US20230151488A1 - Tisin coating method - Google Patents
Tisin coating method Download PDFInfo
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- US20230151488A1 US20230151488A1 US17/847,692 US202217847692A US2023151488A1 US 20230151488 A1 US20230151488 A1 US 20230151488A1 US 202217847692 A US202217847692 A US 202217847692A US 2023151488 A1 US2023151488 A1 US 2023151488A1
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- forming
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- tisin
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- nitrogen
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- 238000000576 coating method Methods 0.000 title abstract description 33
- QRXWMOHMRWLFEY-UHFFFAOYSA-N isoniazide Chemical compound NNC(=O)C1=CC=NC=C1 QRXWMOHMRWLFEY-UHFFFAOYSA-N 0.000 title abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 132
- 239000000758 substrate Substances 0.000 claims abstract description 51
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 34
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 34
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 62
- 239000010936 titanium Substances 0.000 claims description 30
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 28
- 239000010703 silicon Substances 0.000 claims description 28
- 238000009792 diffusion process Methods 0.000 claims description 14
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 11
- 230000004888 barrier function Effects 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims description 4
- 229920005591 polysilicon Polymers 0.000 claims description 4
- 239000004065 semiconductor Substances 0.000 claims description 3
- 239000002243 precursor Substances 0.000 claims 10
- 229910021341 titanium silicide Inorganic materials 0.000 claims 7
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims 4
- 229910052581 Si3N4 Inorganic materials 0.000 claims 2
- UGACIEPFGXRWCH-UHFFFAOYSA-N [Si].[Ti] Chemical compound [Si].[Ti] UGACIEPFGXRWCH-UHFFFAOYSA-N 0.000 claims 2
- 125000004122 cyclic group Chemical group 0.000 claims 1
- 238000002207 thermal evaporation Methods 0.000 claims 1
- 239000012495 reaction gas Substances 0.000 abstract description 70
- 239000007789 gas Substances 0.000 abstract description 46
- 239000011248 coating agent Substances 0.000 abstract description 31
- 229910008482 TiSiN Inorganic materials 0.000 abstract description 15
- 238000011010 flushing procedure Methods 0.000 abstract description 10
- 229910008484 TiSi Inorganic materials 0.000 abstract description 4
- 239000010410 layer Substances 0.000 description 52
- 239000011261 inert gas Substances 0.000 description 30
- 239000011162 core material Substances 0.000 description 19
- 238000010438 heat treatment Methods 0.000 description 7
- 238000000231 atomic layer deposition Methods 0.000 description 5
- 229910008045 Si-Si Inorganic materials 0.000 description 4
- 229910006411 Si—Si Inorganic materials 0.000 description 4
- 238000000151 deposition Methods 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- 229910008332 Si-Ti Inorganic materials 0.000 description 3
- 229910007264 Si2H6 Inorganic materials 0.000 description 3
- 229910003910 SiCl4 Inorganic materials 0.000 description 3
- 229910003822 SiHCl3 Inorganic materials 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- 229910006749 Si—Ti Inorganic materials 0.000 description 3
- 229910003074 TiCl4 Inorganic materials 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- PZPGRFITIJYNEJ-UHFFFAOYSA-N disilane Chemical compound [SiH3][SiH3] PZPGRFITIJYNEJ-UHFFFAOYSA-N 0.000 description 3
- 229910052756 noble gas Inorganic materials 0.000 description 3
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 3
- MNWRORMXBIWXCI-UHFFFAOYSA-N tetrakis(dimethylamido)titanium Chemical compound CN(C)[Ti](N(C)C)(N(C)C)N(C)C MNWRORMXBIWXCI-UHFFFAOYSA-N 0.000 description 3
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910003818 SiH2Cl2 Inorganic materials 0.000 description 2
- 229910008479 TiSi2 Inorganic materials 0.000 description 2
- 229910011208 Ti—N Inorganic materials 0.000 description 2
- DFJQEGUNXWZVAH-UHFFFAOYSA-N bis($l^{2}-silanylidene)titanium Chemical compound [Si]=[Ti]=[Si] DFJQEGUNXWZVAH-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000001419 dependent effect Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910004339 Ti-Si Inorganic materials 0.000 description 1
- 229910010978 Ti—Si Inorganic materials 0.000 description 1
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910052729 chemical element Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000012792 core layer Substances 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- BUMGIEFFCMBQDG-UHFFFAOYSA-N dichlorosilicon Chemical compound Cl[Si]Cl BUMGIEFFCMBQDG-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- -1 having Ti—N bonds Chemical compound 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
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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
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
- H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
- H01L21/285—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation
- H01L21/28506—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers
- H01L21/28512—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic Table
- H01L21/28556—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic Table by chemical means, e.g. CVD, LPCVD, PECVD, laser CVD
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45527—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
- C23C16/45531—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 specially adapted for making ternary or higher compositions
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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
- C23C16/34—Nitrides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45563—Gas nozzles
- C23C16/45565—Shower nozzles
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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
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
- H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
- H01L21/0228—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition deposition by cyclic CVD, e.g. ALD, ALE, pulsed CVD
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- 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
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/324—Thermal treatment for modifying the properties of semiconductor bodies, e.g. annealing, sintering
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- H—ELECTRICITY
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/70—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.
