide is used as an excellent gate dielectric layer material, which can not meet the requirements of semiconductor devices on dielectric layers, so that people can turn the eyes to dielectric layer materials with high dielectric constants. Due to hafnium oxide (HfO) 2 ) The hafnium oxide is a good high-dielectric constant material for replacing a silicon dioxide dielectric layer, and has the characteristics of high dielectric constant, large forbidden bandwidth, moderate valence band and conduction band offset, good thermal stability and the like. And the film prepared by the atomic layer deposition technology has the advantages of controllable thickness, excellent uniformity, high step coverage rate and the like. Accordingly, atomic layer deposition hafnium oxide processes are receiving increasing attention in the trend of shrinking feature linewidths.
In the prior atomic layer deposition hafnium oxide process, the method generally adoptsUsing tetra (dimethylamino) hafnium (TDMAH) as a hafnium source, water (H) 2 O) as an oxygen source, first introducing water into the reaction chamber to adsorb the water on the surface of the substrate, then introducing tetra (dimethylamino) hafnium into the reaction chamber to react with the water adsorbed on the surface of the substrate, and combining the organic ligand of the hafnium source with oxygen in the water, thereby depositing hafnium oxide on the surface of the substrate.
However, in the process of depositing hafnium dioxide by reacting tetra (dimethylamino) hafnium with water, a part of hafnium source organic ligands cannot react with water due to steric hindrance effect, so that the hafnium source organic ligands cannot be combined with oxygen in water, a large amount of oxygen vacancies are generated, the film density is reduced, and the leakage current density, breakdown voltage and other electrical properties of the hafnium dioxide film are affected.
Disclosure of Invention
The invention aims at solving at least one of the technical problems in the prior art, and provides an air inlet device, an air inlet method and semiconductor processing equipment, which can reduce ligand vacancies in a first precursor, thereby improving film density and film quality and electrical property.
In order to achieve the object of the invention, there is provided an air inlet device comprising a first air inlet pipe for introducing a first precursor into a reaction chamber, the air inlet device further comprising a plasma generator and a second air inlet pipe, the plasma generator being connected to the reaction chamber through the second air inlet pipe for supplying a plasma to the reaction chamber, the plasma being capable of reacting with the first precursor and forming a desired film on a surface of a substrate.
Preferably, the reaction chamber further comprises a third air inlet pipeline, wherein the third air inlet pipeline is used for introducing a second precursor into the reaction chamber.
Preferably, the air-conditioning system further comprises an air extracting device and an air extracting pipeline, wherein two ends of the air extracting pipeline are respectively connected with the air extracting device and the second air inlet pipeline; the air extracting device is connected with the reaction chamber.
Preferably, the reaction chamber 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 reaction chamber 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 for providing the plasma includes one or more of oxygen, ozone and nitric oxide, and mixed with argon or nitrogen.
Preferably, on-off valves are arranged on the second air inlet pipeline and the exhaust pipeline.
The invention also provides an air inlet method, which adopts the air 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 air 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 air inlet device further comprises a third air inlet pipeline, and the third air inlet pipeline is connected with the reaction chamber;
before the step of introducing the first precursor into the reaction chamber through the first air inlet pipeline, the method further comprises: and introducing a second precursor into the reaction chamber through the third air inlet pipeline.
The invention also provides semiconductor processing equipment, which comprises a reaction chamber and the air inlet device, wherein the first precursor and the plasma are introduced into the reaction chamber.
The invention has the following beneficial effects:
the air inlet device comprises a first air inlet pipeline, a plasma generator and a second air inlet pipeline, wherein the first air 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 air inlet pipeline so as to provide the plasma for the reaction chamber, and ions in the plasma and ions in the first precursor are mutually attracted and combined by virtue of ions with opposite charges in the plasma and ions in the first precursor, so that the first precursor fully reacts, ligand vacancies in the first precursor are reduced, the density of a required film formed on the surface of a substrate is improved, and the quality and the electrical property of the film are improved.
