CN111607780A - Atomic layer deposition method for surface of three-dimensional bluff body - Google Patents
Atomic layer deposition method for surface of three-dimensional bluff body Download PDFInfo
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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]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- C23C16/405—Oxides of refractory metals or yttrium
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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
- C23C16/52—Controlling or regulating the coating process
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Abstract
The invention relates to the field of atomic deposition, in particular to a three-dimensional bluff body surface atomic layer deposition method. The invention provides a three-dimensional bluff body surface atomic layer deposition method, which comprises the following steps: introducing a fluid containing a reaction source into a reaction cavity, and carrying out atomic deposition reaction in the surface of a device to be treated, wherein a quantitative parameter Z of reaction gas in the reaction cavity meets the following conditions: and Z is not less than 8.5 and not more than (TV/Phi) and not more than 1359.5. The invention can maintain the integral laminar flow condition in the reaction cavity by controlling the quantitative parameters, the gas development distance, the Rayleigh number and other conditions related to the atomic layer deposition reaction cavity and controlling the adjustment of the quantitative Z, thereby ensuring the establishment of the integral laminar flow condition in the reaction zone, the rapid and effective transportation of reactant molecules and the rapid discharge of reaction byproducts during the deposition of the atomic scale film on the surface of the three-dimensional bluff body.
Description
Technical Field
The invention relates to the field of atomic deposition, in particular to a three-dimensional bluff body surface atomic layer deposition method.
Background
In the development of modern science and technology, particularly in the development of nano science and technology, almost all relevant applications relate to nano coating technology aiming at realizing various surface functions, particularly nano coating technology capable of controlling thickness at atomic scale. In the selection of the coating method, although the wet chemical method under the liquid phase condition has low cost, a uniform and compact high-quality nano coating layer with the same thickness is difficult to form. The currently widely used nano-coating technology is based on the nano-coating technology under the gas phase condition, such as physical vapor deposition, chemical vapor deposition, atomic layer deposition, and the like. The atomic layer deposition technology has a unique surface self-limiting growth mechanism, and the application range of the atomic layer deposition technology is rapidly expanded along with the development of semiconductor and microelectronic industries in recent years.
The atomic layer deposition technology adopts modes and mechanisms of orderly and alternately transporting reactant molecules, self-limiting surface growth, stepping surface covering and the like to control the gas-phase chemical reaction on the surface of an object, thereby realizing the accurate control of the growth rate of the film in nanometer/sub-nanometer scale. Currently, atomic layer deposition techniques are irreplaceable in applications requiring the preparation of a variety of thin film materials that are ultra-thin, highly uniform, and excellent in shape retention. As such, atomic layer deposition techniques have a wide range of applications. With incomplete statistics, the use of atomic layer deposition techniques has grown exponentially over the past decade, and this approach has now been widely used in semiconductor and related industries, such as: integrated circuits, sensors, III-V devices, micro/nano-electromechanical systems manufacturing, optical devices and optoelectronic engineering, anti-rust and wear resistant materials, and renewable energy applications (e.g. solar). Other large-scale applications include corrosion protection, energy storage and production (e.g., advanced thin film batteries and fuel cells), flexible electronic moisture or gas sealing coatings, biocompatible coatings for medical devices and implants, water purification, advanced lighting devices (e.g., LEDs), ecological packaging materials, decorative coatings, glass anti-splinters, water-resistant coatings, and the like.
From the material preparation point of view, in the nano coating technology represented by atomic layer deposition, the application objects are basically limited to streamline substrates (i.e. flat substrates), such as silicon wafers, quartz wafers, glass wafers and the like. The main reason is that the nano-coating technology is developed under the continuous development of the semiconductor and microelectronic industries, and the main carrier of the modern semiconductor and microelectronic industries is various flat substrates. From the viewpoint of process control related to the vapor-phase nano-coating technology, in the atomic layer deposition technology, the transport of reactant molecules, the surface and interface physicochemical reactions, and the discharge of reaction byproducts and impurities all occur in a flowing gas environment. The hydrodynamic environment of the gas in the reaction chamber then constitutes the global environment for the growth of the thin film on the surface of the substrate and plays a crucial role in the process control of the coating and the final quality of the film.
