CN115821217A - Large-area palladium sulfide film, preparation process and application - Google Patents
Large-area palladium sulfide film, preparation process and application Download PDFInfo
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Abstract
The invention provides a large-area palladium sulfide film, a preparation process and application, which are realized by applying a double-temperature-area tubular furnace, wherein an upstream constant-temperature area and a downstream constant-temperature area are arranged in the double-temperature-area tubular furnace, heating devices are arranged in the upstream constant-temperature area and the downstream constant-temperature area, a magnetic boat filled with sulfur powder is placed in the upstream constant-temperature area, and a magnetic boat filled with a substrate of a metal Pd film is placed in the downstream constant-temperature area, and the preparation process comprises the following steps: preparing a metal Pd film by using an electron beam evaporation instrument, placing a magnetic boat of a substrate filled with the metal Pd film in a downstream constant temperature area of a double-temperature-area tube furnace, and placing the magnetic boat filled with sulfur powder in an upstream constant temperature area; and (3) introducing hydrogen-containing carrier gas into the double-temperature-zone tubular furnace, controlling the temperature of the upstream constant-temperature zone to be higher than 200 ℃ so as to volatilize sulfur powder into sulfur steam, and controlling the temperature range of the downstream constant-temperature zone to be 350-750 ℃ so as to vulcanize the metal Pd film, thereby finally obtaining a palladium-sulfur product. The preparation process of the invention has no complex operation, simple equipment and good reproducibility.
Description
Technical Field
The invention belongs to the field of film material preparation, and particularly relates to a large-area palladium sulfide film, a preparation process and application.
Background
The two-dimensional material has the ultrathin characteristic, and often has special performance different from that of a block material. Such as energy band structure and magnetic structure, etc. At present, researches on two-dimensional materials are increasing, and the research fields relate to electricity, photoelectricity, spintronics, valley electronics and the like, and the researches show that the two-dimensional materials are expected to be widely varied in the fields of next-generation logic operation, optical detection, light emission, magnetic storage and the like. At this stage, however, two-dimensional materials still face many challenges in synthesis. For example, in the synthesis of two-dimensional materials, under the combined influence of ultra-fast kinetics and thermodynamics, the synthesized materials often have a heterogeneous coexistence phenomenon; the size of the two-dimensional material synthesis of single crystals at present is still relatively small, often in the micrometer range, and the promotion of industrial application is still very challenging.
In order to avoid the phenomenon of multiphase coexistence, a single crystal block material can be grown firstly in a chemical vapor transport mode, and then a two-dimensional material with proper layers is obtained in a mechanical stripping mode. Or, a layer of ultrathin metal film can be deposited firstly, and then the ultrathin metal film reacts with the oxygen family gaseous simple substance at high temperature, so that the reaction rate is reduced, and byproducts caused by ultra-fast kinetics are avoided. The compounds obtained by the two modes are generally single substances, the latter has no limit on the size, and the reaction of the ultrathin metal film layer and the oxygen family gaseous elementary substance is also beneficial to the preparation of large-area two-dimensional materials.
Based on the above studies: considering that elemental sulfur has a melting point of 112.8 ℃, it is expected that a large-area thin film can be produced by sulfurizing a large-area metal film layer because a higher vapor pressure can be formed at a lower temperature. In addition, the palladium sulfur compound has research potential in the fields of catalytic hydrogenation, photoelectricity and the like. There are many kinds of palladium sulfur compounds, including PdS, pdS 3 ，PdS 2 ，Pd 3 S，Pd 4 S and Pd 16 S 7 . Wherein, pdS can kill (HeLa) cancer cells and has superconductivity; theoretical calculation of predicted PdS 2 Narrow bandgap semiconductors in the two-dimensional limit, while having a high valueThe carrier mobility.
However, the palladium-sulfur compound often has a non-pure phase phenomenon during the synthesis process, and the synthesis of a palladium sulfide membrane with a specific compound ratio is expected by sulfurizing an ultrathin metal palladium membrane. Therefore, it is necessary to provide a large-area palladium sulfide thin film, a preparation process and an application thereof to solve the above technical problems.
