CN115874151A - Preparation method of large-area palladium sulfide or/and palladium disulfide nano film - Google Patents
Preparation method of large-area palladium sulfide or/and palladium disulfide nano film Download PDFInfo
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- CN115874151A CN115874151A CN202211050004.1A CN202211050004A CN115874151A CN 115874151 A CN115874151 A CN 115874151A CN 202211050004 A CN202211050004 A CN 202211050004A CN 115874151 A CN115874151 A CN 115874151A
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Abstract
The invention discloses a preparation method of a large-area palladium sulfide or/and palladium disulfide nano film. The controllable preparation of the palladium sulfide, palladium disulfide or the mixed phase nano film of the palladium sulfide and the palladium disulfide can be realized by adopting an electron beam evaporation coating and chemical vapor deposition method and changing the thickness of the pre-deposited palladium metal nano film. The method comprises the following steps: 1. and (3) evaporating palladium metal nano films with different thicknesses to a silicon dioxide substrate by using an electron beam evaporation coating instrument. 2. And placing the sulfur powder in a first temperature zone of a tubular furnace, placing a growth substrate in a second temperature zone, and performing controllable growth of the large-area palladium sulfide, palladium disulfide or mixed phase nano film of the palladium sulfide and the palladium disulfide by using a normal-pressure chemical vapor deposition method. The palladium sulfide and palladium disulfide nano film has wide application prospect in various industrial and technical fields due to unique physical and chemical properties, such as application in catalysts, acid-resistant high-temperature electrodes, solar cells and the like. The method can realize the industrial production of the palladium sulfide, the palladium disulfide or the mixed phase nano film of the palladium sulfide and the palladium disulfide.
Description
Technical Field
The invention relates to palladium-based sulfide, in particular to a preparation method of a large-area palladium sulfide or/and palladium disulfide nano film.
Background
Palladium-based sulfides (PdS ) 2 、Pd x S y ) Is widely applied to various industrial and technical fields, such as photodetectors, catalysts, sensors, acid-resistant high-temperature electrodes, solar cells and the like. The palladium sulfide is an n-type semiconductor of a tetragonal system, has a band gap energy of 1.6eV, and has excellent physical and chemical properties such as thermoelectric, photoelectrochemical, photovoltaic properties and the like, which make it applied to the fields of catalysts, acid-resistant high-temperature electrodes and the like. Palladium disulfide is a member of the group 10 transition metal dihalide family, has a unique pentagonal crystal structure, unlike other common two-dimensional materials, in which each palladium atom is bonded to four sulfur atoms in the same layer, and two adjacent sulfur atoms are bonded to form a covalent bond, and the layers are bonded together by van der waals forces. The single-layer palladium disulfide is an indirect bandgap semiconductor, the bandgap is about 1.28eV, and the electron mobility can reach 258.06cm 2 v -1 s -1 . As the number of layers increases, the band gap of the palladium disulfide gradually decreases and eventually turns into a semi-metallic phase. Due to the interesting characteristics, the method has potential application prospects in the field of two-dimensional functional devices such as field effect transistors, gas sensors and the like. At present, the preparation methods of palladium sulfide include a photochemical method, an aerosol auxiliary method, a chemical vapor deposition method, a direct vulcanization method and the like, and the common preparation methods of palladium disulfide include mechanical stripping, liquid phase stripping, physical vapor deposition and the like. However, these preparation methods are complicated in operation, high in preparation cost, poor in controllability, and incapable of realizing industrial application, and the preparation of large-area palladium sulfide, palladium disulfide or mixed phase nano-film of palladium sulfide and palladium disulfide still has great challenges.