- H01L21/76828—Modification of the material of dielectric layers, e.g. grading, after-treatment to improve the stability of the layers, to increase their density etc. thermal treatment
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/70—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
- H01L21/76829—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 characterised by the formation of thin functional dielectric layers, e.g. dielectric etch-stop, barrier, capping or liner layers
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- H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
- H01L2924/01—Chemical elements
- H01L2924/01022—Titanium [Ti]
Definitions
- the diffusion resistance of the layer can be increased by increasing the silicon content.
- the silicon content is increased in the known process, the electric resistance of the deposited layer increases at the same time, so that the properties of the layer are inferior if it should act as a contact layer.
- US 2015/0279683 and U.S. Pat. No. 6,911,391 also relate to a method for deposition of TiSiN layers on substrates.
- FIG. 3 shows the cross section through a gas inlet element of a device illustrated in FIG. 2 ,
- a substrate transport step (wafer transport) 4 the substrate 17 is introduced into the process chamber 10 where the substrate 17 rests on the susceptor 16 .
- the substrate is heated to a process temperature. This takes place by passing an electric current through a wire resistor of the heater 15 .
- a reaction gas containing silicon is first fed into the process chamber 10 (Si) and then the process chamber 10 is flushed by introducing an inert gas (P).
- the second substep 2.2 is carried out a total of k times, where k is preferably greater than 1.
- reaction gas containing Ti is introduced at a partial pressure of less than 12 ⁇ 10 ⁇ 3 millibar; the reaction gas containing Si and having a partial pressure between 1 ⁇ 10 ⁇ 3 and 4 ⁇ 10 ⁇ 3 millibar is introduced and/or the reaction gas containing N is introduced at a partial pressure between 9 ⁇ 10 ⁇ 3 and 8 ⁇ 10 ⁇ 1 millibar.
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- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
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- Computer Hardware Design (AREA)
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- Chemical Vapour Deposition (AREA)
- Electrodes Of Semiconductors (AREA)
- Internal Circuitry In Semiconductor Integrated Circuit Devices (AREA)
- Silicon Compounds (AREA)
Abstract
Description
- This application is a continuation of U.S. patent application Ser. No. 15/612,853 entitled “TiSiN Coating Method,” filed Jun. 2, 2017, the content of which is incorporated by reference in its entirety. Any and all applications for which a foreign or domestic priority claim is identified in the Application Data Sheet as filed with the present application are hereby incorporated by reference under 37 CFR 1.57.
- The invention relates to a method for ALD coating of a substrate with a layer containing Ti, Si, N.
- In the ALD method, a layer consisting of a plurality of chemical elements is deposited on a substrate in several successive cycles. Reaction gases containing at least one element that is to be deposited in the layer are used in this process. In these cycles, layers of the same elements or a group of elements are deposited, layer for layer, a reaction gas being introduced into the process chamber in each case and remaining there in the process chamber until the surface of the substrate has become saturated with the reaction gas. In a subsequent Flush or purge step, the residues of the process gas are removed from the process chamber and the same reaction gas or another reaction gas is introduced into the process chamber. The deposition process takes place at elevated temperatures at which a chemical reaction takes place on the substrate surface; in particular a decomposition reaction of the reaction gas may take place on the substrate surface. Volatile reaction products are removed from the process chamber with the flushing gas.