The hydrodynamic environment in the reaction chamber is actually the result of the interaction of the reaction chamber design, substrate shape and size, substrate surface state, coating parameter control (temperature, pressure, gas flow rate), and other factors. When the vapor phase nano coating technology is expanded to a three-dimensional bluff body (namely a non-flat substrate), the bluff body replaces the original flat streamlined body, so that the aerodynamic environment in the reaction cavity is fundamentally changed. One of the most important changes is that the aerodynamic boundary layer is separated from the surface of the three-dimensional bluff body. At this time, the transport of reactant molecules, physical and chemical mechanisms associated with surface film growth, control of film growth, and final coating quality are all severely affected. In fact, the surface self-limiting growth mechanism and the stepwise film coating method involved in the conventional atomic layer deposition technology are not unconditionally generated, but are strictly limited to the aerodynamic condition that the aerodynamic boundary layer is not separated from the surface of the plated substrate. In the conventional atomic layer deposition application of the flat substrate, the aerodynamic boundary layer can not be separated from the surface of the substrate, so that the role of the aerodynamic factors in the control of the atomic layer deposition process is neglected for a long time. When the atomic layer deposition technology is expanded to the surface of the three-dimensional blunt body, the parameter control (including temperature, vacuum degree, gas flow rate and the like) of the traditional atomic layer deposition can not ensure the self-limiting and step-by-step film growth of the surface of the whole blunt body, and the necessary correction is carried out on the deposition process on the basis of the consideration of the separation factor of the aerodynamic interface layer, so that the surface self-limiting growth mechanism and the step-by-step film coating mode can be realized on the surface of the three-dimensional blunt body. In addition, besides the influence caused by the boundary layer separation, the intervention of the three-dimensional macroscopic blunt body can also cause the influence of various other complex factors on the nano coating film under the gas phase condition. For example, turbulence of the gas in the reaction chamber. Once the turbulence is formed, the transport of the reaction material and the transport of the reaction by-products and impurities are affected to different degrees, thereby affecting the quality of the coating film. Therefore, besides the separation factor of the gas boundary layer, when the atomic layer deposition coating is carried out on the surface of the three-dimensional bluff body, the whole design of the reaction cavity is also involved so as to ensure the laminar flow condition in the whole cavity as far as possible and avoid the formation of turbulent flow.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, it is an object of the present invention to provide a three-dimensional passive surface atomic layer deposition method for solving the problems of the prior art.
The invention provides a three-dimensional bluff body surface atomic layer deposition method in a first aspect, which comprises the following steps: introducing a fluid containing a reaction source into a reaction cavity, and carrying out atomic deposition reaction in the surface of a device to be treated, wherein a quantitative parameter Z of reaction gas in the reaction cavity meets the following conditions:
8.5≤Z＝(TV/PФ)≤1359.5
wherein,
t is the temperature in the reaction cavity, and the unit can be;
p is the vacuum degree in the reaction cavity and the unit is Torr;
v is the gas flow in the reaction cavity and the unit is sccm;
phi is the perimeter of the cross section of the reaction cavity and the unit is cm.
In some embodiments of the invention, the reaction source is selected from atomic layer deposition reaction sources.
In some embodiments of the invention, the reaction source is selected from trimethylaluminum TMA, diethylzinc DEZn, titanium tetrachloride TiCl, TiCl4One or more of the above.
In some embodiments of the invention, the source of reaction is present in the source-containing fluid in an amount of 0.1to 20 wt%.
In some embodiments of the invention, the carrier gas in the fluid containing the reaction source is an inert gas.
In some embodiments of the invention, the shape of the device to be processed is matched to the shape of the reaction chamber.
In some embodiments of the present invention, the distance between the device to be processed and the inner wall of the reaction chamber satisfies the following condition:
ΔTgH3/Tavv α is less than or equal to 109 and H is more than or equal to 0.1cm
Wherein,
v in the formula represents the aerodynamic viscosity of the gas in m2/s；
g is a gravity constant;
h is the distance between the surface of the device to be processed and the inner wall of the reaction cavity, and the unit is cm;
delta T is the difference between the surface temperature of the device to be processed and the surface temperature of the inner wall of the reaction cavity, and the unit is;
Tavis the average temperature in the reaction zone, and the unit is;
α is the gas thermal diffusion constant in cm2/s。
In some embodiments of the present invention, the distance between the device to be treated and the fluid inlet of the reaction chamber generally satisfies the following condition:
(Len)≥0.03ReD. len is less than or equal to 50 cm;
wherein,
len is the distance between the device to be processed and the fluid inlet of the reaction cavity, and the unit is cm;
re is the Reynolds number of the fluid at the fluid inlet of the reaction cavity;
d is the fluid diameter of the cross section of the reaction cavity and the unit is cm.