Disclosure of Invention
Based on this, the present invention aims to provide a large-area palladium sulfide thin film, a preparation process and an application thereof, so as to solve the above technical problems.
Specifically, the invention provides a preparation process of a large-area palladium sulfide film, which is realized by applying a double-temperature-area tubular furnace, wherein an upstream constant-temperature area and a downstream constant-temperature area are arranged in the double-temperature-area tubular furnace, heating devices are arranged in the upstream constant-temperature area and the downstream constant-temperature area, a magnetic boat filled with sulfur powder is placed in the upstream constant-temperature area, and a magnetic boat filled with a substrate of a metal Pd film is placed in the downstream constant-temperature area, and the preparation process comprises the following steps:
preparing a metal Pd film by using an electron beam evaporation instrument, then placing a magnetic boat of a substrate filled with the metal Pd film in a downstream constant temperature area of a double-temperature-area tube furnace, and placing the magnetic boat filled with sulfur powder in an upstream constant temperature area;
and (3) introducing hydrogen-containing carrier gas into the double-temperature-zone tubular furnace, controlling the temperature of the upstream constant-temperature zone to be higher than 200 ℃ so as to volatilize sulfur powder into sulfur steam, and controlling the temperature range of the downstream constant-temperature zone to be 350-750 ℃ so as to vulcanize the metal Pd film, thereby finally obtaining a palladium-sulfur product.
The preparation process of the large-area palladium sulfide film comprises the following step of preparing a carrier gas containing hydrogen, wherein the carrier gas containing hydrogen comprises Ar and H 2 Ar flow rate of 20sccm, H 2 The flow rate of (2) is 1sccm.
The preparation process of the large-area palladium sulfide film comprises the step of vulcanizing a metal Pd film, wherein the corresponding vulcanizing time is 40min.
The preparation process of the large-area palladium sulfide film comprises the step of preparing a metal Pd film by using an electron beam evaporation instrument, wherein the metal Pd put into the electron beam evaporation instrument is blocky, the particle size is 2.5mm, and the thickness of the prepared metal Pd film is controlled within 10 nm.
The preparation process of the large-area palladium sulfide film comprises the step of adding sulfur powder into a metal Pd film in a two-temperature-zone tubular furnace, wherein the mass ratio of the added sulfur powder to the metal Pd film is more than 10000.
The preparation process of the large-area palladium sulfide film is characterized in that the vulcanization time for preparing the palladium sulfide film with the thickness of 1-10 nm is 20-60 min.
In the preparation process of the large-area palladium sulfide film, in the step of vulcanizing the metal Pd film, when the vulcanization temperature of the metal Pd film is 350 ℃, the corresponding product is PdS 3 (ii) a When the vulcanization temperature of the metal Pd membrane is 450 ℃, the corresponding product is PdS 2 (ii) a When the sulfurization temperature of the metal Pd membrane is 550 ℃, the corresponding product is PdS 2 。
In the preparation process of the large-area palladium sulfide film, in the step of vulcanizing the metal Pd film, when the vulcanization temperature of the metal Pd film is 650 ℃, the corresponding product is PdS; when the sulfidation temperature of the metal Pd film is 750 ℃, the corresponding product is PdS.
The invention also provides a large-area palladium sulfide film, wherein the large-area palladium sulfide film is prepared by applying the preparation process of the large-area palladium sulfide film, and the large-area palladium sulfide film comprises PdS and PdS 2 And PdS 3 。
The invention also provides application of the large-area palladium sulfide film, wherein the large-area palladium sulfide film is prepared by the preparation process of the large-area palladium sulfide film, and PdS is prepared by the large-area palladium sulfide film 2 A MOS transistor.
The invention provides a large-area palladium sulfide film, a preparation process and application thereof, the prepared palladium sulfide film has larger area, and a plurality of substrates of selectable metal Pd films, including silicon wafers, sapphires, metals and the like, are expected to be applied to the fields of catalysis, electronic devices, photoelectricity and the like. The preparation process of the invention has no complicated operation steps, simple equipment, simple and easy operation and good reproducibility.