- The aforementioned document discloses a method for deposition of a diffusion barrier on a layer sequence of an electronic component, for example, a memory component made on silicon substrates, wherein the layer not only serves to limit diffusion but should also be electrically conductive in order to be used as a contact. In a first step a TiN layer is deposited there and then an SiN layer is deposited. The individual cycles are carried out several times one after the other in such a way that a TiSiN layer is formed on the whole.
- The diffusion resistance of the layer can be increased by increasing the silicon content. When the silicon content is increased in the known process, the electric resistance of the deposited layer increases at the same time, so that the properties of the layer are inferior if it should act as a contact layer.
- US 2015/0279683 and U.S. Pat. No. 6,911,391 also relate to a method for deposition of TiSiN layers on substrates.
- Such a method is described in US 2015/0050806 A1.
- The object of the invention is to provide measures with which a diffusion barrier is increased with regard to its diffusion resistance but at the same time the electric conductivity is not impaired.
- This object is achieved by the invention defined in the claims, wherein the dependent claims are not just advantageous refinement of the method defined in the independent claim but also constitute independent approaches to solving the problem, wherein individual subfeatures of the independent claims also have independent inventive significance.
- First and essentially, it is proposed that after an obligatory heating step following transport of the substrate into the process chamber, TiN is deposited on the substrate and/or on a layer already deposited on the substrate, in particular a polysilicon layer. Next an N-free layer or layer sequence of Ti and Si is deposited. Then a TiSiN layer or layer sequence is deposited on the TiS layer. This takes place in three chronologically successive steps, each step being carried out at least once, preferably at least one of these steps or all of these steps being carried out several times in succession. In the first step, a cycle is carried out n times for deposition of TiN, first injecting a reaction gas that contains titanium into the process chamber; then flushing the process chamber with an inert gas; next containing a reaction gas containing nitrogen into the process chamber and finally flushing the process chamber with an inert gas. Nitrogen or argon or some other suitable noble gas or any other suitable gas may be used as the inert gas; n may be 1 but is preferably at least 5. The second step may consist of two substeps, each of which is carried out at least once; but preferably is carried out multiple times. In the first substep a reaction gas containing titanium is injected into the process chamber and then the process chamber is flushed with an inert gas. The first substep may be carried out m times; where m=1, but preferably is at least 5. In the second substep a reaction gas containing silicon is first injected into the process chamber and then the process chamber is flushed with an inert gas. This second substep may be carried out k times; where k=1, but is preferably at least 5. The second step; in which a nitrogen-free area of the coating is essentially preferably deposited; is carried out r times; where r=1, but is preferably at least 10. The third step preferably also consists of two substeps, wherein TiN is deposited in a first substep. To do so, essentially the first step described above is carried out p times. In the first substep of the third step; a reaction gas containing titanium is first injected into the process chamber; then the process chamber is flushed with an inert gas. Next a reaction gas containing nitrogen is injected into the process chamber and then the process chamber is flushed with an inert gas. This first substep of the third step is carried out p times; where p=1, but is preferably at least 2. In the first substep of the third step; a reaction gas containing titanium is first injected into the process chamber. The process chamber is then flushed with an inert gas. Next; a reaction gas containing nitrogen is injected into the process chamber and then the process chamber is flushed with an inert gas. In the first substep of the third step; the coating thus includes an area containing nitrogen. A second substep and in particular the last substep, in which only silicon is deposited by injecting a reaction gas that contains silicon into the process chamber is carried out following the first substep, wherein; here again; a cycle consisting of injecting the reaction gas containing