CN115522180A - Preparation method and application of silicon-based thin film with low dielectric constant - Google Patents
Preparation method and application of silicon-based thin film with low dielectric constant Download PDFInfo
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 63
- 239000010703 silicon Substances 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000010409 thin film Substances 0.000 title claims description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 123
- 239000000758 substrate Substances 0.000 claims abstract description 44
- 239000012686 silicon precursor Substances 0.000 claims abstract description 20
- 238000001179 sorption measurement Methods 0.000 claims abstract description 17
- 239000001257 hydrogen Substances 0.000 claims abstract description 16
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 16
- 239000000126 substance Substances 0.000 claims abstract description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000007789 gas Substances 0.000 claims abstract description 14
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004065 semiconductor Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 239000011229 interlayer Substances 0.000 claims abstract description 8
- 238000005086 pumping Methods 0.000 claims abstract description 8
- LQKJCIRRALFVIT-UHFFFAOYSA-N (2,4,4,6,6,8,8-heptamethyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocan-2-yl) acetate Chemical compound CC(=O)O[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 LQKJCIRRALFVIT-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052786 argon Inorganic materials 0.000 claims abstract description 7
- VLQZJOLYNOGECD-UHFFFAOYSA-N 2,4,6-trimethyl-1,3,5,2,4,6-trioxatrisilinane Chemical compound C[SiH]1O[SiH](C)O[SiH](C)O1 VLQZJOLYNOGECD-UHFFFAOYSA-N 0.000 claims abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 68
- 239000010408 film Substances 0.000 claims description 64
- 229910052757 nitrogen Inorganic materials 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 19
- 238000007599 discharging Methods 0.000 claims description 14
- 239000012495 reaction gas Substances 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 235000012239 silicon dioxide Nutrition 0.000 claims description 10
- 239000000377 silicon dioxide Substances 0.000 claims description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 3
- 229910002601 GaN Inorganic materials 0.000 claims description 2
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 claims description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 230000006698 induction Effects 0.000 claims description 2
- 229910052594 sapphire Inorganic materials 0.000 claims description 2
- 239000010980 sapphire Substances 0.000 claims description 2
- 229910052990 silicon hydride Inorganic materials 0.000 claims description 2
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 235000012431 wafers Nutrition 0.000 description 13
- 239000012535 impurity Substances 0.000 description 9
- 239000010410 layer Substances 0.000 description 9
- 239000006227 byproduct Substances 0.000 description 8
- 229910001873 dinitrogen Inorganic materials 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 239000007795 chemical reaction product Substances 0.000 description 5
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical compound [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 150000002431 hydrogen Chemical group 0.000 description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 125000000962 organic group Chemical group 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 230000003071 parasitic effect Effects 0.000 description 2
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 description 2
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229910018540 Si C Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 150000007529 inorganic bases Chemical class 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000006864 oxidative decomposition reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
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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
- C23C16/401—Oxides containing silicon
- C23C16/402—Silicon dioxide
-
- 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
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
-
- 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
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
- C23C16/0236—Pretreatment of the material to be coated by cleaning or etching by etching with a reactive gas
-
- 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
- C23C16/4554—Plasma being used non-continuously in between 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]
- C23C16/45553—Atomic layer deposition [ALD] characterized by the use of precursors specially adapted for ALD
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
- H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
- H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
- H01L21/76801—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the dielectrics, e.g. smoothing
- H01L21/76822—Modification of the material of dielectric layers, e.g. grading, after-treatment to improve the stability of the layers, to increase their density etc.
Abstract
The invention discloses a preparation method and application of a silicon-based film with a low dielectric constant, which comprises the following steps: (1) Placing the pretreated substrate in a reaction chamber, and pumping the pressure in the reaction chamber to be below 0.1Pa for heating treatment; (2) Introducing a silicon precursor source into the reaction chamber, and carrying out chemical saturation adsorption on the surface of the substrate; the silicon precursor source is one or more of tetramethyldihydro-disiloxane, acetoxy heptamethylcyclotetrasiloxane, methyl-hydro-cyclosiloxane and 2,4, 6-trimethyl-cyclotrisiloxane; (3) Introducing a co-reaction ionization gas source into the reaction chamber for reaction, wherein the co-reaction ionization gas source is one or more of argon, hydrogen and methane; (4) And (4) repeating the steps (2) and (3) to grow the silicon-based film. The preparation process is simple, easy to realize and convenient for large-scale production; the prepared silicon-based film has stable performance, high uniformity and low dielectric constant and can be used as an interlayer medium of a semiconductor device.
