CN114231949A - SnO prepared by utilizing atomic layer deposition method2Method for making thin film - Google Patents
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- CN114231949A CN114231949A CN202111584468.6A CN202111584468A CN114231949A CN 114231949 A CN114231949 A CN 114231949A CN 202111584468 A CN202111584468 A CN 202111584468A CN 114231949 A CN114231949 A CN 114231949A
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- 238000000231 atomic layer deposition Methods 0.000 title claims abstract description 31
- 239000010409 thin film Substances 0.000 title abstract description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 57
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 57
- 239000010703 silicon Substances 0.000 claims abstract description 57
- 239000000758 substrate Substances 0.000 claims abstract description 56
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000004140 cleaning Methods 0.000 claims abstract description 24
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 20
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000011261 inert gas Substances 0.000 claims abstract description 13
- 239000006227 byproduct Substances 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000011049 filling Methods 0.000 claims abstract description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 10
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 8
- 238000000137 annealing Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 229910001868 water Inorganic materials 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 238000010926 purge Methods 0.000 claims description 4
- 239000012159 carrier gas Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 239000008213 purified water Substances 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 2
- 239000010408 film Substances 0.000 abstract description 41
- 238000000151 deposition Methods 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 5
- 230000014759 maintenance of location Effects 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- 230000008021 deposition Effects 0.000 description 5
- 238000011109 contamination Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910001887 tin oxide Inorganic materials 0.000 description 4
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000001755 magnetron sputter deposition Methods 0.000 description 3
- 229910000000 metal hydroxide Inorganic materials 0.000 description 3
- 150000004692 metal hydroxides Chemical class 0.000 description 3
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 3
- 239000005416 organic matter Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 244000137852 Petrea volubilis Species 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000010030 laminating Methods 0.000 description 2
- WHXTVQNIFGXMSB-UHFFFAOYSA-N n-methyl-n-[tris(dimethylamino)stannyl]methanamine Chemical compound CN(C)[Sn](N(C)C)(N(C)C)N(C)C WHXTVQNIFGXMSB-UHFFFAOYSA-N 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 229910000410 antimony oxide Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 150000002738 metalloids Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 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
- C23C16/44—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]
-
- 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
- C23C16/407—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/52—Controlling or regulating the coating process
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- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The invention discloses a method for preparing SnO by utilizing an atomic layer deposition method2A method of forming a thin film, which relates to SnO2The technical field of film preparation comprises the following steps of putting a cleaned silicon substrate into a reaction chamber of atomic layer deposition equipment, and vacuumizing the reaction chamber; performing atomic layer deposition cycles in an atomic layer deposition apparatus, i.e. SnO obtainable2A film; filling inert gas into the vacuum reaction chamber, cleaning excessive tin source and reaction by-products, naturally cooling the silicon substrate to room temperature, and taking out; will deposit SnO2The silicon substrate is put into a tube furnace and annealed to obtain uniform SnO2A thin film having SnO prepared by atomic layer deposition2A thin film, the thickness of which can be precisely controlled by the reaction period, and reactingThe method has the advantages of low process temperature, small damage to the substrate layer, accurate and controllable film thickness, good film uniformity, and excellent film-forming shape retention and three-dimensional fitting effects compared with other deposition methods.
Description
Technical Field
The present invention relates to SnO2The technical field of film preparation, in particular to a method for preparing SnO by utilizing an atomic layer deposition method2A method of making a thin film.
Background
The tin oxide film is a thin film of tin oxide, and is characterized by high conductivity, good light transmittance in a visible light wave band, high infrared exclamation rate and ultraviolet absorptivity, the tin oxide film is generally prepared by adopting a chemical vapor deposition or reactive magnetron sputtering method, and is mainly used as a resistor, a photoelectric element, a solar cell, an electroluminescent element, a display, infrared reflection light-transmitting glass and the like, and antimony oxide is often doped in the tin oxide film in order to enhance the transparent conductive effect.
SnO prepared by chemical vapor deposition or reactive magnetron sputtering method2The film is difficult to control the thickness, has poor uniformity, high deposition temperature and poor bonding force with a substrate material, and cannot meet the actual requirement.