Additional features and advantages of the disclosure will be set forth in the description which follows, or in part may be learned by the practice of the above-described techniques of the disclosure, or may be learned by practice of the disclosure.
In order to make the aforementioned and other objects, features and advantages of the present invention comprehensible, preferred embodiments accompanied with figures are described in detail below.
Drawings
FIG. 1 is a schematic structural view of a dual-temperature-zone tube furnace according to the present invention;
FIG. 2 is a Raman spectrum of a palladium sulfide thin film obtained after vulcanization at 350 ℃ in the present invention;
FIG. 3 is a Raman spectrum of a palladium sulfide thin film obtained after vulcanization at 450 ℃ in the invention;
FIG. 4 is a Raman spectrum of a palladium sulfide thin film obtained after sulfidation at 550 ℃ in the present invention;
FIG. 5 is a Raman spectrum of a palladium sulfide thin film obtained after vulcanization at 650 ℃ in the present invention;
FIG. 6 is a Raman spectrum of a palladium sulfide thin film obtained after vulcanization at 750 ℃ in the present invention;
FIG. 7 shows PdS of the present invention 2 Transfer profile of a MOS transistor.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1, the present invention provides a preparation process of a large-area palladium sulfide thin film, wherein the preparation process is implemented by using a dual-temperature-zone tube furnace, and an upstream constant-temperature zone and a downstream constant-temperature zone are arranged in the dual-temperature-zone tube furnace. Heating devices are arranged in the upstream constant temperature area and the downstream constant temperature area, the magnetic boat filled with the sulfur powder is placed in the upstream constant temperature area, and the magnetic boat filled with the substrate of the metal Pd film is placed in the downstream constant temperature area.
Specifically, the preparation process of the large-area palladium sulfide film provided by the invention comprises the following steps:
step one, preparing a metal Pd film by using an electron beam evaporation instrument, then placing a magnetic boat of a substrate filled with the metal Pd film in a downstream constant temperature area of a double-temperature-area tube furnace, and placing the magnetic boat filled with sulfur powder in an upstream constant temperature area.
In the step of preparing the metal Pd film using the electron beam evaporator, the metal Pd put into the electron beam evaporator was in a block shape with a particle diameter of 2.5mm, and the metal Pd powder could not be used in the experiment. It should be noted that, in the double-temperature-zone tube furnace provided by the present invention, the temperature variation needs to be controlled within ± 10 ℃, and the impurities generated may be caused by the temperature variation exceeding 10 ℃, so the temperature control capability of the vulcanizing device in the present invention needs to be very accurate.
In the invention, the preparation process of the metal Pd film is an electron beam evaporation process, and the growth mode of the metal Pd film is an island-shaped growth mode. Therefore, in the preparation of the nanometer metal Pd film, the nucleation density of the crystal needs to be strictly regulated. Particularly, when the metal Pd film with the thickness of less than 5nm is prepared, in order to avoid the problem that islands generated by nucleation are not connected with each other, nucleation sites in the deposition of the metal Pd film need to be increased in the experiment, and the specific operation mode can be realized by reducing the temperature of a deposition substrate, increasing the deposition rate, increasing the vacuum degree of a cavity and the like.
Further, in this step, the thickness of the prepared metallic Pd film was controlled within 10 nm. It should be added here that the thickness of the metal Pd film is very thin, and notToo thick can result in incomplete curing of the underlying Pd film. Meanwhile, according to the research of the prior theoretical calculation, the method has the following findings: bulk PdS 2 The material is not a semiconductor and therefore the generation of PdS needs to be avoided in experiments 2 The number of layers is too large, and the metal property of the bulk material is presented.
And step two, introducing hydrogen-containing carrier gas into the double-temperature-zone tubular furnace, controlling the temperature of the upstream constant-temperature zone to be higher than 200 ℃ so as to volatilize sulfur powder into sulfur steam, and controlling the temperature range of the downstream constant-temperature zone to be 350-750 ℃ so as to vulcanize the metal Pd film, thereby finally obtaining a palladium-sulfur product.
Wherein the hydrogen-containing carrier gas comprises Ar and H 2 . The flow rate of Ar was 20sccm, H 2 The flow rate of (2) is 1sccm.