Disclosure of Invention
Aiming at the technical problems that the preparation method of palladium-based sulfide in the prior art is complex in operation, high in preparation cost and poor in controllability, and industrial application is difficult to realize, the invention provides a preparation method of a large-area palladium sulfide or/and palladium disulfide nano film. The preparation method has high controllability, and the obtained palladium sulfide, palladium disulfide or mixed phase nano film of the palladium sulfide and the palladium disulfide has wide application prospects in the fields of light detection, catalysts, sensors, acid-resistant high-temperature electrodes, solar cells and the like, and the palladium sulfide and palladium disulfide nano film is very stable in the normal-temperature atmospheric environment, so that guarantee is provided for further research on physical properties of palladium sulfide and palladium disulfide nano materials.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a large-area palladium sulfide or/and palladium disulfide nano film comprises the following steps:
1) Evaporating palladium metal nano films with different thicknesses to a substrate through an electron beam evaporation coating instrument;
2) Placing the alumina boat filled with the sulfur powder to a first temperature zone heating center, and placing a silica substrate evaporated with palladium in a second temperature zone heating center of a double-temperature zone tube furnace;
3) Introducing argon into a reaction cavity in the tubular furnace for cleaning;
4) Raising the temperature of the tubular furnace to ensure that the temperature of the first temperature zone is raised to 200-300 ℃, and the temperature of the second temperature zone is raised to 400-600 ℃ for vulcanization;
5) And after the growth is finished, naturally cooling the temperature to room temperature, and closing argon to obtain the palladium sulfide or/and palladium disulfide nano film.
Further, the thickness of the palladium metal nano-film is one of 1 nm, 2 nm, 4 nm and 10 nm.
Further, in step 1), the area of the substrate can reach 3cm × 3cm.
Further, the substrate is one of soda-lime glass, a fluorine crystal mica substrate, sapphire, graphene, molybdenum disulfide, tungsten disulfide, molybdenum diselenide and tungsten diselenide.
Further, in the step 2), the dosage of the sulfur powder is increased along with the temperature rise of the first temperature zone, the dosage of the sulfur powder is 0.8-1.0g at the temperature of 200 ℃, the mass of the sulfur powder is correspondingly increased by 0.1g every time the temperature is increased by 20 ℃, and the purity of the sulfur powder is more than 99.5%.
Further, in the step 3), the flow rate of argon is 50-100sccm.
Further, in the step 4), the growth time is 10 to 60 minutes.
Further, in the step 5), when a palladium metal film with the thickness of 1 nanometer is evaporated on the substrate in the step 1), the vulcanization product is pure palladium disulfide; when a palladium metal film with the thickness of 2 nanometers is evaporated on a substrate, a vulcanization product is a mixed phase film of palladium disulfide and palladium sulfide, and the area ratio of the palladium disulfide to the palladium sulfide is 30-40%: 70 to 60 percent; when a palladium metal film with the thickness of 4 nanometers is evaporated on a substrate, a vulcanization product is a mixed phase film of palladium disulfide and palladium sulfide, and the area ratio of the palladium disulfide to the palladium sulfide is 2% -7%: 98% -93%; when the palladium metal film with the thickness of 10 nanometers is evaporated on the substrate, the vulcanized product is a pure palladium sulfide film.
Compared with the prior art, the invention has the following beneficial effects:
1) The controllable preparation of large-area high-quality palladium sulfide or/and palladium disulfide nano film can be realized by the method of combining the electron beam evaporation coating with the atmospheric pressure chemical vapor deposition.
2) The traditional method for synthesizing palladium sulfide and palladium disulfide involves using H 2 S gas or vacuum sealed quartz tube devices, and these manufacturing methods are complicated to operate and H 2 S gas is toxic, and the method has strong operation flexibility and high safety.
3) The use of the atmospheric pressure chemical vapor deposition method can realize the precise synthesis of the palladium sulfide, the palladium disulfide or the mixed phase nano film of the palladium sulfide and the palladium disulfide with large area, high uniformity and high quality.
4) The palladium disulfide nano film prepared on the silicon dioxide substrate can be used for preparing a thin film field effect transistor (TFT) array with uniform performance by utilizing a semiconductor process.
5) Different materials can be selected for the evaporation substrate, so that application exploration in different fields can be realized.