Description
Technical Field
The invention relates to the technical field of silicon-based film preparation, in particular to a preparation method and application of a silicon-based film with a low dielectric constant.
Background
With the rapid development of large-scale integrated circuits, the integration level of chips is continuously improved, and the feature size is continuously reduced. The multi-layer routing of metal interconnects leads to an increase in the resistance of metal wires, line-to-line capacitance, and interlayer capacitance, and as the gate width of integrated circuits is scaled down below 10 nanometers, many problems arise, such as an increase in resistance-capacitance (RC) delay, crosstalk noise, power consumption, and the like. Wherein the resistance-capacitance (RC) delay is caused by the increase of parasitic capacitance from the gate to the source/drain, the dielectric constant of the inter-metal interconnection insulating layer is usually decreased to reduce the influence of the parasitic capacitance. In semiconductor devices, low dielectric constant silicon dioxide (SiO) is commonly used 2 ) And silicon nitride (Si) 3 N 4 ) The material serves as a gate spacer that protects the gate stack. Silicon dioxide is used as a gap-fill oxide, interlayer dielectric (ILD) and capping layer in trench isolation, siO 2 The dielectric constant of (2) is 3.9 to 4.2, but the leakage current density is high. And Si 3 N 4 The leakage current of (a) is low, but the dielectric constant thereof is relatively high-5.6.
The interlayer dielectric material of semiconductor device needs to have low dielectric constant and low leakage current density, and the SiO commonly used at present 2 、Si 3 N 4 The requirements of low dielectric constant and low leakage current density cannot be met simultaneously. In order to further improve the integration level and stability of the semiconductor device, it is of great significance to research and prepare a material with low dielectric constant and low leakage current density as an insulating medium between circuits in a chip.
Disclosure of Invention
The invention aims to provide a preparation method and application of a silicon-based film with low dielectric constant, which is applied to SiO 2 Organic groups and terminal hydrogen are introduced into the film, the introduction of C element is beneficial to reducing the dielectric constant of the film, meanwhile, the introduction of the terminal hydrogen generates a nano gap in the film, and under the synergistic effect of the organic groups and the terminal hydrogen, the prepared silicon-based film has a crossed dielectric constant and low leakage current density; and the hair is sentObviously, the silicon-based film prepared by adopting the intermittent ventilation-exhaust mode has good uniformity.
In order to solve the technical problems, the invention provides the following technical scheme:
the invention provides a preparation method of a silicon-based film with a low dielectric constant, which comprises the following steps:
(1) Placing the pretreated substrate in a reaction chamber, and pumping the pressure in the reaction chamber to be below 0.1Pa for heating treatment;
(2) Introducing a silicon precursor source into the reaction chamber after heating treatment, carrying out chemical saturation adsorption on the surface of the substrate, and introducing and discharging nitrogen into and out of the reaction chamber discontinuously after the adsorption is saturated; the silicon precursor source is one or more of tetramethyl dihydro disiloxane, acetoxy heptamethyl cyclotetrasiloxane, methyl-hydrogen-cyclosiloxane and 2,4, 6-trimethyl-cyclotrisiloxane;
(3) Introducing a co-reaction ionization gas source into the reaction chamber for reaction, and intermittently introducing and discharging nitrogen into the reaction chamber after the reaction is completed; the co-reaction ionization gas source is one or more of argon plasma, hydrogen plasma and methane plasma;
(4) And (4) repeating the steps (2) and (3) to grow the silicon-based film.
Further, in the step (1), the substrate is a planar or non-planar surface, and the substrate is made of silicon wafer, silicon dioxide, silicon nitride, silicon hydride, silicon chloride, glass, sapphire, gallium nitride or stainless steel.
