CN110551988A - Large-area zirconium disulfide film and atomic layer deposition preparation method thereof - Google Patents

Large-area zirconium disulfide film and atomic layer deposition preparation method thereof Download PDF

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Publication number
CN110551988A
CN110551988A CN201910920860.XA CN201910920860A CN110551988A CN 110551988 A CN110551988 A CN 110551988A CN 201910920860 A CN201910920860 A CN 201910920860A CN 110551988 A CN110551988 A CN 110551988A
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zirconium
precursor
atomic layer
layer deposition
reaction
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张希威
孟丹
胡丹
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Anyang Normal University
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Anyang Normal University
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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
    • C23C16/305—Sulfides, selenides, or tellurides
    • 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]
    • C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations
    • 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]
    • C23C16/45553—Atomic layer deposition [ALD] characterized by the use of precursors specially adapted for ALD
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/56—After-treatment

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

The invention discloses a large-area zirconium disulfide film and an atomic layer deposition preparation method thereof. The preparation process comprises 10-5000 growth cycles, and each growth cycle comprises four steps: 1) firstly, pulse introducing a zirconium precursor into a reaction cavity of the atomic layer deposition system and enabling the zirconium precursor to be adsorbed on the surface of a substrate, 2) pulse introducing high-purity nitrogen into the reaction cavity of the atomic layer deposition system to clean excessive zirconium precursor and reaction byproducts, 3) pulse introducing a sulfur precursor into the reaction cavity of the atomic layer deposition system and enabling the sulfur precursor to perform self-limiting reaction with the zirconium precursor adsorbed on the surface of the substrate and generate a zirconium disulfide atomic layer, and 4) pulse introducing high-purity nitrogen into the reaction cavity of the atomic layer deposition system to clean excessive sulfur precursor and reaction byproducts. The invention has the advantages of accurate and controllable atomic-scale thickness, large area, uniformity and the like.