silicon into the process chamber and then flushing the process chamber with the inert gas is carried out q times, where q=1 or preferably is at least S. The third step, in which TiSiN is deposited on the whole, can be carried out r times, where r=1 but preferably is at least 10. It is provided in particular that in carrying out the third step, the reaction gas of the last substep does not contain any nitrogen. As a result of the method according to the invention, an area containing TiN, i.e., having Ti—N bonds, is deposited on the layer of the substrate containing silicon in the first step due to the method according to the invention. A second area, which is a core area in which essentially Si—Si bonds or Si—Ti bonds are formed, is deposited on this first area which is a borderline report [sic; area]. These bonds have a much lower bond energy (approximately 100 eV) than the Ti—N bond in which the bond energy is approximately 450 eV. This method is carried out in particular in such a way that TiSi2 is formed in different phases and has a lower electrical resistance than TiSiN, for example. To this extent, it is advantageous if an N-free component is deposited in the last substep of the third step, wherein the reaction gas does not contain any nitrogen component for this purpose which does not take part in the chemical reaction although N2 can. In the last step a third area of the coating is deposited, this being a borderline region containing nitrogen. The individual layer thicknesses of the three layers are preferably 2 Å to 200 A with the sum total of the three layers being 5 A to 500 A. All three layers could be repeated insitu and in sequence to yield film thicknesses of 5 A to 500 A. The gaseous compounds of titanium, silicon and nitrogen known from the prior art, for example, TiCl4, TDMAT or TDEAT are used as the reaction gases. Dichlorosilane (SiH2Cl2) or SiHCl3, SiCl4, SiH4 or Si2H6 may be used for the reaction gas containing silicon. NH3 or MMH may be used as the reaction gas containing nitrogen. This method begins with heating of the substrate to a temperature of 400° C. to 700° C. at a total pressure in the range between 5 millibar and 0.6 millibar (Equivalent to 0.5 mtorr to 7.5 mTorr). Next the three steps described above are carried out. After cooling the substrate, it is removed from the process chamber. The term substrate as used here in particular is understood to refer to a prestructured and precoated wafer on which a structured silicon-containing layer sequence has already been deposited, for example, a layer sequence of a memory module. The TiSiN coating deposited according to the invention can then be connected by means of wires made of copper or the like.
- The coating is preferably deposited in a reactor that can be evacuated using a vacuum system. Inside the reactor there is a gas inlet element for introducing the reaction gases and/or the inert gas. The gas inlet element may be in the form of a shower head. It may have a plurality of sectors or segments, wherein the segments or sectors form separate chambers into which the reaction gas containing Ti, the reaction gas containing Si or the reaction gas containing N can be injected separately from one another. The gas inlet element may extend over the total area extent of the substrate which sits on a heated susceptor. The gas inlet element may be cooled but it may also be heated. The substrate is preferably sitting on a susceptor which may be heated by a plurality of heating element so that the susceptor has a plurality of heating zones which may be heated independently of one another. A uniform temperature profile can be adjusted on the substrate surface in this way. In particular, a temperature profile with a minimal lateral temperature gradient can be adjusted on the substrate surface.
- In addition, the invention relates to a coating applied to a substrate and having a first borderline region with which the coating is adjacent to the substrate or to a layer applied to the substrate. The coating also has a second borderline region which is opposite the first borderline region and to which a metallic or metal ceramic contact is applied. The second borderline region has a surface area, which comes in contact with the contact material. Between the first borderline region and the second borderline region there is a core region. The inventive coating has the following properties: the first borderline region has a higher nitrogen concentration than the core region. The second borderline region has a higher nitrogen concentration than the core region. The core region is preferably free of nitrogen. The surface area of the second borderline region is preferably free of nitrogen.