Further, in the step (1), HCl and HNO are adopted 3 、H 2 SO 4 Cleaning the substrate with one or more solutions of HF, methanol, acetone, isopropanol, water, or/and using UV-O 3 And processing the surface of the substrate by a cleaning machine to obtain the pretreated substrate.
The substrate is chemically treated by a wet method, so that the roughness of the surface of the substrate can be effectively reduced, pollutants on the surface can be removed, impurities and defects can be reduced, the nucleation condition can be improved, the combination of deposited films can be enhanced, and a smooth and flat film can be obtained; furthermore, UV-O 3 Cleaning machineBy utilizing the photosensitive oxidative decomposition effect of ultraviolet light and ozone generated by the ultraviolet light on organic substances, organic pollutants on most inorganic base materials (such as quartz, silicon wafers, gold, nickel, aluminum, gallium arsenide, aluminum oxide and the like) can be quickly removed, and the adhesion between the base materials and the film layer is improved.
In the step (1), the pressure in the reaction chamber is pumped to be lower than 0.1Pa, the atmosphere in the reaction furnace is removed, the atmosphere contains more impurities, the components are complex and not single, and other impurities are easily introduced into the growing film, so that the application performance of the film is influenced.
Further, in the step (1), the temperature of the heat treatment is 50 to 500 ℃. Heating the reaction chamber to provide energy for the impending chemical reaction, improving the chemical adsorption reaction activity, and causing the thermal cracking reaction of the organic groups of the silicon precursor at an excessively high furnace temperature, thereby generating a chemical side reaction, seriously hindering the progress of the target chemical reaction and failing to grow a high-quality target film; too low furnace temperature will not provide enough energy for chemisorption reaction, and large area uniform target film can not be grown, i.e. the grown film has poor uniformity and can not meet the industrial requirements of downstream industry.
Further, in the step (2), the silicon precursor source is heated at 15-200 ℃ and then is introduced into the reaction chamber, and the time for introducing the silicon precursor source into the reaction chamber is 0.1-10s. The silicon precursor source covers the surface of the substrate and is used as a first reaction precursor source for carrying out chemical saturation adsorption on the surface of the substrate.
Further, in the step (2), after adsorption saturation, introducing nitrogen into the reaction chamber for 1-2 s, and discharging the nitrogen until the pressure in the reaction chamber is less than 0.1Pa, wherein the step is repeated for not less than 10 times.
Further, in the step (3), the co-reaction ionized gas source is obtained by processing a co-reaction gas by an ionization system, and the co-reaction gas is one or more of argon, hydrogen and methane. The method adopts argon, hydrogen and methane as co-reaction gas, and grows the silicon-based film under the condition of not introducing other elements, thereby avoiding the influence of other impurities on the performance of the film.
Further, the ionization system comprises a high-voltage corona plasma generator, an arc plasma generator, a high-frequency induction plasma generator and a microwave plasma generator.
Furthermore, the generated plasma needs to be immediately introduced into the reaction chamber, and if the time is long, the energy of the plasma is attenuated, so that sufficient reaction activity cannot be provided for the next reaction, the reaction is insufficient, and a target film layer cannot be grown.
Further, in the step (3), the time for introducing the co-reaction ionized gas source into the reaction chamber is 0.1-10s; after the reaction is completed, introducing nitrogen into the reaction chamber for 1-2 s, discharging the nitrogen until the pressure in the reaction chamber is less than 0.1Pa, and repeating for no less than 5 times.
The invention adopts a method of intermittently introducing and discharging high-purity nitrogen to remove the precursor which is not chemically adsorbed in the reaction chamber in the step (2) and the byproduct generated by the first chemical adsorption, and remove the co-reaction ionized gas source which is not chemically adsorbed in the reaction chamber in the step (3) and the byproduct generated by the second chemical adsorption, thereby providing a cleaner reaction environment for the next chemical reaction, avoiding the unreacted raw materials and the reaction byproducts from participating in the next chemical reaction, avoiding introducing other impurities, and ensuring that the generated film has controllable components and controllable thickness; in addition, the nitrogen consumption is reduced, and the phenomenon of uneven thickness of the thin film at the outer edge of the substrate and the thin film inside the substrate when the thin film is prepared by the method during continuous nitrogen purging is avoided, so that the uniformity of the thin film is improved.