In some embodiments of the invention, the fluid containing the reaction source is also subjected to a feed gas rectification process, which generally satisfies the following conditions:
(d2-d1)V≤1.26ФLd；
wherein,
d1the unit is the fluid diameter of a fluid inlet in the air inlet rectification treatment, and the unit is cm;
d2the unit is the fluid diameter of a fluid outlet in the air inlet rectification treatment, and the unit is cm;
v is the gas flow of the reaction device, and the unit is sccm;
phi is the perimeter of a fluid outlet during intake rectification treatment and the unit is cm;
Ldthe length from the fluid inlet to the fluid outlet in the intake air rectification treatment is expressed in cm.
In some embodiments of the present invention, the fluid that is led out of the reaction chamber is also subjected to an outlet rectification process, which generally satisfies the following conditions:
(d1’-d2’)V’≤1.26Ф’Ld’；
wherein,
d1' is the fluid diameter of the fluid inlet in cm during the treatment of gas outlet rectification;
d2' is the fluid diameter of the fluid outlet in cm during the treatment of the gas outlet rectification;
v' is the gas flow of the reaction device, and the unit is sccm;
phi' is the perimeter of the fluid inlet during the gas outlet rectification treatment, and the unit is cm;
Ld' is the length from the fluid inlet to the fluid outlet in cm during the treatment of the outgoing gas rectification.
Drawings
FIG. 1 is a schematic diagram illustrating operation of an embodiment of the present invention.
FIG. 2 is a schematic diagram of the experimental results of the embodiment of the present invention.
Detailed Description
The inventor of the invention provides a method suitable for atomic layer deposition on the surface of a three-dimensional bluff body by controlling the quantitative parameters, the gas development distance, the Rayleigh number and other conditions related to an atomic layer deposition reaction cavity, and the invention is completed on the basis.
The invention provides a three-dimensional bluff body surface atomic layer deposition method, which comprises the following steps: introducing a fluid containing a reaction source into a reaction cavity, and carrying out atomic deposition reaction on the surface of a device to be treated, wherein a quantitative parameter Z of reaction gas in the reaction cavity meets the following conditions:
8.5≤Z＝(TV/PФ)≤1359.5
wherein,
t is the temperature in the reaction chamber, which can be expressed in units of degrees celsius, usually the temperature of the fluid in the chamber, and can usually be measured in the middle of the stream in the reaction chamber;
p is the vacuum degree in the reaction cavity, and the unit can be Torr;
v is the gas flow in the reaction chamber, and the unit can be sccm (standard-state cubicrefractory injector per minute);
phi is the perimeter of the cross section of the reaction cavity, and the unit can be cm (centimeter).
In the three-dimensional bluff body surface atomic layer deposition method provided by the invention, the integral laminar flow condition in the reaction cavity is established and maintained by controlling the amount Z, for example, most areas in the reaction cavity can meet the laminar flow condition, for example, the area for placing a device to be processed can maintain the laminar flow condition, and the Reynolds number (R) of the fluid containing the reaction source in the reaction cavitye) Usually between 10 and 1600 (i.e. 10-1600, 10-20, 20-50, 50-100, 100-200, 200-300, 300-500, 500-1000, or 1000-1600), Re can be adjusted to a corresponding range by controlling Z, further, Φ can be adjusted by adjusting the design of the reaction chamber, and further, the control amount Z can be maintained within a certain range by adjusting V, P, T parameters in the reaction chamber. In some embodiments of the present invention, T can be 20-500 deg.C, 20-30 deg.C, 30-50 deg.C, 50-100 deg.C, 100-. In other embodiments of the present invention, P may be 0.01 to 700Torr, 0.01 to 0.1Torr, 0.1to 1Torr, 1to 5Torr, 5to 10 TorrTorr, 10-20Torr, 20-50Torr, 50-100Torr, 100-. In other embodiments of the present invention, V can be 1-5000sccm, 1-5sccm, 5-10sccm, 10-50sccm, 50-100sccm, 100-. In other embodiments of the invention, Φ generally needs to be related based on the specific cavity, for example, Φ can be 10-300cm, 10-20cm, 20-30cm, 30-50cm, 50-100cm, 100 + 150cm, 150 + 200cm, 200 + 300 cm.