Description

large-area zirconium disulfide film and atomic layer deposition preparation method thereof
The technical field is as follows:
The invention relates to the field of layered two-dimensional semiconductor materials, in particular to a large-area zirconium disulfide film and an atomic layer deposition preparation method thereof.
background art:
The theoretical calculation shows that ZrS 2 has carrier mobility as high as 1247cm 2 V -1 s -1 and sheet current density of 800 muA/mum at room temperature, and the theoretical calculation band gap of a single layer ZrS 2 is only 1.08eV, so that the narrow band gap makes it very suitable for optoelectronic devices with wide spectral response, and furthermore, similarly to the formation of SiO 2 insulating layer by oxidation in silicon process, ZrS 2 surface can also form high quality ultra-thin high k dielectric film ZrO 2, avoiding the problem that two-dimensional materials such as MoS 2 are difficult to deposit high quality dielectric film due to lack of dangling bond or nucleation point on the surface, thus making it easier to prepare high performance electronic devices, and thus making it more difficult to prepare high performance electronic devices by using a series of methods such as ZrS 2 preparation and photoelectric transistor preparation, ZrS-based on the principle of two-dimensional process, such as the two-dimensional film preparation, the two-dimensional film preparation method is difficult to be applied to prepare large-area, and the problems such as ZrS 9634, ZrS 3637 is difficult to be prepared by a series of two-dimensional chemical peeling, and the method is difficult to prepare high-dimensional thin film with the controlled thickness.
the invention content is as follows:
The invention provides a method for preparing a large-area zirconium disulfide film based on an atomic layer deposition process, aiming at overcoming the problems in the preparation process of the existing atomic-level zirconium disulfide film and obtaining the novel two-dimensional semiconductor material zirconium disulfide with large area, uniformity and accurately controllable thickness and atomic-level thickness.
In order to achieve the purpose, the invention provides a large-area zirconium disulfide film and an atomic layer deposition preparation method thereof, which are characterized in that: the large-area zirconium disulfide film is formed by alternately introducing a zirconium precursor and a sulfur precursor into a reaction cavity and carrying out self-limiting chemical reaction growth on the surface of a substrate.
Preferably, the method is characterized in that: the zirconium precursor is tetra (methylamino) zirconium or tetra (dimethylamino) zirconium, and the purity of the zirconium precursor is 99.9999%.
Preferably, the method is characterized in that: the sulfur precursor is thioacetamide, and the purity of the thioacetamide is 99.9999%.
Preferably, the method is characterized in that: the substrate is one or more of silicon oxide wafer, sapphire, mica, silicon and germanium with smooth surface; the substrate is a whole piece or a fragment with the diameter of 4 inches or less.
Preferably, the method is characterized in that: comprising 10-5000 growth cycles, each growth cycle comprising four steps: 1) firstly, pulse introducing a zirconium precursor into a reaction cavity of the atomic layer deposition system and enabling the zirconium precursor to be adsorbed on the surface of a substrate, 2) pulse introducing high-purity nitrogen into the reaction cavity of the atomic layer deposition system to clean excessive zirconium precursor and reaction byproducts, 3) pulse introducing a sulfur precursor into the reaction cavity of the atomic layer deposition system and enabling the sulfur precursor to perform self-limiting reaction with the zirconium precursor adsorbed on the surface of the substrate and generate a zirconium disulfide atomic layer, and 4) pulse introducing high-purity nitrogen into the reaction cavity of the atomic layer deposition system to clean excessive sulfur precursor and reaction byproducts. Preferably, the method is characterized in that: the temperature of the reaction chamber is set to be 250-400 ℃.
Preferably, the method is characterized in that: setting the temperature of the zirconium precursor to be 80-120 ℃; the pulse time of the zirconium precursor is 0.5 second; the flow rate of the carrier gas of the zirconium precursor was 100 sccm.
preferably, the method is characterized in that: the temperature of the sulfur precursor was set to room temperature: the pulse time of the sulfur precursor is 1 second; the sulfur precursor carrier gas flow was 100 sccm.
Preferably, the method is characterized in that: the purge gas pulse time was 2 seconds and the flow rate was 300 sccm.
preferably, the method is characterized in that: after the required growth cycle is completed, the substrate needs to be taken out of the reaction cavity and placed in a rapid annealing furnace for annealing treatment, wherein the annealing temperature is 500-900 ℃, and the annealing time is 5-20 minutes.
Compared with the prior art, the invention has the following beneficial effects:
1. According to the invention, the atomic layer deposition process is adopted to prepare the atomic-level-thickness two-dimensional zirconium disulfide film, the atomic layer deposition process has the characteristic of self-limitation, and the prepared two-dimensional zirconium disulfide film has the advantages of accurate and controllable atomic-level thickness, large area, uniformity and the like.
2. According to the invention, the atomic layer deposition process is adopted to prepare the atomic-level-thickness two-dimensional zirconium disulfide film, the reaction temperature required by the atomic layer deposition process is lower, the atomic layer deposition process is compatible with a flexible substrate, and the atomic layer deposition process can be combined with subsequent photoetching and other semiconductor processes to realize patterning of the prepared film.
