CN111254412A - Atomic layer deposition technology and method for preparing iridium film - Google Patents

Atomic layer deposition technology and method for preparing iridium film Download PDF

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Publication number
CN111254412A
CN111254412A CN202010229705.6A CN202010229705A CN111254412A CN 111254412 A CN111254412 A CN 111254412A CN 202010229705 A CN202010229705 A CN 202010229705A CN 111254412 A CN111254412 A CN 111254412A
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iridium
atomic layer
layer deposition
hydrazine
liquid
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不公告发明人
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Jiangsu Mnt Micro And Nanotech Co ltd
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Jiangsu Mnt Micro And Nanotech Co ltd
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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
    • C23C16/06—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 metallic material
    • C23C16/18—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 metallic material from metallo-organic compounds
    • 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
    • C23C16/448—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 generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
    • C23C16/4481—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 generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by evaporation using carrier gas in contact with the source material
    • 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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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)
  • Electrodes Of Semiconductors (AREA)

Abstract

The invention discloses an atomic layer deposition technology and method for preparing an iridium film, and the atomic layer deposition technology and method comprise a liquid iridium source and a hydrazine reducing agent, wherein the liquid iridium source is used as a precursor, the hydrazine reducing agent is used as a reductive precursor, and the liquid iridium source can adopt 1-ethylcyclopentadienyl-1, 3-cyclohexadienyl iridium (I) and other raw materials. The method selects the liquid iridium source Ir as the iridium precursor, can avoid the iridium source from being condensed to block a valve in the use process, can well control the deposition process, reduces the production cost, selects the hydrazine reducing agent as the reductive precursor, can directly utilize the thermal atomic layer deposition technology to deposit the simple substance iridium film, is superior to gases such as plasma NH3, hydrogen and the like used in the prior art, is more convenient, safer and easier to operate in the use process, can avoid the inconvenience in the operation of plasma hydrogen, plasma ammonia and the like, can simplify the preparation process of the simple substance iridium film, and saves the cost.

