CN117832058A - Method for depositing nitride film on silicon substrate at low temperature - Google Patents
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Abstract
The invention discloses a method for depositing a nitride film on a silicon substrate at low temperature, which comprises the following steps: pre-cleaning and passivating the monocrystalline silicon substrate by adopting a chemical method: placing a silicon substrate into a pre-baked vacuum chamber, introducing gas, and ionizing the gas by using a radio frequency plasma source in the vacuum chamber to generate plasma, wherein the plasma performs physical and chemical etching on the silicon substrate; introducing nitrogen source gas, exciting the nitrogen source gas into nitrogen plasma by a radio frequency plasma source, and pre-combining the nitrogen plasma with the silicon substrate; starting a metal beam source furnace in the vacuum chamber, directly spraying metal atom beam current on the silicon substrate obtained after treatment, and reacting the metal atom beam current with nitrogen plasma on the surface of the silicon substrate; the silicon substrate periodically passes through the beam source furnace and the upper part of the radio frequency plasma source in turn in a rotating mode, and the low-temperature nitride film is deposited layer by layer. By precisely controlling each technological parameter, the obtained nitride film has flat surface, no holes or protruding defects, and the low-temperature growth of the nitride film with atomic-level flatness is realized.
Description
Technical Field
The invention relates to the field of semiconductor technology, in particular to a method for depositing a nitride film on a silicon substrate at a low temperature.
Background
The nitride material is widely applied to the fields of deep ultraviolet LED, miniLED, microLED, flexible display screens, solar cells, power radio frequency devices and the like by virtue of excellent parameter characteristics, and has huge market and wide application prospect.
High In, high Al composition growth and low cost flexibility have shown two trends In nitride material research. Since nitrides such as InN are easy to decompose and desorb at high temperature (about 600 ℃), and amorphous substrates which are cheap and easy to prepare in large area cannot withstand high temperature, new technical demands for low-temperature epitaxy of nitride materials are induced.
Currently, the predominant nitride growth techniques include Metal Organic Chemical Vapor Deposition (MOCVD), hydride epitaxy (HVPE), and Molecular Beam Epitaxy (MBE). The MOCVD equipment has complex structure and high manufacturing cost, and carbon pollution and component segregation exist in the high-temperature (generally 800-1200 ℃) growth process; HVPE is carried out at high temperature (usually 600-1100 ℃) and is suitable for preparing bulk materials, but cannot grow complex quantum well structures; MBE has a relatively slow growth rate and is suitable for preparing small-sized nitride materials.
However, the mainstream preparation method cannot meet the technical requirements of high-quality low-temperature epitaxy of nitride materials. Therefore, designing a new method for depositing nitride films at low temperatures is a major problem to be solved by the present invention.
Disclosure of Invention
The invention aims to at least solve one of the technical problems, and the invention provides a method for depositing a nitride film on a silicon substrate at a low temperature, which can prepare the nitride film with atomic-level flatness on the silicon substrate at a low temperature, reduce the cost, improve the productivity and solve the problems of easy decomposition and desorption, carbon pollution, component segregation and the like of part of nitride at a high temperature.
In particular, the invention provides the following technical scheme,
a method for low temperature deposition of a nitride film on a silicon substrate, comprising the steps of:
step S1, pre-cleaning and passivating a monocrystalline silicon substrate by adopting a chemical method;
s2, placing the pre-cleaned silicon substrate into a pre-baked vacuum chamber, introducing gas, and ionizing the gas by using a radio frequency plasma source in the vacuum chamber to generate plasma, wherein the plasma performs physical and chemical etching on the silicon substrate;
step S3, introducing nitrogen source gas into the vacuum chamber, exciting the nitrogen source gas into nitrogen plasma by a radio frequency plasma source, and pre-combining the nitrogen plasma with the silicon substrate;
step S4, starting a metal beam source furnace in the vacuum chamber, and directly spraying metal atom beam on the silicon substrate obtained after the treatment in the step 3, wherein the metal atom beam reacts with nitrogen plasma on the surface of the silicon substrate; the silicon substrate periodically passes through the beam source furnace and the upper part of the radio frequency plasma source in turn in a rotating mode, and the low-temperature nitride film is deposited layer by layer.
Further, the step S1 specifically includes: immersing the monocrystalline silicon substrate into etching liquid, and standing for 2-10 min; taking out after cleaning, washing cleanly, and spin-drying for later use; the etching liquid is one or more of HF, BOE, SC and HF/EG.