The specific implementation mode is as follows:
The present invention will be described in detail with reference to the following embodiments in order to make the above objects, features and advantages of the invention comprehensible.
Example 1:
putting the cleaned 4-inch silicon oxide wafer into a reaction cavity of an atomic layer deposition system; setting the temperature in a reaction cavity of the atomic layer deposition system to be 250 ℃; adopting tetra (methylethylamino) zirconium as a zirconium precursor, setting the temperature of the zirconium precursor to 80 ℃, adopting high-purity argon as the precursor, and controlling the carrier gas flow to be 100 sccm; taking thioacetamide as a sulfur precursor, taking high-purity argon as the precursor, wherein the carrier gas flow is 100 sccm; high-purity argon gas is used as the cleaning gas, and the flow rate of the cleaning gas is 300 sccm. In one reaction cycle, the steps are as follows: 1) firstly, pulse-introducing a zirconium precursor into a reaction cavity of an atomic layer deposition system and enabling the zirconium precursor to be adsorbed on the surface of a substrate, wherein the pulse time is 0.5 second, 2) secondly, pulse-introducing high-purity nitrogen into the reaction cavity of the atomic layer deposition system to clean excessive hafnium precursor and reaction byproducts, wherein the pulse time is 2 seconds, 3) secondly, pulse-introducing a sulfur precursor into the reaction cavity of the atomic layer deposition system and enabling the sulfur precursor to perform self-limiting reaction with the hafnium precursor adsorbed on the surface of the substrate and generate a zirconium disulfide atomic layer, wherein the pulse time is 1 second, 4) lastly, pulse-introducing high-purity nitrogen into the reaction cavity of the atomic layer deposition system to clean the excessive sulfur precursor and the reaction byproducts, and the pulse time is 2 seconds. The number of reaction cycles required in this example was 100. After the required growth cycle is completed, the substrate needs to be taken out of the reaction cavity and placed in a rapid annealing furnace for annealing treatment, wherein the annealing temperature is 500 ℃, and the annealing time is 20 minutes.
Example 2:
Putting the cleaned 4-inch silicon wafer into a reaction cavity of an atomic layer deposition system; setting the temperature in a reaction cavity of the atomic layer deposition system to 300 ℃; adopting tetra (methylethylamino) zirconium as a zirconium precursor, setting the temperature of the zirconium precursor to be 100 ℃, adopting high-purity argon as the precursor, and controlling the flow rate of carrier gas to be 100 sccm; taking thioacetamide as a sulfur precursor, taking high-purity argon as the precursor, wherein the carrier gas flow is 100 sccm; high-purity argon gas is used as the cleaning gas, and the flow rate of the cleaning gas is 300 sccm. In one reaction cycle, the steps are as follows: 1) firstly, pulse-introducing a zirconium precursor into a reaction cavity of an atomic layer deposition system and enabling the zirconium precursor to be adsorbed on the surface of a substrate, wherein the pulse time is 0.5 second, 2) secondly, pulse-introducing high-purity nitrogen into the reaction cavity of the atomic layer deposition system to clean excessive hafnium precursor and reaction byproducts, wherein the pulse time is 2 seconds, 3) secondly, pulse-introducing a sulfur precursor into the reaction cavity of the atomic layer deposition system and enabling the sulfur precursor to perform self-limiting reaction with the hafnium precursor adsorbed on the surface of the substrate and generate a zirconium disulfide atomic layer, wherein the pulse time is 1 second, 4) lastly, pulse-introducing high-purity nitrogen into the reaction cavity of the atomic layer deposition system to clean the excessive sulfur precursor and the reaction byproducts, and the pulse time is 2 seconds. The number of reaction cycles required in this example was 100. After the required growth cycle is completed, the substrate needs to be taken out of the reaction cavity and placed in a rapid annealing furnace for annealing treatment, wherein the annealing temperature is 700 ℃ and the annealing time is 10 minutes.
Example 3:
The method comprises the steps of putting a cleaned sapphire substrate with the thickness of 1 x 2cm 2 and a cleaned mica sheet with the thickness of 2 x 2cm 2 into a reaction cavity of an atomic layer deposition system, setting the temperature in the reaction cavity of the atomic layer deposition system to 350 ℃, adopting zirconium tetra (dimethylamino) as a zirconium precursor with the temperature of 120 ℃, adopting high-purity argon gas with the flow rate of 100sccm as a precursor, adopting thioacetamide as a sulfur precursor with the flow rate of 100sccm as a precursor, adopting high-purity argon gas with the flow rate of 100sccm as a cleaning gas with the flow rate of 300sccm as a cleaning gas, and performing a reaction cycle, wherein the steps comprise 1) firstly, pulse-introducing the zirconium precursor into the reaction cavity of the atomic layer deposition system and enabling the zirconium precursor to be adsorbed on the surface of the substrate, the pulse time is 0.5 seconds, 2) secondly, pulse-introducing high-purity nitrogen gas into the reaction cavity of the atomic layer deposition system to clean the excess hafnium precursor and the reaction precursor, the excess reaction time is 2 seconds, 3) then, pulse-introducing the sulfur precursor into the reaction cavity of the atomic layer deposition system, enabling the sulfur precursor to perform self-limiting reaction and the zirconium precursor to generate zirconium disulfide precursor, the atomic layer deposition system, the annealing, and the annealing process is performed for the annealing, and the annealing, the annealing process is performed for the.