Further, in the step (4), the thickness of the silicon-based film is 0.1-1000nm.
Further, in the step (4), the dielectric constant of the silicon-based film is not higher than 2.7.
Further, in the step (4), the non-uniformity of the silicon-based thin film is less than 3.
Further, in the step (4), the leakage current density of the silicon-based film is less than 10 -6 A/cm 2 。
In a second aspect, the present invention provides a low dielectric constant silicon-based thin film prepared by the preparation method of the first aspect.
The third aspect of the present invention provides a use of the silicon-based thin film of the second aspect as an interlayer dielectric in a semiconductor device.
According to the invention, the silicon precursor source with a specific structure is adopted, and carbon elements are introduced into the film by using the preparation method, so that Si-C, C-H bonds and the like with low polarizability are formed, the polarizability of the film is reduced, and the dielectric constant of the film is further reduced; meanwhile, terminal hydrogen directly connected with silicon atoms is introduced, and Si-H bond breakage at high temperature introduces nano-voids into the film to reduce the film density and reduce the number of polarized molecules in unit volume so as to reduce the dielectric constant of the film material. Under the synergistic effect of reducing the polarizability of the film material and the number of polarized molecules in unit volume, the prepared silicon-based film has a lower dielectric constant.
Compared with the prior art, the invention has the beneficial effects that:
1. the silicon precursor source with alkyl and terminal hydrogen used in the invention is prepared by adding the precursor into SiO 2 The film introduces a proper amount of carbon element and nano-voids introduced by terminal hydrogen, and effectively reduces SiO under the synergistic effect of the carbon element and the nano-voids 2 The dielectric constant of the film and the dielectric constant of the prepared silicon-based film are not higher than 2.7.
2. According to the invention, a specific silicon precursor source and a coreaction ionization gas source are adopted for reaction, and nitrogen is discontinuously introduced and discharged, so that the prepared silicon-based thin film has a smooth surface and good uniformity, the preparation process is simple and easy to realize, the quality stability of the thin film is good, and the method is suitable for large-scale production; in addition, the prepared silicon-based film has lower dielectric constant and low leakage current density, shows excellent electrical stability, can be used for replacing the traditional silicon dioxide as an interlayer medium of a semiconductor device, and has good application prospect in the field of electronic devices such as the semiconductor device and the like.
Drawings
FIG. 1 is a FT-IR spectrum of a silicon-based film prepared in example 1;
fig. 2 is a graph showing leakage current densities of the silicon-based thin films prepared in example 1.
Detailed Description
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
Example 1
The embodiment relates to a preparation method of a silicon-based film with a low dielectric constant, wherein tetramethyl dihydro disiloxane is used as a silicon precursor source, argon is used as a co-reaction gas, and the preparation method specifically comprises the following steps:
(1) By means of hydrofluoric acid solution (HF: H) 2 O = 1) treating the surface of the silicon wafer, removing the silicon dioxide layer on the surface of the silicon wafer, and improving the adhesive force of the film layer on the silicon wafer; placing the pretreated substrate in a closed high-temperature reaction furnace, pumping the reaction furnace to below 0.1Pa by using a screw dry pump, removing the atmosphere in the reaction furnace, and then raising the furnace temperature of the closed high-temperature reaction furnace to 150 ℃;
(2) Introducing 0.3s of tetramethyldihydro disiloxane into the closed high-temperature reaction furnace, wherein the tetramethyldihydro disiloxane has good volatility, can uniformly cover the surface of the substrate, and is subjected to chemical saturation adsorption on the surface of the substrate; introducing high-purity nitrogen into the sealed high-temperature reaction furnace, wherein the flow rate is 60SCCM, discharging the high-purity nitrogen to below 0.1Pa by using a screw dry pump after introducing for 1s, repeating the process for 10 times, and removing the tetramethyldihydro-disiloxane which is not chemically adsorbed in the sealed reaction furnace and byproducts of the chemical reaction;
(3) Introducing a co-reaction gas Ar into an ionization system to generate an ionization Ar source, wherein the plasma has higher energy, so that the plasma has better reaction activity; introducing a 7s co-reaction ionization Ar source into the closed high-temperature reaction furnace, and carrying out a second-step chemical reaction on the co-reaction ionization Ar source and a first reaction product on the substrate; introducing high-purity nitrogen gas 30SCCM, discharging the high-purity nitrogen gas to be below 0.1Pa by adopting a screw dry pump after introducing for 1s, repeating the process for 5 times, and removing a co-reaction ionized Ar source which is not chemically adsorbed in the closed reaction cavity and a byproduct generated by the second chemical adsorption;
(4) And (4) repeating the steps (2) and (3) to grow the obtained silicon-based film.