Drawings
FIG. 1 is a digital photograph of a Pd disulfide nano-film prepared by electron beam evaporation (Pd metal nano-film deposition thickness is 1 nm) and chemical vapor deposition method corresponding to example 1;
FIG. 2 shows the results of optical microscopy and Raman spectroscopy of a palladium disulfide nanofilm prepared by electron beam evaporation coating (palladium metal nanofilm deposition thickness is 1 nm) and chemical vapor deposition, corresponding to example 1;
FIG. 3 shows the results of optical microscopy and Raman spectroscopy on the mixed-phase nanofilm of Pd sulfide and Pd disulfide prepared by the electron beam evaporation coating (Pd metal nanofilm deposition thickness is 2 nm) and chemical vapor deposition method in example 6;
FIG. 4 shows the results of optical microscopy and Raman spectroscopy on the mixed-phase nanofilm of palladium sulfide and palladium disulfide prepared by the electron beam evaporation coating (palladium metal nanofilm deposition thickness is 4 nm) and chemical vapor deposition method in example 7;
FIG. 5 shows the results of optical microscopy characterization and Raman spectroscopy characterization of the palladium sulfide nano-film prepared by electron beam evaporation coating (palladium metal nano-film deposition thickness of 10 nm) and chemical vapor deposition method, corresponding to example 8;
FIG. 6 shows the results of atomic force microscopy and Kelvin probe microscopy of the palladium disulfide nano-film prepared by electron beam evaporation coating (palladium metal nano-film deposition thickness is 1 nm) and chemical vapor deposition method corresponding to example 1;
FIG. 7 shows the results of atomic force microscopy and Kelvin probe microscopy of palladium sulfide and palladium disulfide mixed phase nano-film prepared by electron beam evaporation coating (palladium metal nano-film deposition thickness is 4 nm) and chemical vapor deposition method corresponding to example 7;
FIG. 8 shows the results of atomic force microscopy and Kelvin probe microscopy of Pd sulfide nano-film prepared by electron beam evaporation coating (Pd metal nano-film deposition thickness is 10 nm) and chemical vapor deposition method in example 8;
FIG. 9 shows the Raman spectrum surface scanning characterization results of the palladium disulfide nano-film prepared by the electron beam evaporation coating (the deposition thickness of the palladium metal nano-film is 1 nm) and the chemical vapor deposition method corresponding to example 1;
FIG. 10 is the Raman spectrum surface scanning characterization result of the mixed-phase nano-film of palladium sulfide and palladium disulfide prepared by the electron beam evaporation coating (the deposition thickness of the palladium metal nano-film is 2 nm) and the chemical vapor deposition method in example 6;
FIG. 11 is the Raman spectrum surface scanning characterization result of the mixed-phase nano-film of palladium sulfide and palladium disulfide prepared by the electron beam evaporation coating (the deposition thickness of the palladium metal nano-film is 4 nm) and the chemical vapor deposition method in example 7;
FIG. 12 is the Raman spectrum surface scanning characterization result of the Pd sulfide nano-film prepared by the electron beam evaporation coating (Pd metal nano-film deposition thickness is 10 nm) and the chemical vapor deposition method corresponding to example 8;
FIG. 13 shows the TEM and TEM characterization results of the Pd disulfide nano-film prepared by the E-beam evaporation coating (Pd metal nano-film deposition thickness is 1 nm) and the CVD method in example 1;
FIG. 14 shows the TEM and TEM characterization results of example 8, wherein the TEM and TEM characterization results of the Pd sulfide nano-film are obtained by the E-beam evaporation plating (Pd metal nano-film deposition thickness is 10 nm) and the CVD method;
fig. 15 is a transistor array manufactured by a semiconductor process using an electron beam evaporation coating (the deposition thickness of the palladium metal nano film is 1 nm) and a palladium disulfide nano film manufactured by a chemical vapor deposition method, corresponding to example 1.
Detailed Description
The present invention will be described in further detail with reference to the drawings and specific examples, but the present invention is not limited thereto.
Vapor deposition of palladium metal films of different thicknesses
And (3) respectively evaporating palladium metal films with different thicknesses (1 nanometer, 2 nanometers, 4 nanometers and 10 nanometers) to a silicon dioxide substrate through an electron beam evaporation coating instrument.
Example 1
Evaporating a 1 nanometer palladium metal film to a silicon dioxide substrate through an electron beam evaporation coating instrument, placing the substrate to a second temperature zone heating center of a double-temperature-zone tube furnace, placing an aluminum oxide boat containing 0.8g of sulfur powder to the first temperature zone heating center, then introducing argon (500 sccm) into a reaction cavity, cleaning the reaction cavity, discharging residual air in the cavity, and cleaning for 30 minutes. And then, carrying out temperature programming to ensure that the heating central temperature of the first temperature zone of the tubular furnace reaches 200 ℃ of the specified temperature and the heating central temperature of the second temperature zone of the tubular furnace reaches 400 ℃ of the specified temperature. And argon 50 is used as a carrier gas, sulfur vapor is conveyed to the growth substrate area to realize the growth of the palladium disulfide nano film, and the growth time is 30 minutes. And after the growth is finished, naturally cooling the tube furnace to room temperature, closing argon and taking out the growth substrate.