Claims (10)

1. A large area zirconium disulfide film which characterized in that: the large-area zirconium disulfide film is formed by alternately introducing a zirconium precursor and a sulfur precursor into a reaction cavity and carrying out self-limiting chemical reaction growth on the surface of a substrate.
2. The large area zirconium disulfide film of claim 1, wherein: the zirconium precursor is tetra (methylamino) zirconium or tetra (dimethylamino) zirconium, and the purity of the zirconium precursor is 99.9999%.
3. The large area zirconium disulfide film of claim 1, wherein: the sulfur precursor is thioacetamide, and the purity of the thioacetamide is 99.9999%.
4. The large area zirconium disulfide film of claim 1, wherein: the substrate is one or more of silicon oxide wafer, sapphire, mica, silicon and germanium with smooth surface; the substrate is a whole piece or a fragment with the diameter of 4 inches or less.
5. An atomic layer deposition preparation method of a large-area zirconium disulfide film is characterized by comprising the following steps: comprising 10-5000 growth cycles, each growth cycle comprising four steps: 1) firstly, pulse introducing a zirconium precursor into a reaction cavity of the atomic layer deposition system and enabling the zirconium precursor to be adsorbed on the surface of a substrate, 2) pulse introducing high-purity nitrogen into the reaction cavity of the atomic layer deposition system to clean excessive zirconium precursor and reaction byproducts, 3) pulse introducing a sulfur precursor into the reaction cavity of the atomic layer deposition system and enabling the sulfur precursor to perform self-limiting reaction with the zirconium precursor adsorbed on the surface of the substrate and generate a zirconium disulfide atomic layer, and 4) pulse introducing high-purity nitrogen into the reaction cavity of the atomic layer deposition system to clean excessive sulfur precursor and reaction byproducts.
6. The method for preparing large-area zirconium disulfide film by atomic layer deposition according to claim 5, wherein: the temperature of the reaction chamber is set to be 250-400 ℃.
7. The method for preparing large-area zirconium disulfide film by atomic layer deposition according to claim 5, wherein: setting the temperature of the zirconium precursor to be 80-120 ℃; the pulse time of the zirconium precursor is 0.5 second; the flow rate of the carrier gas of the zirconium precursor was 100 sccm.
8. The method for preparing large-area zirconium disulfide film by atomic layer deposition according to claim 5, wherein: setting the temperature of the sulfur precursor to room temperature; the pulse time of the sulfur precursor is 1 second; the sulfur precursor carrier gas flow was 100 sccm.
9. The method for preparing large-area zirconium disulfide film by atomic layer deposition according to claim 5, wherein: the purge gas pulse time was 2 seconds and the flow rate was 300 sccm.
10. The method for preparing large-area zirconium disulfide film by atomic layer deposition according to claim 5, wherein: after the required growth cycle is completed, the substrate needs to be taken out of the reaction cavity and placed in a rapid annealing furnace for annealing treatment, wherein the annealing temperature is 500-900 ℃, and the annealing time is 5-20 minutes.
CN201910920860.XA 2019-09-17 2019-09-17 Large-area zirconium disulfide film and atomic layer deposition preparation method thereof Pending CN110551988A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111876748A (en) * 2020-07-16 2020-11-03 北京大学深圳研究生院 Metal sulfide thin film based on organic sulfur precursor and preparation method thereof
CN113429605A (en) * 2021-06-28 2021-09-24 复旦大学 Polymer semiconductor film, preparation method thereof and gas sensor

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111876748A (en) * 2020-07-16 2020-11-03 北京大学深圳研究生院 Metal sulfide thin film based on organic sulfur precursor and preparation method thereof
CN113429605A (en) * 2021-06-28 2021-09-24 复旦大学 Polymer semiconductor film, preparation method thereof and gas sensor
CN113429605B (en) * 2021-06-28 2022-08-05 复旦大学 Polymer semiconductor film, preparation method thereof and gas sensor

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Application publication date: 20191210