According to the air inlet method provided by the invention, by means of the air inlet device provided by the invention, a first precursor is introduced into the reaction chamber through the first air inlet pipeline; and plasma is formed through the plasma generator, and the plasma is introduced into the reaction chamber through the second air inlet pipeline, so that the ions in the plasma and the ions in the first precursor are mutually attracted and combined by means of the ions with opposite charges in the plasma and the ions in the first precursor, and 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 electrical property of the film.
The semiconductor processing equipment provided by the invention comprises the reaction chamber and the air inlet device provided by the invention, ions in the plasma and ions in the first precursor are mutually attracted and combined by virtue of ions with opposite charges in the plasma and 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 view of a semiconductor processing apparatus according to the present invention;
FIG. 2 is a block flow diagram of an air intake method provided by the present invention;
FIG. 3 is another flow chart of the air intake method provided by the present invention;
reference numerals illustrate:
1-a reaction chamber; 2-a substrate; 31-a first air inlet line; 32-a first source bottle air inlet line; 33-a first precursor source vial; 34-a first connection line; 41-a plasma generator; 42-a second air inlet line; 51-an air extraction device; 52-an air extraction pipeline; 61-a third air intake line; 62-a second source bottle air inlet line; 63-a second precursor source vial; 64-second connecting line.
Detailed Description
In order to enable those skilled in the art to better understand the technical scheme of the present invention, the air inlet device, the air inlet method and the semiconductor processing equipment provided by the present invention are described in detail below with reference to the accompanying drawings.
The present embodiment provides an air inlet device comprising a plasma generator 41, a second air inlet pipe 42 and a first air inlet pipe 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 air inlet pipe 42 for providing plasma to the reaction chamber 1, and the plasma can react with the first precursor and form a required film on the surface of a substrate 2.
The air inlet device provided by the embodiment makes the ions in the plasma and the ions in the first precursor attract and combine with each other by means of the ions with opposite charges in the plasma and the ions in the first precursor, so that the first precursor fully reacts, 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 film quality and the electrical property are improved.
The hafnium oxide thin film is prepared by the following processThe gas inlet means is described in which the first precursor is tetra (methylamino) hafnium (TEMAH, hf [ N (C) 2 H 5 CH 3 ) 2 ] 4 ) The plasma generator 41 is used to form an 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 or nitrogen. Before the process starts, the substrate 2 is placed in the reaction chamber 1, tetra (methyl ethylamino) hafnium is introduced into the reaction chamber 1 through the first air inlet pipeline 31, so that the tetra (methyl ethylamino) hafnium is adsorbed on the surface of the substrate 2, then one or more gases including oxygen, ozone and nitric oxide and mixed with argon or nitrogen are introduced into the plasma generator, the gases are ionized by the plasma generator to form oxygen plasma, and the oxygen plasma is introduced into the reaction chamber 1 through the second air inlet pipeline 42 to react with the tetra (methyl ethylamino) hafnium adsorbed on the surface of the substrate 2, so that a hafnium oxide film is formed on the surface of the substrate 2.
Specifically, tetra (methylethylamino) hafnium (Hf [ N (C) 2 H 5 CH 3 ) 2 ] 4 ) From hafnium ions (Hf) 4+ ) With ligands ([ N (C) 2 H 5 CH 3 ) 2 ] - ) The oxygen plasma contains oxygen ions (O 2- ) Because the oxygen ions are negative anions and the hafnium ions are positive anions, the hafnium ions can be more effectively replaced from the tetra (methyl ethylamino) hafnium through the mutual attraction between the anions and the cations with opposite charges, namely, the tetra (methyl ethylamino) hafnium and oxygen plasma undergo a replacement reaction, so that more hafnium oxide is formed in unit area, namely, the density of the hafnium oxide is improved, namely, ligand vacancies in the tetra (methyl ethylamino) hafnium 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.
In practical applications, the first precursor in the process of preparing the hafnium oxide film may also be tetra (dimethylamino) hafnium (TDMAH) or tetra (diethylamino) hafnium (TDEAH). Argon or nitrogen in the gas used to provide the oxygen plasma is primarily for the purpose of generating ignition in the plasma generator 41 to form an oxygen plasma from one or more of oxygen, ozone and nitric oxide.