The FT-IR spectrum of the prepared silicon-based thin film is shown in FIG. 1, and SiO-C can be observed x And vibrating the peak to show that the silicon-based film is prepared.
Example 2
The embodiment relates to preparation of a silicon-based film with a low dielectric constant, acetoxy heptamethylcyclotetrasiloxane is used as a silicon precursor source, and hydrogen is used as a co-reaction gas, and the preparation method specifically comprises the following operations:
(1) The surface of the silicon wafer substrate is treated by acetone, methanol, isopropanol and water, so that organic impurities on the surface of the silicon wafer can be removed, and the uniformity of a growing film is improved; placing the pretreated substrate in a closed high-temperature reaction furnace, pumping the reaction furnace to below 0.1Pa by using a screw dry pump, removing the atmosphere in the reaction furnace, and then raising the furnace temperature of the closed high-temperature reaction furnace to 170 ℃;
(2) Introducing 1s of acetoxy heptamethylcyclotetrasiloxane into the closed high-temperature reaction furnace, and performing chemical saturation adsorption on the surface of the substrate; introducing high-purity nitrogen into the sealed high-temperature reaction furnace, wherein the flow rate is 50SCCM, discharging the high-purity nitrogen to below 0.1Pa by using a screw dry pump after introducing for 1s, and repeating the process for 15 times;
(3) Co-reaction gas H 2 Introducing into an ionization system to generate ionization H 2 Source, introducing co-reaction ionized H of 7s into a sealed high-temperature reaction furnace 2 A source for causing a second step chemical reaction with the first reaction product on the substrate; introducing high-purity nitrogen gas 30SCCM, introducing for 1s, removing the high-purity nitrogen gas to below 0.1Pa by using a screw dry pump, and repeating the process for 5 times;
(4) And (4) repeating the steps (2) and (3) to grow the obtained silicon-based film.
Example 3
The embodiment relates to preparation of a silicon-based film with a low dielectric constant, which adopts methyl-hydrogen-cyclic siloxane as a silicon precursor source and hydrogen as a co-reaction gas, and comprises the following specific operations:
(1) By UV-O 3 The cleaning machine is used for treating the surface of the silicon wafer substrate, so that organic impurities on the surface of the silicon wafer can be quickly removed, and an ideal substrate environment is provided for the growth of a film layer; placing the pretreated substrate in a closed high-temperature reaction furnace, pumping the reaction furnace to below 0.1Pa by using a screw dry pump, removing the atmosphere in the reaction furnace, and then raising the temperature of the closed high-temperature reaction furnace to 120 ℃;
(2) Introducing 0.5s of methyl-hydrogen-cyclic siloxane into the closed high-temperature reaction furnace to perform chemical saturation adsorption on the surface of the substrate; introducing high-purity nitrogen into the sealed high-temperature reaction furnace at the flow rate of 35SCCM, discharging the high-purity nitrogen to below 0.1Pa by using a screw dry pump after introducing for 2s, and repeating the process for 15 times;
(3) Co-reaction gas H 2 Introducing into an ionization system to generate ionization H 2 Source, 5s of co-reaction ionization H is introduced into a closed high-temperature reaction furnace 2 A source for causing a second step chemical reaction with the first reaction product on the substrate; introducing high-purity nitrogen 35SCCM for 2s, removing the high-purity nitrogen to below 0.1Pa by using a screw dry pump, and repeating the process for 5 times;
(4) And (4) repeating the steps (2) and (3) to grow the obtained silicon-based film.
