CN116377406A - Preparation method of tantalum nitride film and tantalum nitride film - Google Patents
Preparation method of tantalum nitride film and tantalum nitride film Download PDFInfo
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- CN116377406A CN116377406A CN202310244004.3A CN202310244004A CN116377406A CN 116377406 A CN116377406 A CN 116377406A CN 202310244004 A CN202310244004 A CN 202310244004A CN 116377406 A CN116377406 A CN 116377406A
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- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 239000000758 substrate Substances 0.000 claims abstract description 48
- 238000000034 method Methods 0.000 claims abstract description 40
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- 238000007872 degassing Methods 0.000 claims abstract description 11
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 8
- 238000011084 recovery Methods 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 29
- 238000004544 sputter deposition Methods 0.000 claims description 27
- 230000008569 process Effects 0.000 claims description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 239000012495 reaction gas Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- 239000010408 film Substances 0.000 description 52
- 239000002245 particle Substances 0.000 description 12
- 229910052757 nitrogen Inorganic materials 0.000 description 10
- 239000000126 substance Substances 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 229910052715 tantalum Inorganic materials 0.000 description 3
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 3
- 239000013077 target material Substances 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000004886 process control Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 238000005273 aeration Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
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Abstract
The application provides a preparation method of a tantalum nitride film and the tantalum nitride film, wherein the method comprises the following steps: a degassing step of degassing the substrate in the vacuum reaction chamber; continuously contacting the degassed substrate with a carrier with preset temperature for a first preset time to homogenize the substrate temperature by using the carrier temperature; performing direct-current magnetron sputtering on the substrate with the uniform temperature in the vacuum reaction chamber to form a tantalum nitride film; and a recovery step of recovering the air pressure and temperature of the vacuum reaction chamber to the initial state before the next use. The tantalum nitride film with better uniformity and repeatability can be prepared.
Description
Technical Field
The invention relates to the field of film manufacturing, in particular to a preparation method of a tantalum nitride film and the tantalum nitride film.
Background
Tantalum nitride has wide application in the fields of wear-resistant coating, film resistance, diffusion barrier in integrated circuits and the like due to the excellent chemical and physical properties of high hardness, wear resistance, chemical inertness, thermal stability and the like. The reaction magnetic control sputtering to generate the tantalum nitride film relates to the physical and chemical processes, and the uniformity and repeatability of the tantalum nitride film are greatly influenced by the change of the ambient temperature and the air pressure in the preparation process. Improper process parameters in the preparation process are very easy to cause insufficient process gas consumption, excessively rapid heat accumulation and the like, and the environmental change in the cavity causes great difference between physical and chemical properties of tantalum nitride films in the same batch. For example, nitrogen is taken as a reaction gas, the partial pressure of the process gas can directly influence the nitrogen element content in the tantalum nitride film, the nitrogen flow is set to be too large, so that gas consumption is not timely, further, the tantalum nitride film is changed in component quantity and quality in the continuous production process, meanwhile, target poisoning can occur, namely, excessive nitrogen reacts with the surface of a target to generate a compound, the sputtering process is changed from metal sputtering to compound sputtering, and the change of the sputtering process means that the component parts, the structure and the film thickness of the film all fluctuate.
In summary, the atmosphere of the film cavity for preparing tantalum nitride by direct-current magnetron sputtering is difficult to stabilize, and thus the repeatability of the film in the formal production process is difficult to control, which is one of the main obstacles for limiting the mass production and the application of the film.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of a tantalum nitride film and the tantalum nitride film, and the tantalum nitride film with better uniformity and repeatability can be prepared.
In order to achieve the above object, the present application provides a method for preparing a tantalum nitride film, comprising:
a degassing step of degassing the substrate in the vacuum reaction chamber;
continuously contacting the degassed substrate with a carrier with preset temperature for a first preset time to homogenize the substrate temperature by using the carrier temperature;
performing direct-current magnetron sputtering on the substrate with the uniform temperature in the vacuum reaction chamber to form a tantalum nitride film;
and a recovery step of recovering the air pressure and temperature of the vacuum reaction chamber to the initial state before the next use.
In a preferred embodiment, the restoring the air pressure and temperature of the vacuum reaction chamber to the initial state includes: the vacuum reaction chamber is left empty for a predetermined time.
In a preferred embodiment, the predetermined time period for which the vacuum chamber is left empty is related to the current sputtering process parameters for sputtering the substrate to form a tantalum nitride film.
In a preferred embodiment, the degassing the substrate comprises: and carrying out high-temperature heat treatment on the substrate to disperse impurity gas adsorbed on the surface of the substrate.
In a preferred embodiment, the impurity gas comprises water gas and/or other gas molecules.
In a preferred embodiment, the temperature of the high temperature heat treatment of the substrate is 80-350 ℃ and the heat treatment time is 30-300 s.
In a preferred embodiment, the thermostating step comprises: the substrate is contacted with a carrier in advance, the temperature of the carrier is controlled to be 20-60 ℃, and the contact time lasts for 10-200 s.