In this embodiment, the gas inlet device further comprises a third gas inlet line 61, and the third gas inlet line 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 and the plasma jointly act through introducing the second precursor into the reaction chamber 1, so that the first precursor reacts more fully.
Still taking tetra (methyl ethylamino) hafnium as the first precursor to prepare the hafnium oxide film, the effect of the third air inlet pipeline 61 in the air inlet device is described, in the process, the second precursor is taken as an oxygen source to be introduced into the reaction chamber 1 through the third air inlet pipeline 61, so that the oxygen in the second precursor reacts with the hafnium in the first precursor, and the effect is similar to that of plasma, and in the process of reacting the first precursor with the plasma, the second precursor is added, so that the reaction of the first precursor is more sufficient, and the formation of a compact hafnium oxide film is facilitated. Below with water (H) 2 O) is illustrated as a second precursor. Before introducing tetra (methylamino) hafnium into the reaction chamber 1, H is introduced into the reaction chamber 1 through the third inlet pipe 61 2 O, H 2 O is adsorbed on the surface of the substrate 2, and then tetra (methyl ethylamino) hafnium is introduced into the reaction chamber 1 through the first air inlet pipeline 31, so that the tetra (methyl ethylamino) hafnium and H adsorbed on the surface of the substrate 2 2 O reacts to form hafnium oxide, and finally oxygen plasma is introduced into the reaction chamber 1 through the plasma generator 41 and the second air inlet pipeline 42, and the oxygen plasma is not reacted with H on the surface of the substrate 2 2 O reacts with tetra (methyl ethylamino) hafnium to form a dense hafnium oxide film.
Specifically, the composition is prepared in the presence of tetra (methylamino) hafnium (Hf [ N (C) 2 H 5 CH 3 ) 2 ] 4 ) In (C) due to the ligand [ N (C) 2 H 5 CH 3 ) 2 ] - Larger, block H 2 O diffuses to Hf4 + And [ N (C) 2 H 5 CH 3 ) 2 ] - Is blocked by H 2 O and tetra (methyl ethylamino) hafnium undergo displacement reaction, and O 2- Negatively charged, readily and positively charged Hf 4+ Binding at the same time [ N (C2H 5CH 3) 2] - And H is 2 Positively charged holes in O combine to give H 2 O fully reacts with the tetra (methyl ethylamino) hafnium to form a compact hafnium oxide film, so that the film quality is improved.
In practice, the second precursor as an oxygen source may also be oxygen (O 2 ) And ozone (O) 3 ) Etc. The number of the first air intake pipe 31 and the third air intake pipe 61 may be plural. In addition, the second precursor (H 2 The order of introducing O) and tetra (methyl ethylamino) hafnium into the reaction chamber 1 can be that the tetra (methyl ethylamino) hafnium is introduced first and then H is introduced 2 O, however, is preferably introduced by first introducing H 2 O, due to H 2 O is more easily and uniformly adsorbed on the surface of the substrate 2.
In this embodiment, the air intake device further includes an air exhaust device 51 and an air exhaust pipeline 52, two ends of the air exhaust pipeline 52 are respectively connected with the air exhaust device 51 and the second air intake pipeline 42, the plasma generated by the plasma generator 41 can be pumped into the air exhaust device 51 through the air exhaust pipeline 52 by the air exhaust device 51, so that the first precursor or the second precursor can be introduced into the reaction chamber 1, the gas for forming the plasma can be introduced into the plasma generator 41 at the same time, so that stable plasma can be formed, the plasma can enter the air exhaust device 51 through the air exhaust pipeline 52, the reaction of the substrate 2 with the plasma when the first precursor is not saturated and adsorbed is avoided, the film quality is influenced, 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 air intake pipeline 42, so that the plasma meeting the process requirement can be introduced into the reaction chamber 1 in a short time, the plasma is uniformly distributed in the reaction chamber 1, the process time is shortened, and the film quality is improved.