The obtained palladium disulfide nano film sample is characterized by an optical microscope, a Raman spectrum, an atomic force microscope, a Kelvin probe microscope and a transmission electron microscope, and the results are shown in FIG. 2, FIG. 6, FIG. 9 and FIG. 13. The characterization data of the optical microscope show that the palladium disulfide nano film is very uniform. Characterization of the data by Raman spectroscopy indicated 299cm -1 And 425cm -1 Two characteristic peaks respectively correspond to E of the palladium disulfide g And A g And (4) peak. According to the characterization data of the atomic force microscope and the Kelvin probe microscope, the thickness of the palladium disulfide nano film is about 3.3 nanometers, the potential difference between the palladium disulfide nano film and the silicon dioxide substrate is about 40mV, and the surface potential is aboutThe distribution is even. The surface of the palladium disulfide sample is uniform as shown by Raman spectrum surface scanning. High resolution transmission electron microscopy characterization data shows that in palladium disulfide, the (102) plane corresponds to a lattice distance of 0.3164 nm. Fig. 1 is a digital photograph showing comparison between before and after the experiment of example 1, and fig. 15 is a digital photograph and an optical photograph showing a transistor array prepared by a semiconductor process using the palladium disulfide thin film obtained in example 1.
Example 2
The temperature of the first temperature zone in the example 1 is changed to 250 ℃, the quantity of the sulfur powder is changed to 1.0g, and other preparation conditions are not changed, so that the palladium disulfide nano film can be obtained.
Example 3
The temperature of the second temperature zone in the embodiment 1 is changed to 450 ℃, and other preparation conditions are not changed, so that the palladium disulfide nano film can be obtained.
Example 4
The temperature of the second temperature zone in the embodiment 1 is changed to 500 ℃, other preparation conditions are not changed, and the palladium disulfide nano film can also be obtained.
Example 5
The temperature of the second temperature zone in the example 1 is changed to 600 ℃, other preparation conditions are not changed, and the palladium disulfide nano film can also be obtained.
Example 6
The substrate plated with 1 nanometer palladium metal in the example 1 is changed into the substrate plated with 2 nanometer palladium metal, and other preparation conditions are not changed, so that the palladium sulfide and palladium disulfide mixed phase nano film can be obtained.
The obtained palladium sulfide and palladium disulfide mixed phase nano film sample is subjected to optical microscope, raman spectrum and Raman spectrum surface scanning characterization, and the result is shown in figures 3 and 10. The optical microscope characterization data show that the products are two different substances, and the Raman spectrum characterization result shows that one substance is palladium sulfide, and the other substance is palladium disulfide. Raman spectral area scan characterization data can be further confirmed.
Example 7
The substrate plated with 1 nanometer palladium metal in the example 1 is changed into the substrate plated with 4 nanometer palladium metal, and other preparation conditions are not changed, so that the palladium sulfide and palladium disulfide mixed phase nano film can be obtained.
The obtained palladium sulfide and palladium disulfide mixed phase nano film sample is subjected to optical microscope, raman spectrum, atomic force microscope, kelvin probe microscope and raman spectrum surface scanning characterization, and the results are shown in fig. 4, fig. 7 and fig. 11. The optical microscope characterization data show that the products are two different substances, and the Raman spectrum characterization result shows that one substance is palladium sulfide, and the other substance is palladium disulfide. The raman spectral area scan characterization data can be further confirmed. The characterization data of an atomic force microscope and a Kelvin probe microscope show that the potential difference between the palladium sulfide and the palladium disulfide is about 10mV, and the surface potential is uniformly distributed.
Example 8
The substrate plated with 1 nanometer palladium metal in the example 1 is changed into the substrate plated with 10 nanometer palladium metal, and other preparation conditions are not changed, so that the palladium sulfide nano-film can be obtained.