Further, the step S2 specifically includes: setting the temperature in the vacuum chamber in the step S2 to be 200-320 ℃; the power range of the radio frequency coil of the radio frequency plasma source is 150W-450W; the etching time is 30-180 min.
Further preferably, the gas introduced in the step S2 is one or more of nitrogen, argon, hydrogen and silane, the gas flow rate in the vacuum chamber ranges from 10 sccm to 50 sccm, and the vacuum degree in the vacuum chamber is kept at 5E-3Pa to 2E-1 Pa.
Further, in step S3, the power range of the RF coil of the RF plasma source is 300-500W, the voltage range of the beam current is 0- +400V, the extraction voltage range is-200-400V, and the neutralization current is 8-12A.
Further preferably, the nitrogen source gas introduced in the step S3 is one or two of nitrogen and ammonia, the gas flow rate in the vacuum chamber ranges from 3 sccm to 20 sccm, and the vacuum degree in the vacuum chamber is kept at 5E-3Pa to 5E-1Pa.
Further, the deposition time in the step S4 is 1-120 min; the temperature in the vacuum chamber is set to be 200-350 ℃ and the vacuum degree in the vacuum chamber is 5E-3 Pa-5E-1 Pa.
Further preferably, the metal source used In the metal beam source furnace In the step S4 is one or more of Al, ga and In, after the metal source is heated to 600-1000 ℃, a furnace cover of the metal beam source furnace is opened, and one or more metal atom beams are sprayed onto the treated silicon substrate; the temperature of the silicon substrate is 300-500 ℃.
Further, in step S4, the furnace cover of the metal beam source furnace is opened when the silicon substrate rotates right above the metal beam source furnace, and the furnace cover of the metal beam source furnace is closed when the silicon substrate rotates away from the metal beam source furnace.
Further, in step S4, the silicon substrate stays above the rf plasma source for 30-90S.
The beneficial effects obtained by the invention are as follows:
firstly, the invention provides a method for depositing a nitride film on a silicon substrate at low temperature so as to meet the requirement of nitride materials on high-quality low-temperature epitaxial growth; secondly, by the method provided by the invention, not only the natural oxide layer on the surface of the silicon substrate is effectively removed, but also the substrate is subjected to plasma treatment, and when the nitride film is deposited on the silicon substrate, the formation of amorphous compounds of Si on the surface of the silicon substrate is effectively inhibited.
Compared with the prior art, the method for depositing the nitride film on the silicon substrate at low temperature provided by the invention has the advantages of remarkably reducing the cost, effectively improving the productivity, simultaneously having the characteristics of low carbon pollution and no component segregation, realizing the low-temperature atomic-level flatness growth of the nitride film, and realizing the defects of flat, non-hole or protrusion surface of the obtained nitride film. In addition, because the growth process is carried out under the low-temperature condition, the decomposition and desorption of partial nitride under the high temperature and the remelting reaction between partial nitride and the substrate under the high temperature are avoided.
Drawings
The accompanying drawings are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate the invention and together with the description serve to explain, without limitation, the invention.
Fig. 1 is a process flow diagram of low temperature deposition of a nitride film on a silicon substrate according to an embodiment of the present invention.
FIG. 2 is a schematic view of an atomic force microscope of a single crystal silicon wafer after a plasma etching process according to an embodiment of the present invention.
Fig. 3 is a schematic view of an afm after depositing an AlN film at low temperature in accordance with an embodiment of the present invention.
Detailed Description
The following describes specific embodiments of the present invention in detail with reference to the drawings. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention. The invention provides a method for depositing a nitride film on a silicon substrate at a low temperature, which comprises the following steps:
step S1, pre-cleaning a commercially purchased monocrystalline silicon substrate by adopting a chemical method to remove an oxide layer on the surface of the silicon substrate and passivating the oxide layer;
s2, placing the pre-cleaned silicon substrate into a vacuum chamber which is baked in advance, introducing etching gas into the vacuum chamber, and ionizing the gas by using a radio frequency plasma source in the vacuum chamber to generate plasma; performing physical and chemical etching on the silicon substrate through the generated plasma;
step S3, after the silicon substrate is processed, introducing nitrogen source gas into the vacuum chamber; exciting nitrogen source gas into nitrogen plasma by a radio frequency plasma source in the vacuum chamber, so that the nitrogen plasma in the vacuum chamber reaches a set concentration range, and pre-combining with the silicon substrate;
and S4, starting a metal beam source furnace in the vacuum chamber, directly spraying one or more metal atom beams on the silicon substrate obtained after the treatment in the step 3, and reacting with nitrogen plasma on the surface of the substrate. The silicon substrate periodically and sequentially passes through the metal beam source furnace and the upper part of the radio frequency plasma source in a rotating way, and a layer-by-layer deposition process of the low-temperature nitride film is carried out.