In practical applications, on-off valves may be disposed on the second air inlet pipe 42 and the air exhaust pipe 52 to control the plasma to enter the reaction chamber 1 or the air exhaust device 51, when the on-off valve disposed on the second air inlet pipe 42 is closed and the on-off valve disposed on the air exhaust pipe 52 is opened, the plasma enters the reaction chamber 1 through the second air inlet pipe 42; when the on-off valve provided on the second air intake duct 42 is opened and the on-off valve provided on the air exhaust duct 52 is closed, the plasma enters the air exhaust device 51.
In practical application, the air extracting device 51 may be further connected to the reaction chamber 1, so as to extract the residual gas in the reaction chamber 1, thereby avoiding the pollution of the reaction chamber 1 and affecting the quality of the film.
In this embodiment, the air inlet device further includes a first precursor source bottle 33, a first connection pipe 34, and a first source bottle air inlet pipe 32, where the first precursor source bottle 33 is connected to the reaction chamber 1 through the first air inlet pipe 31; two 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 connection pipe 34, the first source bottle inlet pipe 32 and the first inlet pipe 31.
In this embodiment, the on-off of the first connecting pipe 34, the first source bottle air inlet pipe 32 and the first air inlet pipe 31 is controlled only by the on-off valve on the first connecting pipe 34, the on-off valve on the first source bottle air inlet pipe 32 is used for controlling the on-off between the first source bottle air inlet pipe 32 and the first precursor source bottle 33, and the on-off valve on the first air inlet pipe 31 is used for controlling the on-off between the first air inlet pipe 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 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, the carrier gas can enter the reaction chamber 1 through the first connecting pipeline 34 and the first air inlet pipeline 31, so that stable carrier gas flow can be formed in the first source bottle air inlet pipeline 32, and when the first precursor is required to be introduced into the reaction chamber 1, the on-off valve on the first connecting pipeline 34 is closed, the on-off valve on the first source bottle air inlet pipeline 32 and the on-off valve on the first air inlet pipeline 31 are opened, the carrier gas flow stabilized in the first source bottle air inlet pipeline 32 enters the first precursor source bottle 33 through the first source bottle air inlet pipeline 32, the carrier gas can be stably carried into the reaction chamber 1 through the first air inlet pipeline 31, the first precursor can be stably carried into the reaction chamber 1, the first precursor can be uniformly introduced into the reaction chamber 1 in a short time, the first precursor can be uniformly distributed in the reaction chamber 1, and the quality of the first precursor can be uniformly distributed in the reaction chamber can be further reduced.
However, the arrangement of the on-off valves on the first source bottle air inlet pipeline 32 and the first air inlet pipeline 31 is not limited to this, and two on-off valves may be disposed on the first source bottle air inlet pipeline 32, one of the on-off valves is used for controlling the on-off between the first source bottle air inlet pipeline 32 and the first connection pipeline 34, the other on-off valve is used for controlling the on-off between the first source bottle air inlet pipeline 32 and the first precursor source bottle 33, in addition, two on-off valves may be disposed on the first air inlet pipeline 31, one of the on-off valves is used for controlling the on-off between the first air inlet pipeline 31 and the first connection pipeline 34, and the other on-off valve is used for controlling the on-off between the first air inlet pipeline 31 and the first precursor source bottle 33.
In this embodiment, the air inlet device further includes a second precursor source bottle 63, a second connection line 64, and a second source bottle air inlet line 62, where the second precursor source bottle 63 is connected to the reaction chamber 1 through a third air inlet line 61; 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 connection pipe 64, the second source cylinder intake pipe 62, and the third intake pipe 61.