- The invention is explained in greater detail below on the basis of exemplary embodiments, in which:
-
FIG. 1 shows the process steps in chronological succession as a block diagram, -
FIG. 2 shows schematically the structure of a reactor for carrying out the process in a type of cross section and -
FIG. 3 shows the cross section through a gas inlet element of a device illustrated inFIG. 2 , -
FIG. 4 shows schematically and on an enlarged scale a layer deposited by the method according to the invention on asubstrate 17. -
FIG. 2 shows schematically the structure of a coating device arranged inside areactor housing 11 that is sealed airtight. A plurality of inlet lines is provided, such that it is possible to feed a gas stream into agas inlet element 12 through each of these feeder lines. Thegas inlet element 12 has a plurality ofgas outlet openings 13 through which the gas fed into thegas inlet element 12 can enter aprocess chamber 10. The bottom of theprocess chamber 10 is formed by the top side of asusceptor 16 on which thesubstrate 17 to be coated sits. Thesusceptor 16 can be heated to a process temperature by means of aheater 15. - The
susceptor 16 may be rotated about an axis of rotation D in its plane of extent. The rotation takes place relative to thegas inlet element 12. Agas outlet 14 to which a vacuum pump is connected is provided. - An inert gas can be fed into a
chamber 18 of thegas inlet element 12 through a feeder line by means of a first mass flow controller 22. A gas containing nitrogen can be fed by means of amass flow controller 23 into achamber 19 separated from the former by an airtight seal. A gas containing titanium can be fed into achamber 20 separated from the former with an airtight seal, by means of amass flow controller 24. A gas containing silicon can be fed into achamber 21 of thegas inlet element 12 by means of amass flow controller 25. -
FIG. 3 shows as an example the spatial arrangement of theindividual chambers gas inlet element 12. The chambers may be arranged like spokes. When thesubstrate 17 is rotated relative to thegas inlet element 12, the reaction gas or inert gas fed into theprocess chamber 10 comes in contact with all regions of the surface of thesubstrate 17. - Semiconductor components for memory element or the like have electrically active layers containing silicon. These layers must be electrically contactable in order to connect the layers to bond wires, for example. A TiSiN coating is applied between the contact and the layer, the process of application of this layer being designed so that the layer has the lowest possible electrical resistance while at the same time forming a high diffusion barrier which prevents the contact metal applied to the TiSiN coating from diffusing into the silicon layer. For deposition of this layer, an ALD method (atomic layer deposition) is used according to the invention. In this method, a reaction gas is fed into the
process chamber 10 in alternation with an insert gas for flushing theprocess chamber 10. This takes place by introducing the respective gas into the cavity in thegas inlet element 12 and discharge the gas from the plurality ofgas outlet openings 13 arranged like a sieve into theprocess chamber 10. The reaction gas is fed into theprocess chamber 10 in such a concentration and over such a period of time until the surface of thesubstrate 17 applied to thesusceptor 16 has become saturated with the reaction gas and/or a reaction product of the reaction gas, for example, a decomposition product. Then the gas residues are flushed out of theprocess chamber 10. This is accomplished by introducing an inert gas into theprocess chamber 10, wherein the inert gas may be nitrogen or a noble gas. - According to the invention the coating is applied in a number of successive coating steps, each of which may in turn comprise substeps and is preferably repeated several times. The process is carried out in such a way that essentially Si—Si bonds or Si—Ti bonds are formed in the core area of the coating so that the coating consists mostly of TiSi2 which has a lower electrical resistance than TiSiN. On the other hand, however, the process is carried out in such a way that the interface facing underneath layer and the interface of the coating having the subsequent layer have a higher nitrogen content than the core region of the coating. The coating consists essentially of three regions, a lower interface connected to the substrate surface and/or the layer containing the silicon there, said interface consisting essentially of TiN, the core region of the coating consisting essentially of Ti and Si and an upper interface consisting essentially of TiSiN.