Example 4
This example relates to the preparation of a low dielectric constant silicon-based film using 2,4, 6-trimethyl-cyclotrisiloxane as the silicon precursor source and hydrogen as the co-reactant gas, and the specific operations are as follows:
(1) By UV-O 3 The cleaning machine is used for treating the surface of the silicon wafer substrate, so that organic impurities on the surface of the silicon wafer can be quickly removed, and an ideal substrate environment is provided for the growth of a film layer; placing the pretreated substrate in a closed high-temperature reaction furnace, pumping the reaction furnace to below 0.1Pa by using a screw dry pump, removing the atmosphere in the reaction furnace, and then raising the furnace temperature of the closed high-temperature reaction furnace to 200 ℃;
(2) Introducing methyl-hydrogen-cyclosiloxane for 1.5s into the closed high-temperature reaction furnace to perform chemical saturation adsorption on the surface of the substrate; introducing high-purity nitrogen into the sealed high-temperature reaction furnace, wherein the flow rate is 55SCCM, discharging the high-purity nitrogen to be below 0.1Pa by using a screw dry pump after introducing for 1s, and repeating the process for 10 times;
(3) Co-reacting gas CH 4 Introducing into an ionization system to generate ionized CH 4 Source, introducing 3s of co-reaction ionized CH into a closed high-temperature reaction furnace 4 A source that is caused to undergo a second step chemical reaction with the first reaction product on the substrate; introducing high-purity nitrogen gas 55SCCM for 1s, removing the high-purity nitrogen gas to below 0.1Pa by using a screw dry pump, and repeating the process for 10 times;
(4) And (4) repeating the steps (2) and (3) to grow the obtained silicon-based film.
Comparative example
In the comparative example, a silicon-based film is prepared by continuously introducing nitrogen, acetoxyheptamethylcyclotetrasiloxane is used as a silicon precursor source, and hydrogen is used as a co-reaction gas, and the specific operation is as follows:
(1) The surface of the silicon wafer substrate is treated by acetone, methanol, isopropanol and water, so that organic impurities on the surface of the silicon wafer can be removed, and the uniformity of a growing film is improved; placing the pretreated substrate in a closed high-temperature reaction furnace, pumping the reaction furnace to below 0.1Pa by using a screw dry pump, and removing the atmosphere in the reaction furnace; raising the furnace temperature of the closed high-temperature reaction furnace to 170 ℃;
(2) Simultaneously introducing 1s of acetoxy heptamethylcyclotetrasiloxane and 50SCCM high-purity nitrogen into a closed high-temperature reaction furnace, and performing chemical saturation adsorption on the surface of the substrate; discharging reaction byproducts and high-purity nitrogen to below 0.1Pa by a screw dry pump and keeping for 15s;
(3) Co-reaction gas H 2 Introducing into an ionization system to generate ionization H 2 A source; generation of H 2 The plasma needs to be immediately introduced into a closed high-temperature reaction furnace; introducing 7s of co-reaction ionization H into the closed high-temperature reaction furnace simultaneously 2 A source and 30SCCM of high purity nitrogen gas to undergo a second chemical reaction with the first reaction product on the substrate; through a screw dry pumpRemoving reaction by-product and high-purity nitrogen gas, keeping the pressure below 0.1Pa for 5s, and removing unreacted co-reaction ionized H in the closed reaction cavity 2 A source and a byproduct from the second chemisorption;
(4) And (4) repeating the steps (2) and (3) to grow the obtained silicon-based film.