Disclosure of Invention
The invention aims to provide a method for preparing SnO by utilizing an atomic layer deposition method2The method for preparing the film comprises the step of preparing SnO by adopting an atomic layer deposition method2The film can accurately control the thickness of the film through a reaction period, has low temperature in the reaction process, small damage to a substrate layer, accurate and controllable thickness and good uniformity, has excellent effects of film forming shape retention and three-dimensional bonding compared with other deposition methods, and solves the problem of SnO prepared by using a chemical vapor deposition or reactive magnetron sputtering method2The film has the problems of difficult thickness control, poor uniformity, high deposition temperature, poor bonding force with a substrate material and incapability of meeting the actual requirement.
In order to achieve the purpose, the invention provides the following technical scheme: SnO prepared by utilizing atomic layer deposition method2A method of making a film comprising the steps of:
step S1: cleaning the silicon substrate by adopting RCA standard, then washing by using deionized water, and drying by using dry nitrogen;
step S2: putting the cleaned silicon substrate into a reaction chamber of atomic layer deposition equipment, and pumping the vacuum degree of the reaction chamber to be below 10-3 Pa;
step S3: tetra (dimethylamino) tin is used as a tin source, the heating temperature of the tin source is 45 ℃, H2O is used as an oxygen source, and the tin source is arranged in an inert gas atmosphereIn which atomic layer deposition cycles are carried out, i.e. SnO is obtained2A film;
step S4: deposited SnO2After the film is formed, filling inert gas into the vacuum reaction chamber, cleaning excessive tin source and reaction by-products, naturally cooling the silicon substrate to room temperature, and taking out;
step S5: will deposit SnO2The silicon substrate is put into a tube furnace and annealed to obtain uniform SnO2A film.
Optionally, the RCA standard cleaning method in step S1 mainly includes the following cleaning solutions; SPM: consists of concentrated sulfuric acid and hydrogen peroxide; hydrofluoric acid; APM, which consists of ammonia water, purified water and hydrogen peroxide; HPM: the silicon substrate is cleaned by an RCA standard cleaning method, and a silanol bond is formed on the surface of the silicon substrate.
Optionally, before the silicon substrate is placed in the reaction chamber of the atomic layer deposition device in step S2, the silicon substrate is preheated by hot air, the temperature of the hot air is 250 to 400 ℃, the flow rate is 500 to 2000 standard liters/minute, and the silicon substrate carrier is preheated to 190 to 250 ℃.
Optionally, in the step S4, the inert gas purging time is 10 to 50S, the flow rate is 10 to 300mL/min, and the system pressure is maintained at 1.5 × 103 to 8 × 103 Pa.
Optionally, in step S3, the pulse time of the tin source and the oxygen source are set to be 0.3S and 0.5S, the exposure time in the chamber is 10S, the exhaust time is 30S, and the flow rate of the carrier gas is 50 sccm.
Optionally, in the step S5, the annealing treatment is performed in a volume ratio of 9: 1, annealing at 500 ℃ for 0.5h in argon-hydrogen mixed gas.
Optionally, the inert gas in step S3 and step S4 is high-purity argon gas with a purity of 99.999%.
Optionally, before the silicon substrate is cleaned in step S1, the surface of the silicon substrate is polished by using water-grinding sandpaper of P400, P600, P800, P1200 and P2000 in sequence.
Compared with the prior art, the invention has the following beneficial effects:
firstly, the invention prepares SnO by adopting an atomic layer deposition method2The film can accurately control the thickness of the film through a reaction period, the temperature in the reaction process is low, the damage to a substrate layer is small, the thickness of the film is accurate and controllable, the uniformity of the film is good, and compared with other deposition methods, the film has the effects of excellent film forming shape retention and three-dimensional laminating property.
The silicon substrate is cleaned by adopting the RCA standard method, heavy organic contamination, partial metal and metal hydroxide attached to the natural oxide film on the surface of the silicon substrate can be removed, and the silicon substrate is cleaned by adopting the RCA standard cleaning method to form a silanol bond on the surface of the silicon substrate, so that the quality of subsequent deposition is improved.
Before cleaning the silicon substrate, the surface of the silicon substrate is polished by using the water-milled sand paper of P400, P600, P800, P1200 and P2000 in sequence, and the surface of the substrate is polished step by adopting the sand paper, so that the surface of the substrate is smoother, the subsequent treatment is convenient, and the deposition quality is improved.