- The conduct of the process is explained in greater detail below with reference to the accompanying
FIG. 1 . First, in a substrate transport step (wafer transport) 4, thesubstrate 17 is introduced into theprocess chamber 10 where thesubstrate 17 rests on thesusceptor 16. By heating thesusceptor 16 with aheater 15 having a plurality of heating zones, the substrate is heated to a process temperature. This takes place by passing an electric current through a wire resistor of theheater 15. - In a first process step 1, TiN is deposited. To do so, a reaction gas containing Ti is first introduced into the
process chamber 10 until the surface of thesubstrate 17 is saturated with the process gas (Ti). Then residues of the reaction gas containing Ti or its reaction products which do not remain on the surface of thesubstrate 17 are flushed out of theprocess chamber 10 by means of an inert gas (P). Next a reaction gas containing nitrogen is fed into the process chamber until the surface of thesubstrate 17 has been saturated with it (N). Next by introducing the inert gas, the reaction gas containing nitrogen is flushed out of the process chamber 10 (P). These four successive sequences form a first step 1 that is repeater n times resulting in a layer preferably 10 A thick but up to 50 nm thick. - In a second following
step 2 the TiSi core material is deposited. Thissecond step 2 consists of two substeps 2.1,2.2, wherein Ti is deposited in the first substep and Si is deposited in the second substep. In the first substep 2.1, a reaction gas containing Ti is first introduced into the process chamber 10 a total of m times and then gas residues are flushed out of theprocess chamber 10 by introducing an inert gas (P). Following this first substep 2.1 of thesecond step 2 which is carried out at least once but preferably several times, the second substep 2.2 is performed. In this second substep 2.2, a reaction gas containing silicon is first fed into the process chamber 10 (Si) and then theprocess chamber 10 is flushed by introducing an inert gas (P). The second substep 2.2 is carried out a total of k times, where k is preferably greater than 1. - The
second step 2 consisting of the two substeps 2.1 and 2.2 is preferably carried out a total of r times until the required layer thickness of a core layer, which consists of TiSi and is essentially free of nitrogen is deposited, this layer thickness may also be preferably 10 A thick but up to 50 nm. - The
second step 2 is followed by athird step 3 in which TiSiN is deposited. The third step consists of two substeps 3.1,3.2 which follow one another and can be carried out a total of 1 times where 1 is 1 or preferably greater than 1. - The first substep 3.1 of the
third step 3 corresponds essentially to the first step 1. TiN is deposited; so a reaction gas containing titanium is first fed into the process chamber 10 (Ti)f which is then flushed by introducing an inert gas (P). Following that a reaction gas containing nitrogen is introduced into the process chamber 10 (N) whereupon theprocess chamber 10 is again flushed by introducing an inert gas (P). The substep 3.1 can be carried out a total of p times where p=1 or is preferably greater than 1. - The second substep 3.2 of the
third step 3 is carried out without the use of a reaction gas containing N. First the reaction gas containing silicon is fed into the process chamber 10 (Si). Then theprocess chamber 10 is flushed by introducing the inert gas (P)f whereupon the second substep 3.2 of thethird step 3 can be carried out a total of q times where q=1 or is preferably greater than 1. - After cooling the
process chamber 10, thesubstrate 17 is removed from theprocess chamber 10 in a transport step (wafer transport) 4. - The gases mentioned in the introduction are used as the reaction gases, for example; the reaction gas containing Ti may be TiCl4, TDMAT or TDEAT and the reaction gas containing Si may be SiH2Cl2, SiHCl3, SiCl4, SiH4 or Si2H6. The reaction gas containing N may be NH3 or MMH. The inert gas may be N2 or a noble gas.
- Due to the use of a
gas inlet element 12 havingchambers gas inlet element 12 which is in the form of a shower head can be cooled or heated. A thermal equilibrium can be established. Thesusceptor 16 may also be heated or cooled. Theheater 15 is in particular a multizone heater, preferably two heaters being at different distances radially from the center are arranged around the center. Thechambers 19 to 21 may each be flushed with the inert gas in the respective gas change so that no reaction gas remains there. - By means of SiN measurements or XPS measurements, it has been shown that the bonding energy between the individual atoms is much lower in the core region of the layer than in the two interfaces, thus indicating that TiSiN is formed only in the boundary regions and essentially Si—Si and/or Si—Ti is formed in the core region.