Study of Properties
The silicon-based thin films prepared in examples 1 to 4 and comparative example 2 were tested for non-uniformity, relative dielectric constant, and leakage current density, and the results are shown in table 1 below:
TABLE 1 Performance parameters of silicon-based films prepared in examples and comparative examples
| Silicon-based thin film | Non-uniformity (%) | Relative dielectric constant k | Leakage current density (A/cm) 2 ) |
| Example 1 | 2.2 | 2.09 | 5.3×10 -7 |
| Example 2 | 1.9 | 2.70 | 3.1×10 -7 |
| Example 3 | 1.7 | 2.25 | 8.0×10 -7 |
| Example 4 | 2.1 | 2.31 | 8.5×10 -7 |
| Comparative example | 4.5 | 3.39 | 2.0×10 -6 |
As can be seen from the test results of the silicon-based films in Table 1, the uniformity of the silicon-based film prepared by the method of the present invention is superior to that of the film prepared by the comparative example in which nitrogen is continuously introduced, the dielectric constant and the leakage current are both lower than those of the comparative example, and the dielectric constant k is much lower than that of the conventional SiO 2 The silicon-based film prepared by the invention is used as an interlayer medium of a semiconductor device, and the RC delay problem is favorably improved.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitutions or changes made by the person skilled in the art on the basis of the present invention are all within the protection scope of the present invention. The protection scope of the invention is subject to the claims.
Claims (10)
1. A preparation method of a silicon-based film with low dielectric constant is characterized by comprising the following steps:
(1) Placing the pretreated substrate in a reaction chamber, pumping the pressure in the reaction chamber to be below 0.1Pa, and heating;
(2) Introducing a silicon precursor source into the reaction chamber after heating treatment, carrying out chemical saturation adsorption on the surface of the substrate, and introducing and discharging nitrogen into and out of the reaction chamber discontinuously after the adsorption is saturated; the silicon precursor source is one or more of tetramethyldihydro-disiloxane, acetoxy heptamethylcyclotetrasiloxane, methyl-hydro-cyclosiloxane and 2,4, 6-trimethyl-cyclotrisiloxane;
(3) Introducing a co-reaction ionization gas source into the reaction chamber for reaction, and intermittently introducing and discharging nitrogen into the reaction chamber after the reaction is completed; the co-reaction ionization gas source is one or more of argon plasma, hydrogen plasma and methane plasma;
(4) And (4) repeating the steps (2) and (3) to grow the silicon-based film.
2. The method according to claim 1, wherein in the step (1), the substrate is a planar or non-planar surface, and the substrate is made of silicon wafer, silicon dioxide, silicon nitride, silicon hydride, silicon chloride, glass, sapphire, gallium nitride or stainless steel; by using HCl, HNO 3 、H 2 SO 4 Cleaning the substrate with one or more solutions of HF, methanol, acetone, isopropanol, water, or/and using UV-O 3 And processing the surface of the substrate by a cleaning machine to obtain the pretreated substrate.
3. The production method according to claim 1, wherein the temperature of the heat treatment in the step (1) is 50 to 500 ℃.
4. The method according to claim 1, wherein in the step (2), the silicon precursor source is heated at 15-200 ℃ and then introduced into the reaction chamber, and the time for introducing the silicon precursor source into the reaction chamber is 0.1-10s.
5. The preparation method according to claim 1, wherein in the step (2), after the adsorption is saturated, nitrogen is introduced into the reaction chamber for 1 to 2 seconds, and then the nitrogen is discharged until the pressure in the reaction chamber is less than 0.1Pa, and the process is repeated for not less than 10 times.
6. The preparation method according to claim 1, wherein in the step (3), the co-reaction ionization gas source is obtained by processing a co-reaction gas with an ionization system, wherein the co-reaction gas is one or more of argon, hydrogen and methane, and the ionization system comprises a high-voltage corona plasma generator, an arc plasma generator, a high-frequency induction plasma generator and a microwave plasma generator.
7. The method according to claim 1, wherein in the step (3), the co-reaction ionized gas source is introduced into the reaction chamber for 0.1-10s; after the reaction is completed, introducing nitrogen into the reaction chamber for 1-2 s, discharging the nitrogen until the pressure in the reaction chamber is less than 0.1Pa, and repeating for no less than 5 times.
8. The method according to claim 1, wherein in the step (4), the thickness of the silicon-based thin film is 0.1 to 1000nm; the dielectric constant of the silicon-based film is not higher than 2.7.
9. A silicon-based film having a low dielectric constant prepared by the method of any one of claims 1 to 8.
10. Use of a silicon-based film according to claim 9 as an interlayer dielectric in a semiconductor device.
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