In a preferred embodiment, in the magnetron sputtering step: the flow rate of the nitrogen gas which is introduced into the reaction gas is 5-40sccm, the flow rate of the argon gas which is introduced into the process gas is 20-80sccm, the sputtering power is 500-13000W, the target base distance is 100-600mm, and the air pressure in the vacuum reaction chamber is 1.8-10mTorr.
The application discloses a tantalum nitride film prepared by the method.
According to the preparation method of the tantalum nitride film, provided by the embodiment of the application, the impurity moisture of the substrate is removed in advance, the substrate is subjected to constant temperature treatment and the vacuum reaction chamber used each time is treated, so that the quality and the temperature uniformity of the substrate are ensured, the problem that the quality of the film is unstable due to continuous use of the vacuum reaction chamber and different conditions each time is solved, and the tantalum nitride film with better uniformity and repeatability can be prepared.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flowchart of a method for preparing a tantalum nitride film according to an embodiment of the present application;
FIG. 2 is a graph showing the uniformity results of continuous Wafer (Wafer to Wafer) in one embodiment of the present application;
FIG. 3 is a graph showing the results of batch-to-batch (Lot) uniformity in one embodiment of the present application.
Detailed Description
For the purposes of making the objects, technical solutions and advantages of the present application more apparent, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application, and it is apparent that the described embodiments are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present disclosure.
The following describes in detail a specific implementation procedure of a method for preparing a tantalum nitride film according to an embodiment of the present invention, with reference to a specific example shown in fig. 1. The target material for the sputtering process in this example may be tantalum.
As shown in fig. 1, the preparation method of the tantalum nitride film comprises the following steps:
step S101: the substrate is degassed.
Under the action of intermolecular forces or the characteristic of the material, a small amount of gas molecules or water vapor can be attached to the surface of the substrate, so that the quality of a coating film is affected, and the coating film atmosphere is destroyed. For this purpose, the substrate needs to be degassed.
The substrate may be subjected to a high-temperature heat treatment to disperse impurity gases adsorbed on the surface of the substrate. The heat treatment temperature and time influence the degassing effect and the degassing efficiency, so that the two are required to be in balance fit, and are important variables for controlling the step.
The inventors found through a large number of experiments that the temperature of the heat treatment can be 80-350 ℃ and the heat treatment time can be 30-300 s.
Step S102: and performing constant temperature control on the substrate.
The substrate surface is one of the tantalum nitride generation places, the substrate temperature before film coating influences the film forming process and the film quality, the selection and the stabilization of the substrate temperature are one of key influencing factors of the stability of the film in the production process, but the substrate temperature after the degassing in the step S101 needs to be stabilized to a proper interval, so that the process stability is ensured. And directly contacting the substrate with a carrier with preset temperature for a certain time, and performing subsequent coating operation after the temperature of the substrate is consistent with the temperature of the carrier.
The inventors found through a lot of experiments that the temperature of the stage in this step may be: the temperature of 20-60 ℃ and the time for the substrate to contact the carrier for constant temperature control can be: 10s-200s.
Step S103: in the vacuum reaction chamber, a tantalum nitride film is formed on the surface of the substrate by a sputtering method.
The process control parameters of the sputtering process in this step include the flow rate of the reactive gas nitrogen, the flow rate of the process gas inert gas (e.g., argon), the sputtering power, the target base distance, the gas pressure, etc. The inventor concludes through a large number of experiments and analyses that the influence relationship between the process control parameters and the thin film sputtering result is as follows:
wherein nitrogen is one of elements constituting the tantalum nitride film as a reactive gas. The amount of nitrogen aeration is related to the nitrogen content of the film, and indirectly affects the physical and chemical properties of the film. The flow and power of process gases such as argon affect the deposition rate of target particles (e.g., tantalum particles) and the rate of tantalum nitride formation.
The sputtering power influences the quantity and momentum of sputtering target particles (such as tantalum particles), and finally influences the growth rate of the tantalum nitride film, and the sputtering power and the flow of process gas are adjusted in a matching way, so that the film components can be adjusted to realize the purpose of controlling the physical and chemical properties of the film.
The target base distance is the distance between the target material and the substrate, and the uniformity of the film can be adjusted by changing the size of the target base distance. If the sputtering process adopts a magnetron sputtering method, sputtering particles can reach the substrate to gather and nucleate at different incidence angles under the action of a magnetic field, so that the substrate can collect different numbers of incidence particles at different positions under different target base distances. In addition, the target base distance can also control the film growth rate, the collision times of the sputtering particles reaching the substrate under different target base distances are different, namely the incident kinetic energy of the sputtering particles is different, and the quality of the finally obtained film is also different.
The gas pressure in the reaction chamber mainly affects the energy of sputtered particles, which affects the ability of particles to migrate and diffuse when reaching the substrate, and can affect resistivity and surface smoothness. The gas pressure in the reaction chamber is too high, the ionization of the gas is improved, but the reduction of the mean free path causes more kinetic energy loss of sputtered particles, the migration capacity is limited after reaching the substrate, and the crystallization quality is poor. And too low a pressure in the reaction chamber will result in difficulty in ignition.