Drawings
FIG. 1 is a process flow diagram of the structure of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
referring to FIG. 1, the present invention provides a method for preparing SnO by atomic layer deposition2A method of making a film comprising the steps of:
step S1: the silicon substrate is cleaned by adopting RCA standard, then is washed by deionized water, and is dried by drying nitrogen, heavy organic contamination and partial metal on the surface of the silicon substrate and metal hydroxide attached to a natural oxidation film can be removed by adopting RCA standard cleaning, and a silanol bond is formed on the surface of the silicon substrate after the silicon substrate is cleaned by adopting RCA standard cleaning method, so that the quality of subsequent deposition is improved.
Step S2: putting the cleaned silicon substrate into a reaction chamber of atomic layer deposition equipment, and pumping the vacuum degree of the reaction chamber to be below 10-3 Pa;
step S3: performing atomic layer deposition circulation in inert gas atmosphere by taking tetra (dimethylamino) tin as a tin source, heating the tin source at 45 ℃, taking H2O as an oxygen source, and obtaining SnO2A film;
step S4: deposited SnO2After the film is formed, filling inert gas into the vacuum reaction chamber, cleaning excessive tin source and reaction by-products, naturally cooling the silicon substrate to room temperature, and taking out;
step S5: will deposit SnO2The silicon substrate is put into a tube furnace and annealed to obtain uniform SnO2A film.
Further, the RCA standard cleaning method in step S1 mainly includes the following cleaning solutions; SPM: consists of concentrated sulfuric acid and hydrogen peroxide; SPM has high oxidizing ability, metal can be dissolved in cleaning liquid after being oxidized, organic matter can be oxidized to generate CO2 and H2O, heavy organic contamination and partial metal on the surface of the silicon wafer can be removed by cleaning the silicon wafer with SPM, but when the organic matter contamination is particularly serious, the organic matter can be carbonized and is difficult to remove, hydrofluoric acid can remove metal hydroxide attached to a natural oxidation film, and when the natural oxidation film is corroded by cleaning with hydrofluoric acid, silicon on the surface of the silicon wafer is hardly corroded; APM, which consists of ammonia water, purified water and hydrogen peroxide, wherein a layer of natural oxide film (SiO2) is arranged on the surface of the silicon wafer and is hydrophilic under the action of the hydrogen peroxide, the surface of the silicon wafer and the particles can be soaked by cleaning liquid, and particles attached to the surface of the silicon wafer fall into the cleaning liquid because the natural oxide layer on the surface of the silicon wafer and Si on the surface of the silicon wafer are corroded by NH4OH, so that the purpose of removing the particles is achieved, and the hydrogen peroxide forms a new oxide film on the surface of the oxidized silicon wafer while NH4OH corrodes the surface of the silicon wafer; HPM: the silicon substrate is cleaned by an RCA standard cleaning method, a silanol bond is formed on the surface of the silicon substrate, silicon is a semiconductor material which is most commonly used widely, monocrystalline silicon has the physical properties of metalloid and has weaker conductivity, the conductivity of the monocrystalline silicon increases along with the rise of the temperature, and the monocrystalline silicon has remarkable semi-conductivity.
Further, before the silicon substrate is placed into the reaction chamber of the atomic layer deposition equipment in the step S2, the silicon substrate is preheated by hot air, the temperature of the hot air is 250-400 ℃, the flow rate is 500-2000 standard liters/minute, the silicon substrate carrier is preheated to 190-250 ℃, and the temperature stabilization time of the substrate material is effectively shortened and the working efficiency is improved by preheating.
Further, in the step S4, the inert gas purging time is 10-50S, the flow rate is 10-300 mL/min, the system pressure is maintained at 1.5 × 103-8 × 103Pa, the purging of excessive tin sources and reaction byproducts is ensured, and the subsequent reaction quality is improved.
Further, in step S3, the pulse time of the tin source and the oxygen source are set to be 0.3S and 0.5S, respectively, the exposure time in the chamber is 10S, the exhaust time is 30S, and the flow rate of the carrier gas is 50 sccm.
Further, in step S5, the annealing treatment is performed at a volume ratio of 9: 1, annealing at 500 ℃ for 0.5h in argon-hydrogen mixed gas, and annealing in argon-hydrogen mixed gas to enable SnO2The film quality is higher.
In the second embodiment, on the basis of the previous embodiment, another embodiment may be:
further, the inert gas in the step S3 and the step S4 is high-purity argon gas with a purity of 99.999%, the argon gas is a rare gas which is widely used in industry, the argon gas is very inert and can not burn and support combustion, the silicon substrate is protected, and the stability of the preparation process is improved.