As described above, the method for depositing the nitride film on the silicon substrate at low temperature provided by the invention adopts a molecular beam-like epitaxy process, and realizes epitaxial growth of the nitride film through alternate deposition of metal atoms and nitrogen plasmas.
In step S1, a commercially purchased silicon substrate is pre-cleaned by a chemical method, and oxide layers and impurities on the surface of the silicon substrate to be processed can be removed and the surface thereof can be passivated.
Specifically, a commercially available monocrystalline silicon wafer is immersed in the etching solution and left for 2 to 10 minutes, depending on the thickness of the oxide layer. This process aims to allow the surface silicon oxide layer to react and be removed sufficiently in a suitable time. Meanwhile, the cleaning liquid effectively prevents the silicon substrate from further oxidation or other surface reactions by reacting with the surface of the silicon substrate. And taking out after the cleaning is finished, washing with deionized water, and spin-drying at a high speed by a spin dryer for later use.
In the above embodiment, the etching liquid is one or more of HF, BOE, SC and HF/EG. The centrifugal speed of the spin dryer is 800-2600 rpm, the spin drying time is 5-15 min, and the spin drying temperature is 40-80 min.
In the etching solution, HF is hydrofluoric acid; BOE is HF and NH 4 F, the pH value of the solution is stable, the mixture is not influenced by the addition of a small amount of acid, and the etching rate is stable; SC1 is a mixture of ammonium hydroxide, hydrogen peroxide and water, the greater the concentration and the temperatureThe higher the etching is, the faster; HF/EG is a mixture of hydrofluoric acid and ethylene glycol and is mainly characterized by not reacting with base silicon or dry etching damaged silicon.
In step S2, the pre-cleaned silicon substrate is placed in a vacuum chamber baked in advance, gas is introduced, and the gas is ionized by a radio frequency plasma source in the vacuum chamber to generate plasma. And carrying out physical and chemical etching on the silicon substrate through the generated plasma.
Specifically, the silicon substrate pre-cleaned in the step 1 is placed in a vacuum chamber baked in advance, and the temperature of the chamber is set to be 200-320 ℃. And (3) introducing gas into the vacuum chamber, ionizing the gas by utilizing a radio frequency plasma source in the vacuum chamber, wherein the power range of a radio frequency coil loaded to the radio frequency plasma source is 150W-450W. And carrying out physical and chemical etching on the silicon substrate through the generated plasma, wherein the etching time is 30-180 min.
It is easy to understand that by setting the temperature in the vacuum chamber to 200-320 ℃, the silicon substrate can be etched, the etching rate is stable, and is not too fast or too slow, when the temperature is too low, the etching rate is fast, the surface morphology of the silicon substrate is difficult to control, and when the temperature is too high, the etching rate is too slow, and the expected etching effect is difficult to achieve.
By controlling the process parameters, the surface roughness of the etched silicon substrate is less than 0.2nm (10 μm×10 μm range) as shown in fig. 1 by Atomic Force Microscope (AFM) test.
As a preferable implementation mode, the gas introduced in the step S2 is one or more of nitrogen, argon, hydrogen and silane, the gas flow rate in the vacuum chamber ranges from 10 sccm to 50 sccm, and the vacuum degree in the vacuum chamber is kept at 5E-3Pa to 2E-1 Pa.
As described above, the SVT rf plasma source is used for ionization, mainly for dissociating nitrogen, hydrogen, argon, and the like. High-energy ions are not generated in the dissociation process, so that the high-quality film can be grown, and the substrate can be cleaned under the condition of not damaging the surface of the substrate. When the SVT radio frequency plasma source works, two bias voltages need to be loaded, wherein the loaded beam current voltage is positive voltage bias and is used for focusing plasma. The loaded extraction voltage is biased at a negative voltage for acceleration of the plasma and extraction of positively charged ions from the plasma.
In addition, the SVT rf plasma source has a certain requirement for vacuum degree, and the vacuum degree is too low and can have an adverse effect on the SVT rf plasma source when used for a long time. Therefore, the gas flow rate ranges from 10 sccm to 50 sccm, and the vacuum degree of the chamber is kept at 5E-3Pa to 2E-1Pa。
In step S3, after the silicon substrate processing is completed, a nitrogen source gas is introduced into the vacuum chamber. And exciting the nitrogen source gas into nitrogen plasma by a radio frequency plasma source in the vacuum chamber, so that the nitrogen plasma in the chamber reaches a set concentration range, and pre-combining with the Si substrate.