Description

Atomic layer deposition technology and method for preparing iridium film
Technical Field
The invention relates to the technical field related to an iridium film preparation method, in particular to an atomic layer deposition technology and method for preparing an iridium film.
Background
The noble metal Ir has stronger oxidation resistance, high conductivity, strong catalytic activity and good corrosion resistance, and the properties of the iridium Ir can ensure that the iridium film can be widely applied to electrode materials, microelectronics, optical devices and high-temperature oxidation-resistant coatings. The prior Ir film preparation method generally comprises physical vapor deposition, electrochemical deposition, sol-gel, halide chemical vapor deposition, metal organic chemical vapor deposition and the like. Physical vapor deposition and chemical vapor deposition are the most commonly used, however, the physical vapor deposition method has high deposition temperature and poor film forming capability on the surface of a part with a complex shape; chemical vapor deposition has drawbacks in terms of precise control of film purity and thickness.
Atomic Layer Deposition (ALD) is a vapor phase thin film deposition technique that relies on sequential, self-limiting surface reactions. This is accomplished by alternately pulsing the precursors onto the substrate (separated by evacuation or purge cycles) to avoid gas phase reactions that occur in closely related Chemical Vapor Deposition (CVD) techniques. Self-limiting reactions can deposit pure, high quality films with excellent conformality and precisely controlled film thickness and composition. Therefore, the atomic layer deposition technology has good application prospect in the aspect of preparing high-quality Ir films and devices.
In the prior art ALD processes for Ir most commonly use O3 and Ir2, Ir2 as reactants at temperatures above 200 ℃, while Ir can be deposited at temperatures below 200 ℃ using successive O3 and H2 pulses, and plasma enhanced ALD processes using H2 plasma, NH3 plasma or mixed O2-H2 plasma have also been demonstrated, e.g., ALD iridium films have been used for optical and catalytic, and diffusion barrier and seed layer applications, with ALD techniques for depositing silver films mainly: the iridium precursor is reduced by plasma hydrogen or ozone, the deposition temperature is greatly reduced due to high reaction activity of the plasma hydrogen or ozone, but simultaneously due to high activity of the iridium precursor, the iridium precursor can be recombined when the iridium precursor does not enter a groove, the deposition and coating effects of the groove with a high aspect ratio are poor, meanwhile, the storage and use safety of hydrogen bring inconvenience to the whole process, the precursors required by the prior atomic layer deposition technology for depositing the iridium film are all solid substances, such as Ir2, Ir2 and the like, the volatility is poor in the use process, and the precursors are easy to be condensed into a solid state, so that a manual valve and a manual valve are blocked.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides an atomic layer deposition technology and a method for preparing an iridium film, which have the advantages that: the hydrazine substance is cheap and easily available, is a little liquid and is convenient to store and transport. The deposited simple substance film has excellent uniformity and good step coverage rate; the method is superior to the gases such as plasma NH3, hydrogen and the like reported in the literature; in the using process, the operation is more convenient, safer and easier; the method can avoid the inconvenience in operation of plasma hydrogen, plasma ammonia and the like, simplify the preparation process of the simple substance film, save the cost, effectively avoid the iridium source from being condensed in the use process to block the valve, well control the deposition process, reduce the production cost and solve the problems that the iridium source blocks the valve and the production cost is higher.
(II) technical scheme
The invention provides the following technical scheme: an atomic layer deposition technology and a method for preparing an iridium film comprise a liquid iridium source and a hydrazine reducing agent, wherein the liquid iridium source is used as a precursor, and the hydrazine reducing agent is used as a reductive precursor.
Preferably, the liquid iridium source can adopt 1-ethyl cyclopentadienyl-1, 3-cyclohexadienyl iridium (I) as a raw material.
Preferably, the hydrazine reducing agent comprises anhydrous hydrazine, methyl hydrazine, ethyl hydrazine, propyl hydrazine, tert-butyl hydrazine and other C1-C5 hydrocarbon chains, and the reducing agent has the structural formula R1R2N-NR3R4Wherein R is1、R2、R3And R4Comprising a hydrogen atom, a hydrocarbon chain of C1-C5, R1、R2、R3And R4May be the same or different.
Another technical problem to be solved by the present invention is to provide an atomic layer deposition technique and a method for preparing an iridium thin film, wherein the method comprises the following steps:
s1, heating the liquid iridium source raw material to a temperature range of 100-150 ℃ by adopting atomic layer deposition equipment, and vacuumizing to a limit pressure, wherein the limit pressure after vacuumizing is 0.1-10 Pa;
s2, after the atomic layer deposition system is heated uniformly, the heating time is 40min, then the carrier gas flow is started to be 10-200sccm, the temperature range of the atomic layer deposition system heated uniformly is 100-400 ℃, and the pressure range in the atomic layer deposition system is 10-200 Pa;
s3, opening a liquid iridium source atomic layer deposition pulse valve, wherein the opening time range of the pulse valve is 50-2000ms, so that the liquid iridium source is led into the equipment reaction chamber to be adsorbed and react with the surface of the substrate;
s4, using inert gas as carrier gas to clean liquid iridium sources which do not react completely, and byproducts such as 1-ethylcyclopentadienyl-1 and 3-cyclohexadiene generated by the reaction, wherein the cleaning time is 1-200S;
s5, opening a hydrazine reducing agent atomic layer deposition pulse valve, wherein the opening time of the pulse valve is 10-500ms, so that a hydrazine reducing agent precursor is introduced into the equipment reaction chamber, and is adsorbed and reacted with the surface of the substrate;
s6, using inert gas as carrier gas to clean hydrazine reducing agent which is not reacted completely and byproducts such as amine generated by the reaction;
s7, forming a circulating simple substance iridium film;
s8, the thickness of the simple substance iridium film can be accurately controlled by controlling the cycle number.
(III) advantageous effects