In the present embodiment, the on-off of the second connecting line 64, the second source bottle air inlet line 62 and the third air inlet line 61 is controlled only by the on-off valve on the second connecting line 64, the on-off valve on the second source bottle air inlet line 62 is used for controlling the on-off between the second source bottle air inlet line 62 and the second precursor source bottle 63, and the on-off valve on the third air inlet line 61 is used for controlling the on-off between the third air inlet line 61 and the second precursor source bottle 63. While introducing the first precursor or the plasma into the reaction chamber 1, introducing the carrier gas into the second source bottle gas inlet pipeline 62, opening the on-off valve on the second connecting pipeline 64, closing the on-off valves on the second source bottle gas inlet pipeline 62 and the third gas inlet pipeline 61, so that the carrier gas can enter the reaction chamber 1 through the second connecting pipeline 64 and the third gas inlet pipeline 61, a stable carrier gas flow can be formed in the second source bottle gas inlet pipeline 62, when the second precursor is required to be introduced into the reaction chamber 1, the on-off valve on the second connecting pipeline 64 is closed, the on-off valves on the second source bottle gas inlet pipeline 62 and the third gas inlet pipeline 61 are opened, the carrier gas flow stabilized in the second source bottle gas inlet pipeline 62 enters the second precursor source bottle 63 through the second source bottle gas inlet pipeline 62, the carrier gas can be stably carried into the reaction chamber 1 through the third gas inlet pipeline 61, the second precursor can be introduced into the reaction chamber 1 in a short time, the second precursor can be uniformly distributed in the reaction chamber 1, and the quality of the reaction chamber is further shortened.
However, the arrangement of 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 connection line 64, 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, and in addition, 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 connection 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 for supplying plasma includes one or more of oxygen, ozone, and nitric oxide, and mixed with argon or nitrogen.
In this embodiment, the carrier gas includes nitrogen or an inert gas, and preferably high purity nitrogen is used.
The embodiment also provides an air intake method, which adopts the air intake 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 a first air inlet pipeline 31;
s2, plasma is formed by the plasma generator 41, and the plasma is introduced into the reaction chamber 1 through the second gas inlet line 42.
In the air inlet method provided in this embodiment, by means of the air inlet device provided in this embodiment, the first precursor is introduced into the reaction chamber 1 through the first air 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 ions with opposite charges in the plasma and ions in the first precursor, so that the first precursor fully reacts, ligand vacancies in the first precursor are reduced, the density of the required film formed on the surface of the substrate 2 is improved, and the film quality and the electrical property are improved.
In the present embodiment, the air inlet device further includes a third air inlet pipe 61, and the third air inlet pipe 61 is connected to the reaction chamber 1; before the step of introducing the first precursor into the reaction chamber 1 through the first inlet line 31, it further comprises:
and S3, introducing a second precursor into the reaction chamber 1 through a third air inlet pipeline 61.
Specifically, the second precursor can also react with the first precursor to form a required film, and the second precursor and the plasma jointly act through introducing the second precursor into the reaction chamber 1, so that the first precursor reacts more fully.
The air inlet device according to this embodiment will be described by taking a process for preparing a hafnium oxide film as an example, wherein the first precursor is tetra (methylamino) hafnium (TEMAH, hf [ N (C) 2 H 5 CH 3 ) 2 ] 4 ) The second precursor is water (H 2 O), the plasma generator 41 is used to form an oxygen plasma, and the carrier gas is preferably high purity nitrogen.
Before the process starts, the reaction temperature is set to be 30-450 ℃, the reaction pressure is 1-5 Torr, the gas flow rate of high-purity nitrogen is 20-2000 standard milliliters per minute (sccm), the high-purity nitrogen is firstly introduced into the second source bottle gas inlet pipeline 62, the on-off valve on the second connecting pipeline 64 is closed, the on-off valves on the second source bottle gas inlet pipeline 62 and the third gas inlet pipeline 61 are opened, and the carrier gas enters the second precursor source bottle 63 through the second source bottle gas inlet pipeline 62, so that the carrier gas carries H 2 O enters the reaction chamber 1 through the third air inlet pipeline 61, thereby leading H 2 O is adsorbed on the substrate 2, typically carrying H 2 The flow rate of the carrier gas of O is 20 to 2000 standard milliliters per minute, 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 typically 20 to 150 ℃. At the same time, 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 enters 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 20-2000 standard milliliters per minute is simultaneously 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 oxygen plasma enters the air suction device 51 through the second air inlet pipeline 42 and the air suction pipeline 52, so that oxygen plasma is stably formed in the second air inlet pipeline 42.