In the third embodiment, on the basis of the previous embodiment, another embodiment may be:
further, before the silicon substrate is cleaned in step S1, the surfaces of the silicon substrate are polished by using P400, P600, P800, P1200 and P2000 water abrasive paper in sequence, and the substrate is polished step by using the abrasive paper, so that the surface of the substrate is smoother, thereby facilitating subsequent processing and improving the quality of finished products.
Preparation of SnO by Using atomic layer deposition method2The film can accurately control the thickness of the film through a reaction period, the temperature in the reaction process is low, the damage to a substrate layer is small, the thickness of the film is accurate and controllable, the uniformity of the film is good, and compared with other deposition methods, the film has the effects of excellent film forming shape retention and three-dimensional laminating property.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. SnO prepared by utilizing atomic layer deposition method2A method of making a film, comprising the steps of:
step S1: cleaning the silicon substrate by adopting RCA standard, then washing by using deionized water, and drying by using dry nitrogen;
step S2: putting the cleaned silicon substrate into a reaction chamber of atomic layer deposition equipment, and pumping the vacuum degree of the reaction chamber to be below 10-3 Pa;
step S3: taking four-tin as a tin source, heating the tin source at 45 ℃, taking H2O as an oxygen source, and carrying out atomic layer deposition circulation in an inert gas atmosphere to obtain the SnO2The film thickness can be accurately controlled by setting the reaction period;
step S4: deposited SnO2After the film is formed, filling inert gas into the vacuum reaction chamber, cleaning excessive tin source and reaction by-products, naturally cooling the silicon substrate to room temperature, and taking out;
step S5: will deposit SnO2The silicon substrate is put into a tube furnace and annealed to obtain uniform SnO2A film.
2. SnO prepared by atomic layer deposition according to claim 12Film(s)The method of (2), characterized by: the RCA standard cleaning method in the step S1 mainly comprises the following cleaning solutions; SPM: consists of concentrated sulfuric acid and hydrogen peroxide; hydrofluoric acid; APM, which consists of ammonia water, purified water and hydrogen peroxide; HPM: the silicon substrate is cleaned by an RCA standard cleaning method, and a silanol bond is formed on the surface of the silicon substrate.
3. SnO prepared by atomic layer deposition according to claim 12A method of making a film, comprising: and preheating the silicon substrate by hot air before the silicon substrate is placed into the reaction chamber of the atomic layer deposition equipment in the step S2, wherein the temperature of the hot air is 250-400 ℃, the flow rate is 500-2000 standard liters/minute, and the temperature of the silicon substrate carrier is 190-250 ℃.
4. SnO prepared by atomic layer deposition according to any of claims 1 to 32A method of making a film, comprising: in the step S4, the inert gas purging time is 10-50S, the flow rate is 10-300 mL/min, and the system pressure is maintained at 1.5 × 103-8 × 103 Pa.
5. SnO prepared by atomic layer deposition according to claim 12A method of making a film, comprising: in the step S3, the pulse time of the tin source and the oxygen source is set to be 0.3S and 0.5S respectively, the exposure time in the cavity is 10S, the exhaust time is 30S, and the flow rate of the carrier gas is 50 sccm.
6. SnO prepared by atomic layer deposition according to claim 12A method of making a film, comprising: in the step S5, the annealing treatment is performed at a volume ratio of 9: 1, annealing at 500 ℃ for 0.5h in argon-hydrogen mixed gas.
7. SnO prepared by atomic layer deposition according to claim 12A method of making a film, comprising: the inert gas in the step S3 and the step S4 is high-purity argon gas with the purity of 99.999 percent.
8. SnO prepared by atomic layer deposition according to claim 12A method of making a film, comprising: before the silicon substrate is cleaned in step S1, the surface thereof is polished with water-abrasive sandpaper of P400, P600, P800, P1200, and P2000 in this order.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115584483A (en) * | 2022-09-23 | 2023-01-10 | 隆基绿能科技股份有限公司 | Tin dioxide film and preparation method and application thereof |
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| CN109594059A (en) * | 2018-10-31 | 2019-04-09 | 青岛大学 | A kind of atomic layer deposition preparation method of the heterogeneous sensitive thin film for triethylamine detection |
| CN113481485A (en) * | 2021-07-13 | 2021-10-08 | 南方科技大学 | Tin oxide film and preparation method thereof, and solar cell and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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