As a supplementary note, the volatilization temperature of the sulfur powder needs to exceed 200 ℃ in order to obtain highly active S 2 Molecule, S 2 The molecule needs to start to be produced above 200 ℃. Although the temperature of metal Pd is more than 350 ℃ during the vulcanization process, the temperature already exceeds S 2 The molecular generation temperature, but if the volatilization temperature of the sulfur powder is less than 200 ℃, the vulcanization effect is found to be poor through experiments, and the possible reason is that when the temperature is less than 200 ℃, the volatilized sulfur powder is S consisting of polysulfides n (n > 2), when these molecules are volatilized above the metal Pd film, they are not readily decomposed into highly active S due to the flow of the carrier gas even if they are deposited on the surface of the metal Pd film 2 Molecules are transported into the exhaust by the carrier gas.
Specifically, in this embodiment, 250 ℃ is selected as the volatilization temperature of the sulfur powder, so as to adjust the proper S by temperature 2 The vapor pressure of the molecule. In addition, the volatilization temperature of the sulfur powder cannot be too high, because the liquefaction temperature of the sulfur powder is 112.8 ℃, so the sulfur powder is easy to volatilize, and the sulfur powder is completely volatilized before the metal Pd membrane is raised to the set temperature due to too high temperature. In this example, the maximum limit temperature of the S powder was 400 ℃. Secondly, there is a certain requirement for the amount of sulfur powder, and since sulfur powder is very easy to volatilize, S powder must be present in excess, in this example, sulfur powder: the mass ratio of the metal Pd membrane is more than 10000.
This implementationIn one embodiment, the carrier gas is a hydrogen-containing carrier gas, the purpose of the hydrogen gas is to react with S 2 The molecular combination reaction generates a hydrogen sulfide intermediate with higher activity, the sulfuration efficiency is improved, the content of hydrogen is not easy to be too high, and a large amount of toxic H can be generated 2 S gas, which is found to contain H by adjusting the experiment for a plurality of times 2 The hydrogen in the carrier gas is 1sccm to meet the requirement. In addition, the content of Ar gas in the carrier gas also needs to be controlled, and too high content of Ar gas can cause S 2 The molecules are transported away directly in the high flow carrier gas without reaction, and S is also reduced 2 The vapor pressure of (a); too low recycle of Ar gas results in insufficient transport of S to the reaction zone 2 The molecular weight is not sufficient. In this example, it was found that the vulcanization effect was very poor when Ar was less than 10sccm and more than 50 sccm. The best effect is found by multiple times of optimization when the flow rate of Ar is 20sccm, and the best vulcanization effect is obtained at the moment.
In addition, as for the vulcanization time, the reaction in the embodiment is a solid-gas reaction, and the reaction rate is relatively slow, so that sufficient reaction time is required to complete the complete vulcanization process. Among them, too short a sulfidation time leads to insufficient sulfidation, and it was found in experiments that the sulfidation time is appropriately increased as the thickness of the metal Pd film is increased. According to multiple experimental experiences, the following results are obtained: the vulcanization time of the palladium film with the thickness of 1-10 nm needs to be 20-60 min, and the vulcanization time is approximately linear along with the thickness. As a supplementary note, the vulcanization time cannot be too long, and the film cannot be formed due to the graininess of the synthesized film under the action of surface tension. In this embodiment, the preferred vulcanization time is 40min.
The technical solution of the present invention will be described in more detail with reference to several examples.
The first embodiment is as follows:
the preparation process of the large-area palladium sulfide film provided by the first embodiment of the invention comprises the following steps:
step one, preparing a metal Pd film by using an electron beam evaporation instrument, then placing a magnetic boat of a substrate filled with the metal Pd film in a downstream constant temperature area of a double-temperature-area tube furnace, and placing the magnetic boat filled with sulfur powder in an upstream constant temperature area.