Compared with the prior art, the invention provides the atomic layer deposition technology and the method for preparing the iridium film, and the atomic layer deposition technology and the method have the following beneficial effects:
the liquid iridium source Ir is selected as the iridium precursor, so that the problem that the valve is blocked due to condensation of the iridium source in the using process can be avoided, the deposition process can be well controlled, and the production cost is reduced.
The hydrazine reducing agent is selected as the reducing precursor, the simple substance iridium film can be deposited by directly utilizing a thermal atomic layer deposition technology, the method is superior to the gases such as plasma NH3, hydrogen and the like used in the prior art, is more convenient, safer and easier to operate in the use process, can avoid the inconvenience in the operation of plasma hydrogen, plasma ammonia and the like, can simplify the preparation process of the simple substance iridium film, and saves the cost.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
An atomic layer deposition technology and a method for preparing an iridium film comprise a liquid iridium source and a hydrazine reducing agent, wherein the liquid iridium source is used as a precursor, and the hydrazine reducing agent is used as a reductive precursor.
Preferably, the liquid iridium source can adopt 1-ethyl cyclopentadienyl-1, 3-cyclohexadienyl and other raw materials.
Preferably, the hydrazine reducing agent comprises anhydrous hydrazine, methyl hydrazine, ethyl hydrazine, propyl hydrazine, tert-butyl hydrazine and other C1-C5 hydrocarbon chains, and the reducing agent has the structural formula R1R2N-NR3R4Wherein R is1、R2、R3And R4Comprising a hydrogen atom, a hydrocarbon chain of C1-C5, R1、R2、R3And R4May be the same or different.
The first embodiment is as follows:
an iridium film atomic layer deposition method taking 1-ethylcyclopentadienyl-1 as a liquid iridium source precursor and an anhydrous hydrazine reducing agent as a reducing precursor comprises the following steps:
s1, heating the 1-ethyl cyclopentadienyl-1 liquid iridium source raw material to 120 ℃ by adopting atomic layer deposition equipment, and vacuumizing to a limit pressure, wherein the limit pressure after vacuumizing is 0.5 Pa;
s2, after the atomic layer deposition system is heated uniformly, the heating time is 40min, then the carrier gas flow is started to be 20sccm, the temperature of the atomic layer deposition system is heated uniformly to be 200 ℃, and the pressure applied to the atomic layer deposition system is 30 Pa;
s3, opening a 1-ethyl cyclopentadienyl-1 liquid iridium source atomic layer deposition pulse valve, wherein the opening time of the pulse valve is 1000ms, so that the 1-ethyl cyclopentadienyl-1 liquid iridium source is led into the equipment reaction chamber to be adsorbed and reacted with the surface of the substrate;
s4, using nitrogen as carrier gas to clean the 1-ethyl cyclopentadienyl-1 liquid iridium source which is not reacted completely and byproducts such as 1-ethyl cyclopentadienyl-1 and 3-cyclohexadiene generated by the reaction, wherein the cleaning time is 50S;
s5, opening an anhydrous hydrazine reducing agent atomic layer deposition pulse valve, wherein the opening time of the pulse valve is 200ms, so that an anhydrous hydrazine reducing agent precursor is introduced into the equipment reaction chamber, and is adsorbed and reacted with the surface of the substrate;
s6, using nitrogen as carrier gas to clean the anhydrous hydrazine reducing agent which is not completely reacted and the byproducts such as amine generated by the reaction;
s7, forming a circulating simple substance iridium film;
s8, the thickness of the simple substance iridium film can be accurately controlled by controlling the cycle number, 500 cycles are carried out, the thickness of the deposited simple substance iridium film is about 43nm, and the resistivity of the iridium film is tested to be 12 mu omega/cm by a four-probe tester.
Example two:
an iridium film atomic layer deposition method taking 3-cyclohexadienyl as a liquid iridium source precursor and a methylhydrazine reducing agent as a reducing precursor comprises the following steps:
s1, heating the 3-cyclohexadienyl liquid iridium source raw material to 130 ℃ by adopting atomic layer deposition equipment, and vacuumizing to the limit pressure, wherein the limit pressure after vacuumizing is 0.5 Pa;
s2, after the atomic layer deposition system is heated uniformly, the heating time is 40min, then the carrier gas flow is started to be 50sccm, the temperature of the atomic layer deposition system is heated uniformly to be 300 ℃, and the pressure in the atomic layer deposition system is 80 Pa;
s3, opening a 3-cyclohexadienyl liquid iridium source atomic layer deposition pulse valve, wherein the opening time of the pulse valve is 2000ms, so that the 3-cyclohexadienyl liquid iridium source is introduced into the equipment reaction chamber, and is adsorbed and reacted with the surface of the substrate;
s4, using nitrogen as carrier gas to clean the 3-cyclohexadienyl liquid iridium source which is not reacted completely and byproducts such as 1-ethylcyclopentadienyl-1 and 3-cyclohexadiene generated by the reaction, wherein the cleaning time is 80S;
s5, opening a methyl hydrazine reducing agent atomic layer deposition pulse valve, wherein the opening time of the pulse valve is 500ms, so that a methyl hydrazine reducing agent precursor is introduced into the equipment reaction chamber, and is adsorbed and reacted with the surface of the substrate;
s6, using nitrogen as carrier gas to clean the methyl hydrazine reducing agent which is not completely reacted and the byproducts such as amine generated by the reaction;
s7, forming a circulating simple substance iridium film;
s8, the thickness of the simple substance iridium film can be accurately controlled by controlling the cycle times, 300 cycles are carried out, the thickness of the deposited simple substance iridium film is about 27nm, and the resistivity of the iridium film is 35 mu omega/cm through a four-probe tester.
The invention has the beneficial effects that: the liquid iridium source Ir is selected as the iridium precursor, so that the valve blockage caused by the condensation of the iridium source in the use process can be avoided, the deposition process can be well controlled, and the production cost is reduced;
the hydrazine reducing agent is selected as the reducing precursor, the simple substance iridium film can be deposited by directly utilizing a thermal atomic layer deposition technology, the method is superior to the gases such as plasma NH3, hydrogen and the like used in the prior art, is more convenient, safer and easier to operate in the use process, can avoid the inconvenience in the operation of plasma hydrogen, plasma ammonia and the like, can simplify the preparation process of the simple substance iridium film, and saves the cost.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (4)