In the three-dimensional body surface atomic layer deposition method provided by the invention, the fluid containing the reaction source generally comprises the carrier gas and the reaction source, and the type and content of the reaction source in the fluid containing the reaction source can be determined by those skilled in the art according to the type of the surface atomic layer to be deposited, for example, the reaction source can be various atomic layer deposition reaction sources, and specifically can be, but not limited to, trimethylaluminum TMA, diethylzinc DEZn, titanium tetrachloride TiCl4And the like, and the content of the reactive source in the fluid containing the reactive source may be 0.1to 20 wt%, 0.1to 1 wt%, 1to 3 wt%, 3 to 5 wt%, 5to 10 wt%, 10 to 15 wt%, or 15 to 20 wt%. The carrier gas is typically an inert gas, which generally refers to a gaseous substance that does not chemically react with the main substance in the reaction system (e.g., the reaction source, the object to be deposited, the reaction chamber, etc.), for example, the inert gas may be a combination of one or more of nitrogen, helium, neon, argon, krypton, xenon, etc.
In the three-dimensional bluff body surface atomic layer deposition method provided by the invention, the reaction cavity generally extends along the fluid flowing direction (which can be the flowing direction of the fluid at the center of the stream), the reaction cavity generally is a cavity with uniformly changed size and shape, for example, the reaction cavity can be a column (for example, an elliptic column, a cylinder, a cuboid and other polygonal columns) with the axis consistent with the fluid flowing direction at the inlet of the reaction cavity, the fluid inlet of the reaction cavity and the fluid outlet of the reaction cavity are generally located at two ends of the cylindrical reaction cavity, and more specifically, can be symmetrically located at two ends of the cylindrical reaction cavity respectively; for another example, the reaction chamber may also be a cylinder whose axis is perpendicular to the fluid flowing direction (for example, an elliptic cylinder, a rectangular parallelepiped, or other polygonal cylinder), and the fluid inlet of the reaction chamber and the fluid outlet of the reaction chamber are respectively located at two sides of the cylindrical reaction chamber, and more specifically, may be symmetrically located at two sides of the cylindrical reaction chamber respectively. The shape of the fluid inlet of the reaction cavity may be circular, oval, polygonal (e.g., triangular, rectangular, rhombic, pentagonal, hexagonal, etc.) and other various shapes, the shape of the fluid outlet of the reaction cavity may be circular, oval, polygonal (e.g., triangular, rectangular, rhombic, pentagonal, hexagonal, etc.) and other various shapes, the shape of the fluid inlet of the reaction cavity may be the same as or different from that of the fluid outlet of the reaction cavity, and the plane where the fluid inlet of the reaction cavity is located may be parallel to the plane where the fluid outlet of the reaction cavity is located. The size of the fluid inlet of the reaction chamber and/or the fluid outlet of the reaction chamber may correspond to the size of the cross-section of the reaction chamber, for example, the size of the fluid inlet of the reaction chamber and/or the fluid outlet of the reaction chamber may be equal to or smaller than the cross-section of the reaction chamber (cross-section of the reaction chamber relative to the fluid inlet of the reaction chamber).
In the atomic layer deposition method for the surface of the three-dimensional bluff body provided by the invention, the device to be processed can be various devices suitable for surface atomic layer deposition in the field, the device to be treated may in particular be a three-dimensional bluff body, which is generally referred to as a non-planar bluff body, which is generally referred to as a bluff body, for example, it may be cylindrical, spherical, etc., and the cross-section of the cylinder may be, for example, circular, elliptical, polygonal (e.g., triangular, rectangular, diamond, pentagonal, hexagonal, etc.), etc., and one skilled in the art can generally select a suitable shape of the reaction chamber, so that the shape of the device to be treated can be matched with the shape of the reaction chamber, for example, the shape of the reaction chamber is generally, when the device to be treated is a cylinder, the cylindrical reaction cavity can be used, and when the device to be processed is a cuboid, the cuboid reaction cavity can be used.