H is typically introduced into the reaction chamber 1 for 10 milliseconds to 30 seconds 2 After O, saturated adsorption can be achieved in the reaction chamber 1, then a first purging process is performed, 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 the introduction of H into the reaction chamber 1 is stopped 2 O, and simultaneously passing the carrier gas through the first source bottle inlet line 32, the first inlet line 31, the second source bottle inlet line 62, and the third inlet line 61Into the reaction chamber 1 to purge the third inlet line 61 and the reaction chamber 1, typically for a period of 1 second to 3 minutes.
After the first purging process, the on-off valve on the first connecting pipe 34 is closed, the on-off valves on the first source bottle air inlet pipe 32 and the first air inlet pipe 31 are opened, and the carrier gas is led into the first precursor source bottle 33 through the first source bottle air inlet pipe 32, so that the carrier gas carries tetra (methyl ethyl amino) hafnium into the reaction chamber 1 through the first air inlet pipe 31, and the tetra (methyl ethyl amino) hafnium and H adsorbed on the substrate 2 are led 2 The O reaction produces hafnium oxide, typically with a flow rate of carrier gas carrying tetra (methylamino) hafnium of 20 to 2000 standard milliliters per minute. In practical applications, the first precursor source vessel 33 may be heated, typically at a temperature of 20-150 degrees celsius. Meanwhile, high-purity nitrogen is continuously introduced into the second source bottle air inlet pipeline 62, the on-off valve on the second connecting pipeline 64 is opened, the on-off valves on the second source bottle air inlet pipeline 62 and the third air inlet pipeline 61 are closed, carrier gas enters the reaction chamber 1 through the second connecting pipeline 64 and the third air inlet pipeline 61, gas for providing oxygen plasma with the gas flow rate of 20 standard milliliters per minute to 2000 standard milliliters per minute is simultaneously introduced into the plasma generator 41, the on-off valve arranged on the second air inlet pipeline 42 is closed, the on-off valve arranged on the air suction pipeline 52 is opened, and oxygen plasma enters the air suction device 51 through the second air inlet pipeline 42 and the air suction pipeline 52, so that oxygen plasma is stably formed in the second air inlet pipeline 42.
After introducing tetra (methylamino) hafnium into the reaction chamber 1 for 10 ms-30 s, saturated adsorption can be achieved in the reaction chamber 1, then a second purging process is performed, on-off valves on the first connecting pipeline 34 are opened, on-off valves on the first source bottle air inlet pipeline 32 and the first air inlet pipeline 31 are closed, introducing tetra (ethylamino) hafnium into the reaction chamber 1 is stopped, and 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 to purge the third air inlet pipeline 61 and the reaction chamber 1, wherein the typical purging time is 1 s-3 min.
After the second purging process, the on-off valve arranged on the second air inlet pipeline 42 is opened, the on-off valve arranged on the air exhaust pipeline 52 is closed, so that oxygen plasma generated by the plasma generator 41 enters the reaction chamber 1 through the second air inlet pipeline 42, and the time for the oxygen plasma to enter the reaction chamber 1 is generally 1 millisecond-3 minutes, so that the oxygen plasma can fully react with the first precursor, and a compact hafnium oxide film is formed.
Then, the third purging process is performed, the on-off valve arranged on the second air inlet pipeline 42 is opened, the on-off valve arranged on the air extraction pipeline 52 is closed, the oxygen plasma is stopped from being introduced into the reaction chamber 1, and the carrier gas enters 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 that the first air inlet pipeline 31, the third air inlet pipeline 61 and the reaction chamber 1 are purged, and the purging time is generally 1 second to 3 minutes. From this, the sequential cycle of preparing the hafnium oxide thin film is completed.
After the third purging process, a judging process is performed, and whether the cycle number reaches the set cycle number or not needs to be judged, if the cycle number reaches the set cycle number, the process is ended, and if the cycle number does not reach the set cycle number, the process cycle is performed again.