In the above embodiment, the power range of the rf coil loaded to the rf plasma source is 300 to 500W, the beam voltage range of the rf plasma source is 0 to +400V, the extraction voltage range of the rf plasma source is-200 to-400V, and the neutralization current of the rf plasma source is 8 to 12A.
As an alternative implementation mode, the introduced nitrogen source gas is one or two of nitrogen and ammonia, the gas flow rate in the vacuum chamber ranges from 3 sccm to 20 sccm, and the vacuum degree in the vacuum chamber is kept at 5E-3Pa to 5E-1Pa. The nitrogen source gas is excited into plasma by a radio frequency plasma source and then sprayed to the surface of the processed Si substrate, and the temperature in the vacuum chamber is 300-500 ℃.
In step S4, a metal beam source furnace in the vacuum chamber is started, one or more metal atom beams are directly sprayed onto the silicon substrate obtained after the treatment in step 3, and the reaction is carried out on the surface of the substrate and nitrogen plasma. The silicon substrate periodically and sequentially passes through the metal beam source furnace and the upper part of the radio frequency plasma source in a rotating way, and a layer-by-layer deposition process of the low-temperature nitride film is carried out. By precisely controlling each technological parameter, the low-temperature growth of the atomic-level flatness nitride film is realized.
It should be noted that, as shown in fig. 2, after the test of Atomic Force Microscope (AFM), the result shows that the surface of the nitride film grown at low temperature on the silicon substrate processed in the step 2 is flat, no hole or protrusion defect is generated, the surface morphology of the silicon substrate is well inherited, and the surface roughness is less than 0.2nm (10 μm×10 μm range).
In the above embodiment, the metal source used In the metal beam source furnace is one or more of Al, ga, and In, and after the metal source is heated to 600-1000 ℃, the furnace cover of the metal beam source furnace is opened, and one or more metal atomic beams are sprayed onto the processed silicon substrate. The silicon substrate periodically and sequentially passes through the metal beam source furnace and the upper part of the radio frequency plasma source in a rotating way, and a layer-by-layer deposition process of the low-temperature nitride film is carried out. The temperature of the silicon substrate is 300-500 ℃ and the deposition time is 1-120 min.
As described above, in the step S4, the rotation mode and the residence time of the silicon substrate are controlled, so that the substrate sequentially passes through the metal beam source furnace and the rf plasma source, different III/V ratios are satisfied, and the layer-by-layer deposition process of the low-temperature nitride film is performed, so as to realize the low-temperature growth of the atomic-level-flatness nitride film. The temperature of the vacuum chamber is set to be 200-350 ℃, and the vacuum degree in the vacuum chamber is 5E-3 Pa-5E-1 Pa.
In the control mode of the rotation of the silicon substrate, the rotation of the silicon substrate and the opening and closing of the furnace cover of the metal beam source furnace are controlled in a linkage manner, and the residence time of the substrate above the radio frequency plasma source in each rotation period can be specifically set. The opening and closing time of the furnace cover of the metal beam source furnace can be set according to the time for the silicon substrate to rotationally sweep over the metal beam source furnace, when the silicon substrate rotates to pass near the position right over the metal beam source furnace, the furnace cover of the metal beam source furnace is opened, and when the silicon substrate rotates to leave the metal beam source furnace, the furnace cover of the metal beam source furnace is closed, so that excessive III-group reactants caused by the fact that metal atom beam flows drift over the whole reaction chamber under low vacuum can be avoided; the residence of the substrate above the plasma source can compensate for the deficiency in the effective group v plasma concentration. The spin residence time of the silicon substrate is set to 30 to 90 s.
The method provided by the invention has the advantages that the plasma treatment and the low-temperature deposition of the nitride film are carried out on the silicon substrate, so that the natural oxide layer on the surface of the silicon substrate is effectively removed, and the formation of the amorphous compound of Si on the surface of the silicon substrate is effectively inhibited by the plasma treatment of the substrate, thereby improving the quality of the nitride film deposited on the silicon substrate; the setting of the spin-stop time of the substrate and the linkage control of the furnace cover of the metal beam source furnace can accurately regulate and control the III/V ratio so as to grow nitride films with different component contents; the low-temperature growth mode avoids decomposition and desorption of nitride at high temperature and remelting reaction with the substrate at high temperature. Compared with the defects of high energy consumption, high cost, carbon pollution, component segregation and the like of the MOCVD method in the prior art, the HVPE method cannot prepare the limitation of the complex quantum well structure, the low growth rate of the MBE method greatly reduces the cost, effectively improves the productivity, has low carbon pollution and no component segregation, realizes the low-temperature growth of the atomic-level flatness nitride film, and well meets the high-quality low-temperature epitaxial growth requirement of the nitride material.