In the three-dimensional bluff body surface atomic layer deposition method provided by the invention, a device to be processed generally needs to keep a proper distance from the inner wall of the reaction cavity, and the distance between the device to be processed and the inner wall of the reaction cavity generally meets the following conditions:
ΔTgH3/Tavv α is less than or equal to 109 and H is more than or equal to 0.1cm
Wherein ν in the formula denotes the aerodynamic viscosity of the gas in m2/s；
g is the gravitational constant (i.e., 9.8N/kg);
h is the distance between the surface of the device to be processed and the inner wall of the reaction cavity, and the unit can be cm;
delta T is the difference between the surface temperature of the device to be processed and the surface temperature of the inner wall of the reaction cavity, and the unit can be;
Tavthe average temperature in the reaction zone can be expressed in units of ℃;
α is the gas thermal diffusion constant, and can be in cm2(e.g., nitrogen has a gas thermal diffusion constant of 0.185 cm)2/s)。
In the three-dimensional bluff body surface atomic layer deposition method provided by the invention, a device to be processed generally needs to keep a proper distance from the inner wall of the reaction cavity, specifically, the distance between the surface of the device to be processed and the inner wall of the reaction cavity can not be too large or too small, so that the device to be processed can be positioned at a relatively stable part in a fluid in the reaction cavity, and the relatively stable state of the fluid in the reaction cavity can be kept. The Δ T typically depends on the sample heating and insulation means, and the v typically depends on the nature of the carrier gas. In other embodiments of the present invention, TavCan be 20-500 ℃, 20-30 ℃, 30-50 ℃, 50-100 ℃, 100-.
In the three-dimensional bluff body surface atomic layer deposition method provided by the invention, a device to be processed is usually kept at a certain distance from a fluid inlet of a reaction cavity, and the distance between the device to be processed and the fluid inlet of the reaction cavity usually meets the following conditions:
(Len)≥0.03ReD. len is less than or equal to 50 cm;
len is the distance between the device to be processed and a fluid inlet of the reaction cavity, and the unit can be cm;
re is the Reynolds number of the fluid at the fluid inlet of the reaction cavity;
d is the fluid diameter of the cross section of the reaction chamber, and may be expressed in cm, more specifically, the fluid diameter of the cross section at the fluid inlet of the reaction chamber (D ═ 4 × the area of the cross section of the reaction chamber/the perimeter of the cross section of the reaction chamber), which is the cross section of the reaction chamber relative to the fluid inlet of the reaction chamber.
In the three-dimensional bluff body surface atomic layer deposition method provided by the invention, the device to be processed is usually kept a certain distance away from the fluid inlet of the reaction cavity, so that a sufficient distance is kept for forming a stable stream (for example, gas flow) after the fluid containing the reaction source enters the reaction cavity, and further, a stable overall laminar flow condition can be formed, so that the device to be processed can be positioned in a stable laminar flow area. In some embodiments of the present invention, the Re at the fluid inlet is typically 10-1600, 10-20, 20-50, 50-100, 100-. In other embodiments of the present invention, D may be 3-30cm, 3-5cm, 5-10cm, 10-15cm, 15-20cm, 20-25cm, or 25-30 cm.
In the three-dimensional bluff body surface atomic layer deposition method provided by the invention, the gas inlet rectification treatment can be carried out on the fluid containing the reaction source, and the gas inlet rectification treatment generally meets the following conditions:
(d2-d1)V≤1.26ФLd；
wherein,
d1the fluid diameter of the fluid inlet for the intake air rectification treatment may be generally expressed in cm for the fluid inlet for the intake air rectification treatment (4 × the area of the fluid inlet for the intake air rectification treatment/the circumferential length of the fluid inlet for the intake air rectification treatment), for example, the fluid diameter may be expressed in (4 × the area/the circumferential length) for a circular (including elliptical) inlet and/or outlet, and the fluid diameter may be expressed in (2 × side length 1 × side length 2/(side length 1+ side length 2)) for a rectangular inlet and/or outlet;
d2the fluid diameter of the fluid outlet in the intake air rectification treatment is expressed in cm, and the fluid diameter of the fluid outlet in the intake air rectification treatment can be generally (4 × area of the fluid outlet in the intake air rectification treatment/perimeter of the fluid outlet in the intake air rectification treatment);
v is the gas flow of the reaction device, and the unit is sccm;
phi is the perimeter of a fluid outlet during intake rectification treatment and the unit is cm;
Ldthe length from the fluid inlet to the fluid outlet in cm is used for the intake air rectification treatment, and the center of the outlet and the inlet can be generally used as a reference when calculating the length of the pipeline between the fluid inlet and the fluid outlet.