-
FIG. 4 shows schematically a section through acoating 30 deposited on asubstrate 17. Thesubstrate 17 is shown only symbolically and includes a silicon wafer with a layer structure deposited on it, wherein the interface of thesubstrate 17 facing thecoating 30 may be a surface of a layer containing silicon. - The
coating 30 consists of afirst boundary region 31, which is deposited directly on the surface of thesubstrate 17, acore region 33, which is connected to thefirst boundary region 31 and asecond boundary region 32, which has asurface 34 to which a contact wire can be connected. - The
layer 30 deposited with the method described previously has afirst interface 31, which has an elevated nitrogen concentration, wherein the nitrogen concentration in thefirst boundary region 31 is greater than that in thecore region 33. Thecore region 33 is preferably essentially free of nitrogen. Thesecond boundary region 32 has a higher nitrogen concentration than thecore region 33. Thesurface 34 is preferably free of nitrogen. - In the
first boundary region 31 and in thesecond boundary region 32, TiSiN compounds with a high bond energy are formed (TiN 455.6 eV). In thecore region 33 essentially Si—Si bonds with a bond energy of 99.6 eV and Ti—Si bonds are formed. Thecoating 30 deposited by the method according to the invention has a high electrical conductivity and forms a high diffusion barrier. It has an essentially crystalline property and a layer thickness of approximately 0.65 nm to 650 nm. - The preceding discussion serves to illustrate the inventions covered by the patent application as a whole, each also independently improving upon the prior art at least through the following combinations of features, wherein two, more or all of these combinations of features may also be combined further, namely:
- A method for ALD coating of a
substrate 17 with a layer containing Ti, Si, N, wherein a reaction gas is fed into aprocess chamber 10 containing thesubstrate 17 in a plurality ofsuccessive steps -
- wherein TiN is deposited in a first step 1 with a reaction gas containing TI and with a reaction gas containing N,
- in a
second step 2 which follows the former step, TiSi is deposited with a reaction gas containing Ti and a reaction gas containing Si, - and in a
third step 3 following thesecond step 2, TiSiN is deposited with a reaction gas containing Ti, with a reaction gas containing N and with a reaction gas containing Si is deposited.
- A method which is characterized in that a cycle consisting of introducing the reaction gas containing Ti, flushing the
process chamber 10 with an inert gas, feeding the reaction gas containing N and flushing theprocess chamber 10 with a reaction gas is carried n times in the first step 1, where n>1. - A method which is characterized in that in the second step 2 a first substep 2.1 consisting of introducing the reaction gas containing Ti and then flushing the
process chamber 10 with an inert gas is carried out m times, where m>1 and in which a second substep 2.2 in which the reaction gas containing Si is introduced into theprocess chamber 10 and then theprocess chamber 10 is flushed with the inert gas, is carried out k times where k>1. - A method which is characterized in that the two substeps 2.1,2.2 are carried out 1 times in succession where 1>1.
- A method which is characterized in that in the third step 3 a first substep 3.1, in which the reaction gas containing Ti is introduced into the
process chamber 10 and then theprocess chamber 10 is flushed with an inert gas, next the reaction gas containing N is introduced into theprocess chamber 10 and then theprocess chamber 10 is flushed with an inert gas is carried out p times where p>1, and in a second substep 3.2 the process gas containing Si is fed into theprocess chamber 10 and next theprocess chamber 10 is flushed with an inert gas wherein the second substep 3.2 is carried out q times in succession, where q>1. - A method which is characterized in that the
third step 3 is carried out r times in succession where r>1. - A method which is characterized in that the reaction gas containing Ti is introduced at a partial pressure of less than 12×10−3 millibar; the reaction gas containing Si and having a partial pressure between 1×10−3 and 4×10−3 millibar is introduced and/or the reaction gas containing N is introduced at a partial pressure between 9×10−3 and 8×10−1 millibar.
- A method that is characterized in that the total pressure inside the
process chamber 10 is in the range between 0.6 and 6 millibar and thesteps - A method which is characterized in that the reaction gas containing Ti is TiCl4, TDMAT or TDEAT and/or the reaction gas containing Si is SiH2Cl2, SiHCl3, SiCl4, SiH4 or Si2H6 and/or the reaction gas containing N is NH3 or MMH.
- A coating which is characterized in that the nitrogen content in the first and second boundary ranges 31, 32 is greater than that in the
core region 33. - A coating which is characterized in that the
core region 33 is essentially free of nitrogen. - A coating which is characterized in that the
surface 34 of the second boundary region facing away from thesubstrate 17 is free of nitrogen. - All the features disclosed here are essential to the invention (either alone or in combination with one another). Thus, the full disclosure content of the respective/attached priority documents (photocopy of the previous patent application) has also been included for the purpose of incorporating features of these documents into the claims in the present patent application). The dependent claims characterized with their features independent inventive refinements of the prior art even without the features of a claim that has been included by way of reference, in particular to compile divisional applications on the basis of these claims. The invention defined in each claim may additionally have one or more of the features defined in the preceding description, in particular features provided with reference numerals and/or cited in the list of reference numerals. The invention also relates to design forms in which individual features of those cited in the preceding description are not implemented, in particular inasmuch as they are recognizably not essential for the respective intended purpose or can be replaced by other means having the same technical effect.