In summary, the interaction of process parameter variables such as the flow of reaction gas (i.e. nitrogen), the flow of process gas (e.g. argon), the sputtering power, the target base distance, the air pressure in the reaction chamber and the like need to be coordinated and arranged in an optimization interval, which is more beneficial to producing the tantalum nitride film with physical and chemical properties meeting the application requirements and better uniformity and repeatability.
The inventor finds through experiments that the flow rate of nitrogen introduced into the reaction gas can be: the flow rate of argon gas introduced into the process gas can be 5-40 sccm: the sputtering power can be 500-13000W, the target base distance can be 100-600mm, and the air pressure in the vacuum reaction chamber can be 1.8-10mTorr.
Step S104: and (5) restoring the sputtering atmosphere.
After the sputtering cavity is coated, the temperature of the internal shielding piece and the target material rises after absorbing the kinetic energy of sputtering particles, and the improper process parameters can cause the pressure and the temperature of the cavity to gradually accumulate. The gradual change of the atmosphere of the cavity of the reaction chamber eventually causes the fluctuation of the stability of the film along with the continuous accumulation of the number of the processed substrates in the production process. Therefore, after each substrate is coated, the reaction chamber cavity needs to wait for the air pressure and the temperature to be restored to the initial state.
The recovery of the air pressure and temperature of the vacuum reaction chamber to the initial state can be achieved specifically by the following means: the vacuum reaction chamber is left empty for a predetermined time. The idle time of the reaction chamber cavity in the step is related to the pumping speed of the cavity using a pump and the sputtering process condition.
The inventor finds through a large number of experiments that the idle time of the reaction chamber cavity in the step can be 10s-360s.
Some experimental results of the tantalum nitride thin film prepared by the preparation method of the above example are as follows:
taking the film square resistance as an example, the following test results were obtained:
resistance (49 point mean): 30-100ohm
Resistance value range (maximum resistance value and minimum resistance value difference value in 49 points): <3.5ohm
Resistance uniformity: 2 + -0.13%.
The uniformity results for continuous film forming (Wafer to Wafer) are shown in FIG. 2.
Fig. 3 shows the results of inter-Lot (Lot to Lot) uniformity.
In summary, the preparation method of the tantalum nitride film provided by the embodiment of the application can prepare the tantalum nitride film with better uniformity and repeatability.
The application also discloses a tantalum nitride film which is prepared by the method. The uniformity of the film is better.
The foregoing description of the preferred embodiments of the present application is not intended to limit the invention to the particular embodiments of the present application, but to limit the scope of the invention to the particular embodiments of the present application.
Claims (9)
1. A method for preparing a tantalum nitride film, comprising:
a degassing step of degassing the substrate in the vacuum reaction chamber;
continuously contacting the degassed substrate with a carrier with preset temperature for a first preset time to homogenize the substrate temperature by using the carrier temperature;
performing direct-current magnetron sputtering on the substrate with the uniform temperature in the vacuum reaction chamber to form a tantalum nitride film;
and a recovery step of recovering the air pressure and temperature of the vacuum reaction chamber to the initial state before the next use.
2. The method of claim 1, wherein the restoring step of restoring the air pressure and temperature of the vacuum reaction chamber to the initial state before the next use comprises: the vacuum reaction chamber is left empty for a second predetermined time.
3. The method of claim 2, wherein the second predetermined time is determined based on current sputtering process parameters for dc magnetron sputtering the substrate to form the tantalum nitride film.
4. The method of claim 1, wherein the step of degassing comprises: the substrate is subjected to a high-temperature heat treatment to disperse impurity gases adsorbed on the surface of the substrate.
5. The method of claim 4, wherein the impurity gas comprises water gas and/or other gas molecules.
6. The method of claim 4, wherein the substrate is subjected to the high temperature heat treatment at a temperature of 80 ℃ to 350 ℃ for a heat treatment time of 30s to 300s.
7. The method of claim 6, wherein the step of thermostating comprises: and (3) contacting the degassed substrate with a carrier with the temperature of 20-60 ℃ for 10-200 s.
8. The method of claim 7, wherein in the magnetron sputtering step, the flow rate of nitrogen gas which is introduced into the reaction gas is 5-40sccm, the flow rate of argon gas which is introduced into the process gas is 20-80sccm, the sputtering power is 500-13000W, the target base distance is 100-600mm, and the air pressure in the vacuum reaction chamber is 1.8-10mTorr.
9. A tantalum nitride film, characterized in that said tantalum nitride film is produced by the method according to any one of claims 1 to 8.
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| CN202310244004.3A CN116377406A (en) | 2023-03-14 | 2023-03-14 | Preparation method of tantalum nitride film and tantalum nitride film |
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| CN202310244004.3A CN116377406A (en) | 2023-03-14 | 2023-03-14 | Preparation method of tantalum nitride film and tantalum nitride film |
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