In the three-dimensional bluff body surface atomic layer deposition method provided by the invention, the air inlet rectification treatment is specifically that fluid containing a reaction source is introduced into a rectification device for rectification treatment, the fluid subjected to the air inlet rectification treatment can be further introduced into the reaction cavity, and the air inlet rectification treatment can prevent the fluid containing the reaction source from generating turbulence and/or backflow, so that the fluid containing the reaction source is more stable, and the integral laminar flow condition can be further formed in the reaction cavity. In some embodiments of the invention, d1Can be 0.7-10 cm, 0.7-1 cm, 1-2 cm, 2-3 cm, 3-5cm, or 5-10 cm. In other embodiments of the present invention, d2Can be 5-100 cm, 5-10cm, 10-20cm, 20-30cm, 30-50cm, 50-70 cm, or 70-100 cm. In other embodiments of the present invention, V can be 10-1000 sccm, 10-20 sccm, 20-30 sccm, 30-50 sccm, 50-100sccm, 100-200sccm, 200-300 sccm, 300-500 sccm, or 500-1000 sccm. In other embodiments of the present invention, Φ may be 15 to 157cm, 15 to 20cm, 20to 30cm, 30 to 50cm, 50to 70cm, 70 to 100cm, or 100to 157 cm. In other embodiments of the present invention, LdCan be 10-200 cm, 10-20cm, 20-30cm, 30-50cm, 50-70 cm, 70-100 cm, 100-150cm, or 150-200 cm.
In the three-dimensional bluff body surface atomic layer deposition method provided by the invention, the fluid led out of the reaction cavity can be subjected to gas outlet rectification treatment, and the gas outlet rectification treatment generally meets the following conditions:
(d1’-d2’)V’≤1.26Ф’Ld’；
wherein,
d1' is the fluid diameter of the fluid inlet in cm during the gas outlet rectification treatment, and the fluid diameter of the fluid inlet during the gas outlet rectification treatment can be generally (4 × the area of the fluid inlet during the gas outlet rectification treatment/the perimeter of the fluid inlet during the gas outlet rectification treatment);
d2' is the fluid diameter of the fluid outlet in cm during the outlet rectification treatment, and the fluid diameter of the fluid outlet during the outlet rectification treatment can be generally (4 × area of the fluid outlet during the outlet rectification treatment/perimeter of the fluid outlet during the outlet rectification treatment);
v' is the gas flow of the reaction device, and the unit is sccm;
phi' is the perimeter of the fluid inlet during the gas outlet rectification treatment, and the unit is cm;
Ld' the length from the fluid inlet to the fluid outlet in cm in the treatment of rectification of the gas outlet, and the center of the outlet and the inlet can be generally used as a reference when calculating the length of the pipeline between the fluid inlet and the fluid outlet.
In the three-dimensional bluff body surface atomic layer deposition method provided by the invention, the gas outlet rectification treatment is specifically that the fluid in the reaction cavity is introduced into the gas outlet rectification device for gas outlet rectification treatment and is further discharged out of the reaction system, and the gas outlet rectification treatment can prevent turbulent flow and/or backflow when the fluid in the reaction cavity is led out of the reaction cavity, so that the fluid in the reaction cavity can be more stable, and the condition of forming integral laminar flow in the reaction cavity can be further maintained. In some embodiments of the invention, d1The' can be 5to 100cm, 5to 10cm, 10 to 20cm, 20to 30cm, 30 to 50cm, 50to 70cm, or 70 to 100 cm. In other embodiments of the present invention, d2The' can be 0.7 to 10cm, 0.7 to 1cm, 1to 2cm, 2 to 3cm, 3 to 5cm, or 5to 10 cm. In other embodiments of the present invention, V' may be10 to 1000sccm, 10 to 20sccm, 20to 30sccm, 30 to 50sccm, 50to 100sccm, 100to 200sccm, 200to 300sccm, 300to 500sccm, or 500to 1000 sccm. In other embodiments of the present invention, Φ' may be 15 to 157cm, 15 to 20cm, 20to 30cm, 30 to 50cm, 50to 70cm, 70 to 100cm, or 100to 157 cm. In other embodiments of the present invention, LdThe' may be 10 to 200cm, 10 to 20cm, 20to 30cm, 30 to 50cm, 50to 70cm, 70 to 100cm, 100to 150cm, or 150 to 200 cm.