-
List of Reference Numerals 1 Process step 2 Process step 2.1 Substep 2.2 Substep 3 Process step 3.1 Substep 3.2 Substep 4 Transport step 5 Heating step 6 Transport step 10 Process chamber 11 Reactor housing 12 Gas inlet element 13 Gas outlet opening 14 Gas outlet 15 Heater 16 Susceptor 17 Substrate 18 Chamber 19 Chamber 20 Chamber 21 Chamber 22 Mass flow controller 23 Mass flow controller 24 Mass flow controller 25 Mass flow controller 30 Coating 31 Boundary region 32 Boundary region 33 Core region 34 Surface D Axis of rotation k Cycle number l Cycle number m Cycle number n Cycle number p Cycle number q Cycle number r Cycle number
Claims (20)
Priority Applications (1)
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US17/847,692 US20230151488A1 (en) | 2017-06-02 | 2022-06-23 | Tisin coating method |
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US15/612,853 US11401607B2 (en) | 2017-06-02 | 2017-06-02 | TiSiN coating method |
US17/847,692 US20230151488A1 (en) | 2017-06-02 | 2022-06-23 | Tisin coating method |
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US15/612,853 Continuation US11401607B2 (en) | 2017-06-02 | 2017-06-02 | TiSiN coating method |
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US20230151488A1 true US20230151488A1 (en) | 2023-05-18 |
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US15/612,853 Active 2038-03-19 US11401607B2 (en) | 2017-06-02 | 2017-06-02 | TiSiN coating method |
US17/847,692 Abandoned US20230151488A1 (en) | 2017-06-02 | 2022-06-23 | Tisin coating method |
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JP (1) | JP2020522611A (en) |
KR (1) | KR102661268B1 (en) |
CN (1) | CN110800083A (en) |
DE (1) | DE102017114249A1 (en) |
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US11942365B2 (en) | 2017-06-02 | 2024-03-26 | Eugenus, Inc. | Multi-region diffusion barrier containing titanium, silicon and nitrogen |
JP2021031686A (en) * | 2019-08-15 | 2021-03-01 | 東京エレクトロン株式会社 | Film deposition method and film deposition apparatus |
US11587784B2 (en) | 2019-10-08 | 2023-02-21 | Eugenus, Inc. | Smooth titanium nitride layers and methods of forming the same |
US11361992B2 (en) | 2019-10-08 | 2022-06-14 | Eugenus, Inc. | Conformal titanium nitride-based thin films and methods of forming same |
US11832537B2 (en) | 2019-10-08 | 2023-11-28 | Eugenus, Inc. | Titanium silicon nitride barrier layer |
US20230037960A1 (en) * | 2020-01-15 | 2023-02-09 | Tokyo Electron Limited | Film forming method, film forming device, and method for manufacturing semiconductor device |
CN113035776A (en) * | 2021-03-11 | 2021-06-25 | 长鑫存储技术有限公司 | Semiconductor structure and preparation method thereof |
TW202334482A (en) * | 2021-12-03 | 2023-09-01 | 美商應用材料股份有限公司 | Nh radical thermal nitridation to form metal silicon nitride films |
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2018
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- 2018-05-31 CN CN201880034943.2A patent/CN110800083A/en active Pending
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- 2018-06-01 TW TW107119067A patent/TWI791529B/en active
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KR102661268B1 (en) | 2024-04-26 |
TW201908510A (en) | 2019-03-01 |
US20180347040A1 (en) | 2018-12-06 |
KR20200004426A (en) | 2020-01-13 |
DE102017114249A1 (en) | 2018-12-06 |
TWI791529B (en) | 2023-02-11 |
CN110800083A (en) | 2020-02-14 |
WO2018222920A1 (en) | 2018-12-06 |
JP2020522611A (en) | 2020-07-30 |
US11401607B2 (en) | 2022-08-02 |
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