The judging process can be further divided into a first judging process and a second judging process, wherein after the first judging process is performed in the second purging process, if the first judging process reaches the set cycle number, oxygen plasma is introduced into the reaction chamber 1, the third purging process is performed, and 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 second judging process does not reach the set cycle number, the process is restarted from the step S3; if the first determination process does not reach the set number of cycles, the process starts again from step S3 until the set number of cycles is reached during the first determination process, which is typically 2-10 cycles.
The present embodiment also provides a semiconductor processing apparatus, which includes the reaction chamber 1 and the gas inlet device described above, so as to introduce the first precursor and the plasma into the reaction chamber 1, thereby forming a desired thin film on the surface of the substrate 2.
The semiconductor processing apparatus provided in this embodiment makes the ions in the plasma and the ions in the first precursor attract and combine with each other by means of the ions in the plasma and the ions in the first precursor, so that the first precursor fully reacts, thereby reducing ligand vacancies in the first precursor, further improving the density of the required thin film formed on the surface of the substrate 2, and improving the quality and electrical properties of the thin film.
It is to be understood that the above embodiments are merely illustrative of the application of the principles of the present invention, but not in limitation thereof. Various modifications and improvements may be made by those skilled in the art without departing from the spirit and substance of the invention, and are also considered to be within the scope of the invention.
Claims (7)
1. The air inlet method is applied to an air inlet device and is characterized in that the air inlet device comprises a first air inlet pipeline, a plasma generator, a second air inlet pipeline, a third air inlet pipeline, an air exhaust device and an air exhaust pipeline, so that a first precursor, a second precursor and plasma are introduced into a reaction chamber, and two ends of the air exhaust pipeline are respectively connected with the air exhaust device and the second air inlet pipeline; the air intake method comprises the following steps:
introducing a second precursor into the reaction chamber through the third air inlet pipeline;
introducing the first precursor into the reaction chamber through the first air inlet pipeline;
forming plasma through the plasma generator, and introducing the plasma into the reaction chamber through the second air inlet pipeline;
circularly introducing the second precursor, the first precursor and the plasma, wherein the plasma is introduced after the second precursor and the first precursor, or the plasma is introduced after the second precursor and the first precursor are circularly introduced for a plurality of times;
in the process of introducing the first precursor or the second precursor into the reaction chamber, opening an on-off valve on the third air inlet pipeline to introduce the second precursor into the reaction chamber or opening an on-off valve on the first air inlet pipeline to introduce the first precursor into the reaction chamber, simultaneously introducing gas for forming plasma into the plasma generator, and opening the on-off valve on the air exhaust pipeline and closing the on-off valve on the second air inlet pipeline to enable the plasma to enter the air exhaust device through the air exhaust pipeline so as to form stable plasma; after the first precursor reacts with the second precursor, the on-off valve on the third air inlet pipeline, the on-off valve on the first air inlet pipeline and the on-off valve on the air exhaust pipeline are all closed, and the on-off valve on the second air inlet pipeline is opened so as to enable stable plasmas to be introduced into the reaction chamber to form the hafnium oxide film.
2. The method of claim 1, wherein the gas inlet apparatus further comprises 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;
on-off valves are arranged on the second connecting pipeline, the second source bottle air inlet pipeline and the third air inlet pipeline;
the on-off valve on the second connecting pipeline is closed only when the second gas inlet pipeline is used for introducing the second precursor carried by the carrier gas in the second source bottle gas inlet pipeline into the reaction chamber.
3. The method of claim 2, wherein the evacuation device is connected to the reaction chamber.
4. The method of claim 2, further comprising a first precursor source bottle, a first connecting line, and a first source bottle inlet line, the first precursor source bottle being connected to the reaction chamber through the first 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 method of claim 2, wherein the gas used to provide the plasma comprises one or more of oxygen, ozone, and nitric oxide mixed with argon or nitrogen.
6. An air intake method according to claim 3, wherein on-off valves are provided on both the second air intake pipe and the air extraction pipe.
7. A semiconductor processing apparatus comprising a reaction chamber and an air intake device for air intake of the reaction chamber using the air intake method of any one of claims 1 to 6.
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