The atomic layer deposition method for the surface of the three-dimensional bluff body is a method for ensuring the establishment of integral laminar flow conditions in a reaction cavity and inhibiting the separation of an aerodynamic boundary layer of the surface of the bluff body based on aerodynamic calculation, and can be applied and implemented through the design of the reaction cavity meeting related conditions.
The invention can maintain the integral laminar flow condition in the reaction cavity by controlling the quantitative parameters, the gas development distance, the Rayleigh number and other conditions related to the atomic layer deposition reaction cavity and controlling the adjustment of the quantitative Z, thereby ensuring the establishment of the integral laminar flow condition in the reaction zone, the rapid and effective transportation of reactant molecules and the rapid discharge of reaction byproducts during the deposition of the atomic scale film on the surface of the three-dimensional bluff body. On the other hand, the design also inhibits the gas backflow, thereby avoiding the backflow of redundant reactant molecules and reaction byproduct molecules and avoiding the pollution to the substrate surface, the cavity and the gas transportation system caused by the backflow.
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
It is to be understood that the processing equipment or apparatus not specifically identified in the following examples is conventional in the art.
Furthermore, it is to be understood that one or more method steps mentioned in the present invention does not exclude that other method steps may also be present before or after the combined steps or that other method steps may also be inserted between these explicitly mentioned steps, unless otherwise indicated; it is also to be understood that a combined connection between one or more devices/apparatus as referred to in the present application does not exclude that further devices/apparatus may be present before or after the combined device/apparatus or that further devices/apparatus may be interposed between two devices/apparatus explicitly referred to, unless otherwise indicated. Moreover, unless otherwise indicated, the numbering of the various method steps is merely a convenient tool for identifying the various method steps, and is not intended to limit the order in which the method steps are arranged or the scope of the invention in which the invention may be practiced, and changes or modifications in the relative relationship may be made without substantially changing the technical content.
Example 1
The reaction chamber used in this example was cylindrical (as shown in FIG. 1), the chamber size was 20cm diameter by 50cm long, the inlet was standard size, and nitrogen was chosen as the reactant carrier gas (nitrogen has a gas thermal diffusion constant of 0.185 cm)2Per second), the maximum allowable gas flow rate of the reaction zone is Qmax＝226.6cm3In seconds. The size of the device to be processed in the reaction cavity is 3x3cm, the position is the positive center of the cavity, the control volume Z is regulated, and the result is shown in Table 1:
TABLE 1
As can be seen from table 1, by adjusting the controlled amount Z, the overall laminar flow condition in the reaction chamber can be maintained, specifically, the reynolds number of the gas in the reaction chamber can be maintained between 10 and 1600, so that the establishment of the overall laminar flow condition in the reaction region, the rapid and effective transport of the reactant molecules, and the rapid discharge of the reaction by-products during the deposition of the atomic scale thin film on the surface of the three-dimensional bluff body are ensured. On the other hand, the design also inhibits the gas backflow, thereby avoiding the backflow of redundant reactant molecules and reaction byproduct molecules and avoiding the pollution to the substrate surface, the cavity and the gas transportation system caused by the backflow.
Example 2
The deposition experiment was performed under the conditions of condition 3, comparative example 1, and comparative example 2. Plating TiO on the surface of the ring2By using H2O and TiCl4As a precursor source, the atomic layer deposition control cycle is: 0.005 second TiCl4 spray +10 second purge +0.003 second H2O spray +15 second purge. The carrier gas was 99.999% pure nitrogen. The coating temperature is 100 ℃. The gas flow rate was 200sccm and the chamber pressure was 1 torr. The number of atomic layer deposition cycles was 250. The specific results are shown in FIG. 2. As can be seen from fig. 2, when Z is beyond the predetermined range, the fluid environment in the ald chamber cannot be well controlled, especially the laminar flow condition, so that the reaction gas is separated from the surface of the object to be plated in the defluiding direction of the ring, and as a result, the ald cannot be uniformly plated in the defluiding direction (fig. 2b), even cannot be plated (fig. 2 c). After adjusting the amount to the range specified in this patent, it can be seen that atomic layer deposition can be achieved uniformly on all surfaces of the three-dimensional ring (fig. 2 d).