1. The atomic layer deposition technology and the method for preparing the iridium thin film are characterized by comprising a liquid iridium source and a hydrazine reducing agent, wherein the liquid iridium source is used as a precursor, and the hydrazine reducing agent is used as a reducing precursor.
2. The atomic layer deposition technique and the method according to claim 1, wherein the liquid iridium source is 1-ethylcyclopentadienyl-1, 3-cyclohexadienyl iridium (I) as a raw material.
3. The atomic layer deposition technology and method for preparing iridium film according to claim 1, wherein the hydrazine reducing agent includes anhydrous hydrazine, methyl hydrazine, ethyl hydrazine, propyl hydrazine, tert-butyl hydrazine and other C1-C5 hydrocarbon chains, and the reducing agent has a structural formula of R1R2N-NR3R4Wherein R is1、R2、R3And R4Comprising a hydrogen atom, a hydrocarbon chain of C1-C5, R1、R2、R3And R4May be the same or different.
4. The atomic layer deposition technique and method for preparing an iridium thin film according to claim 1, wherein the method comprises the following steps:
s1, heating the liquid iridium source raw material to a temperature range of 100-150 ℃ by adopting atomic layer deposition equipment, and vacuumizing to a limit pressure, wherein the limit pressure after vacuumizing is 0.1-10 Pa;
s2, after the atomic layer deposition system is heated uniformly, the heating time is 40-60 min, then the carrier gas flow is started to be 10-200sccm, the temperature range of the atomic layer deposition system heated uniformly is 100-400 ℃, and the pressure range in the atomic layer deposition system is 10-200 Pa;
s3, opening a liquid iridium source atomic layer deposition pulse valve, wherein the opening time range of the pulse valve is 50-2000ms, so that the liquid iridium source is led into the equipment reaction chamber to be adsorbed and react with the surface of the substrate;
s4, using inert gas as carrier gas to clean liquid iridium sources which do not react completely, and byproducts such as 1-ethylcyclopentadienyl-1 and 3-cyclohexadiene generated by the reaction, wherein the cleaning time is 1-200S;
s5, opening a hydrazine reducing agent atomic layer deposition pulse valve, wherein the opening time of the pulse valve is 10-500ms, so that a hydrazine reducing agent precursor is introduced into the equipment reaction chamber, and is adsorbed and reacted with the surface of the substrate;
s6, using inert gas as carrier gas to clean hydrazine reducing agent which is not reacted completely and byproducts such as amine generated by the reaction;
s7, forming a circulating simple substance iridium film;
s8, the thickness of the simple substance iridium film can be accurately controlled by controlling the cycle number.
CN202010229705.6A 2020-03-27 2020-03-27 Atomic layer deposition technology and method for preparing iridium film Pending CN111254412A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009235439A (en) * 2008-03-26 2009-10-15 Tosoh Corp Method for manufacturing thin film of metallic iridium and/or iridium oxide
TW201139715A (en) * 2010-03-19 2011-11-16 Sigma Aldrich Co Methods for preparing thin films by atomic layer deposition using hydrazines
CN107428677A (en) * 2015-03-06 2017-12-01 株式会社Adeka Diaza dialkenyl compound, film, which are formed, uses raw material, the manufacture method of film and diaza diolefin compound
JP2018178177A (en) * 2017-04-07 2018-11-15 東ソー株式会社 Manufacturing method of metallic thin film
US20190367545A1 (en) * 2017-03-24 2019-12-05 Tanaka Kikinzoku Kogyo K.K. Chemical deposition raw material including iridium complex and chemical deposition method using the chemical deposition raw material

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009235439A (en) * 2008-03-26 2009-10-15 Tosoh Corp Method for manufacturing thin film of metallic iridium and/or iridium oxide
TW201139715A (en) * 2010-03-19 2011-11-16 Sigma Aldrich Co Methods for preparing thin films by atomic layer deposition using hydrazines
CN107428677A (en) * 2015-03-06 2017-12-01 株式会社Adeka Diaza dialkenyl compound, film, which are formed, uses raw material, the manufacture method of film and diaza diolefin compound
US20190367545A1 (en) * 2017-03-24 2019-12-05 Tanaka Kikinzoku Kogyo K.K. Chemical deposition raw material including iridium complex and chemical deposition method using the chemical deposition raw material
JP2018178177A (en) * 2017-04-07 2018-11-15 東ソー株式会社 Manufacturing method of metallic thin film

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