It is to be understood that the above embodiments are merely illustrative of the application of the principles of the present invention, but not in limitation thereof. Various modifications and improvements may be made by those skilled in the art without departing from the spirit and substance of the invention, and are also considered to be within the scope of the invention.
Claims (10)
1. A method for low temperature deposition of a nitride film on a silicon substrate, comprising the steps of:
step S1, pre-cleaning and passivating a monocrystalline silicon substrate by adopting a chemical method;
s2, placing the pre-cleaned silicon substrate into a pre-baked vacuum chamber, introducing gas, and ionizing the gas by using a radio frequency plasma source in the vacuum chamber to generate plasma, wherein the plasma performs physical and chemical etching on the silicon substrate;
step S3, introducing nitrogen source gas into the vacuum chamber, exciting the nitrogen source gas into nitrogen plasma by a radio frequency plasma source, and pre-combining the nitrogen plasma with the silicon substrate;
step S4, starting a metal beam source furnace in the vacuum chamber, and directly spraying metal atom beam on the silicon substrate obtained after the treatment in the step 3, wherein the metal atom beam reacts with nitrogen plasma on the surface of the silicon substrate; the silicon substrate periodically passes through the beam source furnace and the upper part of the radio frequency plasma source in turn in a rotating mode, and the low-temperature nitride film is deposited layer by layer.
2. The method of low temperature deposition of a nitride film on a silicon substrate according to claim 1, wherein said step S1 is specifically: immersing the monocrystalline silicon substrate into etching liquid, and standing for 2-10 min; taking out after cleaning, washing cleanly, and spin-drying for later use; the etching liquid is one or more of HF, BOE, SC and HF/EG.
3. The method of low temperature deposition of a nitride film on a silicon substrate according to claim 1, wherein said step S2 is specifically: setting the temperature in the vacuum chamber in the step S2 to be 200-320 ℃; the power range of the radio frequency coil of the radio frequency plasma source is 150W-450W; the etching time is 30-180 min.
4. The method of claim 1, wherein the gas introduced in the step S2 is one or more of nitrogen, argon, hydrogen and silane, the gas flow rate in the vacuum chamber ranges from 10 sccm to 50 sccm, and the vacuum degree in the vacuum chamber is kept at 5E-3Pa to 2E-1 Pa.
5. The method according to claim 1, wherein the power of the rf coil of the rf plasma source in the step S3 is 300-500-W, the voltage of the beam is 0- +400-V, the extraction voltage is-200-400-V, and the neutralization current is 8-12A.
6. The method according to claim 1, wherein the nitrogen source gas introduced in the step S3 is one or both of nitrogen gas and ammonia gas, the gas flow rate in the vacuum chamber ranges from 3 sccm to 20 sccm, and the vacuum degree in the vacuum chamber is kept at 5E-3Pa to 5E-1Pa.
7. The method for low temperature deposition of a nitride film on a silicon substrate according to claim 1, wherein the deposition time in step S4 is 1 to 120 min; the temperature in the vacuum chamber is set to be 200-350 ℃ and the vacuum degree in the vacuum chamber is 5E-3 Pa-5E-1 Pa.
8. The method for low temperature deposition of a nitride film on a silicon substrate according to claim 1, wherein the metal source used In the metal beam source furnace In the step S4 is one or more of Al, ga, and In, and after the metal source is heated to 600-1000 ℃, the furnace cover of the metal beam source furnace is opened, and one or more metal atom beams are sprayed onto the processed silicon substrate; the temperature of the silicon substrate is 300-500 ℃.
9. The method according to claim 1, wherein in the step S4, the furnace lid of the metal beam source furnace is opened when the silicon substrate rotates directly above the metal beam source furnace, and the furnace lid of the metal beam source furnace is closed when the silicon substrate rotates away from the metal beam source furnace.
10. The method of depositing a nitride film on a silicon substrate according to claim 1, wherein the silicon substrate is stopped above the rf plasma source in step S4 for a time period of 30 to 90S.
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