In conclusion, the present invention effectively overcomes various disadvantages of the prior art and has high industrial utilization value.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (10)
1. A method of atomic layer deposition on a surface of a three-dimensional bluff body, the method comprising: introducing a fluid containing a reaction source into a reaction cavity, and carrying out atomic deposition reaction in the surface of a device to be treated, wherein a quantitative parameter Z of reaction gas in the reaction cavity meets the following conditions:
8.5≤Z＝(TV/PФ)≤1359.5
wherein,
t is the temperature in the reaction cavity, and the unit can be;
p is the vacuum degree in the reaction cavity and the unit is Torr;
v is the gas flow in the reaction cavity and the unit is sccm;
phi is the perimeter of the cross section of the reaction cavity and the unit is cm.
2. The method according to claim 1, wherein the reaction source is selected from atomic layer deposition reaction sources, preferably from trimethylaluminum TMA, diethylzinc DEZn, titanium tetrachloride TiCl4The content of the reaction source in the fluid containing the reaction source is 0.1-20 wt%, and the carrier gas is inert gas.
3. The method of claim 2, wherein the reaction source is selected from the group consisting of trimethylaluminum TMA, diethylzinc DEZn, titanium tetrachloride TiCl4One or more of the above.
4. The method according to claim 2, wherein the fluid containing the reactive source contains the reactive source in an amount of 0.1to 20 wt%.
5. The method according to claim 2, wherein the carrier gas in the fluid containing the reaction source is an inert gas.
6. The method of claim 1, wherein the shape of the device to be processed is adapted to the shape of the reaction chamber.
7. The method according to claim 1, wherein the distance between the device to be processed and the inner wall of the reaction chamber satisfies the following condition:
ΔTgH3/Tavv α is less than or equal to 109 and H is more than or equal to 0.1cm
Wherein,
v in the formula represents the aerodynamic viscosity of the gas in m2/s；
g is a gravity constant;
h is the distance between the surface of the device to be processed and the inner wall of the reaction cavity, and the unit is cm;
delta T is the difference between the surface temperature of the device to be processed and the surface temperature of the inner wall of the reaction cavity, and the unit is;
Tavis the average temperature in the reaction zone, and the unit is;
α is the gas thermal diffusion constant in cm2/s。
8. The method of claim 1, wherein the distance between the device to be processed and the fluid inlet of the reaction chamber is generally as follows:
(Len)≥0.03ReD. len is less than or equal to 50 cm;
wherein,
len is the distance between the device to be processed and the fluid inlet of the reaction cavity, and the unit is cm;
re is the Reynolds number of the fluid at the fluid inlet of the reaction cavity;
d is the fluid diameter of the cross section of the reaction cavity and the unit is cm.
9. The method according to claim 1, wherein the inlet gas rectification process is performed on the fluid containing the reaction source, and the inlet gas rectification process generally satisfies the following conditions:
(d2-d1)V≤1.26ФLd；
wherein,
d1the unit is the fluid diameter of a fluid inlet in the air inlet rectification treatment, and the unit is cm;
d2the unit is the fluid diameter of a fluid outlet in the air inlet rectification treatment, and the unit is cm;
v is the gas flow of the reaction device, and the unit is sccm;
phi is the perimeter of a fluid outlet during intake rectification treatment and the unit is cm;
Ldthe length from the fluid inlet to the fluid outlet in the intake air rectification treatment is expressed in cm.
10. The method of claim 1, wherein the fluid exiting the reaction chamber is further subjected to an exit gas rectification process, wherein the exit gas rectification process generally satisfies the following conditions:
(d1’-d2’)V’≤1.26Ф’Ld’；
wherein,
d1' is the fluid diameter of the fluid inlet in cm during the treatment of gas outlet rectification;
d2' is the fluid diameter of the fluid outlet in cm during the treatment of the gas outlet rectification;
v' is the gas flow of the reaction device, and the unit is sccm;
phi' is the perimeter of the fluid inlet during the gas outlet rectification treatment, and the unit is cm;
Ld' is the length from the fluid inlet to the fluid outlet in cm during the treatment of the outgoing gas rectification.
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