The obtained palladium sulfide nano film sample is subjected to optical microscope, raman spectrum, atomic force microscope, kelvin probe microscope and raman spectrum surface scanning, and is characterized by a transmission electron microscope, and the results are shown in fig. 5, fig. 8, fig. 12 and fig. 14. The characterization data of the optical microscope show that the palladium sulfide nano film is very uniform. The results of Raman spectrum characterization show 134cm -1 And 334cm -1 Two characteristic peaks at (A) are respectively A of palladium sulfide g And B g And (4) peak. The characterization data of an atomic force microscope and a Kelvin probe microscope prove that the thickness of the palladium sulfide nano film is about 27 nanometers, the potential difference between the palladium sulfide nano film and the silicon dioxide substrate is about 58mV, and the surface potential is uniformly distributed. The scanning and characterization of the spectrum surface of the Raman spectrum shows that the surface of the palladium sulfide sample is uniform. Characterization data from high resolution transmission electron microscopy showed that in palladium sulfide, the (101) plane corresponds to a lattice distance of 0.4801 nanometers.
Examples 9 to 16
The silica substrate in example 1 was replaced with two-dimensional layered materials of soda lime glass, sapphire, a fluorophlogopite base, graphene, molybdenum disulfide, tungsten disulfide, molybdenum diselenide, and tungsten diselenide, respectively.
Claims (8)
1. A preparation method of a large-area palladium sulfide or/and palladium disulfide nano film is characterized by comprising the following steps:
1) Evaporating palladium metal nano films with different thicknesses to a substrate through an electron beam evaporation coating instrument;
2) Placing the alumina boat filled with the sulfur powder to a first temperature zone heating center, and placing a silica substrate evaporated with palladium in a second temperature zone heating center of a double-temperature zone tube furnace;
3) Introducing argon into a reaction cavity in the tubular furnace for cleaning;
4) Raising the temperature of the tubular furnace to ensure that the temperature of the first temperature zone is raised to 200-300 ℃, and the temperature of the second temperature zone is raised to 400-600 ℃ for vulcanization;
5) And after the growth is finished, naturally cooling the temperature to room temperature, and closing argon to obtain the palladium sulfide or/and palladium disulfide nano film.
2. The method of claim 1, wherein the palladium metal nanofilm has a thickness of one of 1 nm, 2 nm, 4 nm, or 10 nm.
3. The method for preparing large-area palladium sulfide or/and palladium disulfide nano film according to claim 1, wherein in step 1), the area of the substrate can reach 3cm x 3cm.
4. The method for preparing a large area palladium sulfide or/and palladium disulfide nano film according to claim 1, wherein the substrate is one of soda-lime glass, fluorine crystal mica substrate, sapphire, graphene, molybdenum disulfide, tungsten disulfide, molybdenum diselenide, and tungsten diselenide.
5. The method for preparing a large-area palladium sulfide or/and palladium disulfide nano film according to claim 1, wherein in the step 2), the amount of sulfur powder is increased along with the temperature rise of the first temperature zone, the amount of sulfur powder is 0.8-1.0g at the temperature of 200 ℃, the mass of sulfur powder is correspondingly increased by 0.1g every time the temperature is increased by 20 ℃, and the purity of sulfur powder is more than 99.5%.
6. The method for preparing a large area palladium sulfide or/and disulfide nano film according to claim 1, wherein in step 3), the flow rate of argon is 50-100sccm.
7. The method for preparing large-area palladium sulfide or/and palladium disulfide nano film according to claim 1, wherein in the step 4), the growth time is 10 to 60 minutes.
8. The method for preparing a large-area palladium sulfide or/and disulfide nano film according to claim 1, wherein in step 5), when a palladium metal film with a thickness of 1 nm is evaporated on the substrate in step 1), the sulfide product is pure palladium disulfide; when a palladium metal film with the thickness of 2 nanometers is evaporated on a substrate, a vulcanization product is a mixed phase film of palladium disulfide and palladium sulfide, and the area ratio of the palladium disulfide to the palladium sulfide is 40% -60%: 60% -50%; when a palladium metal film with the thickness of 4 nanometers is evaporated on the substrate, the vulcanization product is a mixed phase film of palladium disulfide and palladium sulfide, and the area ratio of the palladium disulfide to the palladium sulfide is 1% -3%: 99 to 97 percent; when the palladium metal film with the thickness of 10 nanometers is evaporated on the substrate, the vulcanized product is a pure palladium sulfide film.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117613140A (en) * | 2023-11-23 | 2024-02-27 | 济南大学 | Oxygen-doped palladium diselenide material, preparation method and application thereof in preparation of photoelectric detector |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117613140A (en) * | 2023-11-23 | 2024-02-27 | 济南大学 | Oxygen-doped palladium diselenide material, preparation method and application thereof in preparation of photoelectric detector |
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