Step two, introducing hydrogen-containing carrier gas into the double-temperature-zone tubular furnace, controlling the temperature of an upstream constant-temperature zone to be higher than 200 ℃ so as to volatilize sulfur powder into sulfur steam, and controlling the temperature of a downstream constant-temperature zone to be 350 ℃ so as to vulcanize the metal Pd film, thereby finally obtaining a palladium-sulfur product PdS 3 。
Wherein the hydrogen-containing carrier gas comprises Ar and H 2 . The flow rate of Ar was 20sccm, H 2 The flow rate of (2) was 1sccm, and the vulcanization time was 40min. Palladium sulphur product PdS 3 The characteristic peaks of Raman scattering of (a) are shown in fig. 2.
The second embodiment:
the preparation process of the large-area palladium sulfide film provided by the second embodiment of the invention comprises the following steps:
step one, preparing a metal Pd film by using an electron beam evaporation instrument, then placing a magnetic boat of a substrate filled with the metal Pd film in a downstream constant temperature area of a double-temperature-area tube furnace, and placing the magnetic boat filled with sulfur powder in an upstream constant temperature area.
Step two, introducing hydrogen-containing carrier gas into the double-temperature-zone tubular furnace, controlling the temperature of an upstream constant-temperature zone to be higher than 200 ℃ so as to volatilize sulfur powder into sulfur steam, and controlling the temperature of a downstream constant-temperature zone to be 450 ℃ so as to vulcanize the metal Pd film, thereby finally obtaining a palladium-sulfur product PdS 2 。
Wherein the hydrogen-containing carrier gas comprises Ar and H 2 . The flow rate of Ar was 20sccm, H 2 The flow rate of (2) was 1sccm, and the vulcanization time was 40min. Palladium sulphur product PdS 2 The characteristic peaks of Raman scattering of (a) are shown in fig. 3.
Example three:
the preparation process of the large-area palladium sulfide film provided by the third embodiment of the invention comprises the following steps:
step one, preparing a metal Pd film by using an electron beam evaporation instrument, then placing a magnetic boat of a substrate filled with the metal Pd film in a downstream constant temperature area of a double-temperature-area tube furnace, and placing the magnetic boat filled with sulfur powder in an upstream constant temperature area.
Step two, introducing hydrogen-containing carrier gas into the double-temperature-zone tubular furnace, controlling the temperature of the upstream constant-temperature zone to be higher than 200 ℃ so as to volatilize sulfur powder into sulfur steam, and controlling the downstream constant-temperature zoneAt 550 ℃ to vulcanize the metal Pd membrane and finally obtain the Pd sulfur product PdS 2 。
Wherein the hydrogen-containing carrier gas comprises Ar and H 2 . The flow rate of Ar was 20sccm, H 2 The flow rate of (2) was 1sccm, and the vulcanization time was 40min. Palladium sulphur product PdS 2 Characteristic peaks of Raman scattering of (a) are shown in fig. 4.
Example four:
the preparation process of the large-area palladium sulfide film provided by the fourth embodiment of the invention comprises the following steps:
step one, preparing a metal Pd film by using an electron beam evaporation instrument, then placing a magnetic boat of a substrate filled with the metal Pd film in a downstream constant temperature area of a double-temperature-area tube furnace, and placing the magnetic boat filled with sulfur powder in an upstream constant temperature area.
And step two, introducing hydrogen-containing carrier gas into the double-temperature-zone tubular furnace, controlling the temperature of the upstream constant-temperature zone to be higher than 200 ℃ so as to volatilize sulfur powder into sulfur steam, and controlling the temperature of the downstream constant-temperature zone to be 650 ℃ so as to vulcanize the metal Pd film, thereby finally obtaining a palladium-sulfur product PdS.
Wherein the hydrogen-containing carrier gas comprises Ar and H 2 . The flow rate of Ar was 20sccm, H 2 The flow rate of (2) was 1sccm, and the vulcanization time was 40min. The characteristic peaks of Raman scattering of the palladium sulphur product PdS are shown in figure 5.
Example five:
the preparation process of the large-area palladium sulfide film provided by the fifth embodiment of the invention comprises the following steps:
step one, preparing a metal Pd film by using an electron beam evaporation instrument, then placing a magnetic boat of a substrate filled with the metal Pd film in a downstream constant temperature area of a double-temperature-area tube furnace, and placing the magnetic boat filled with sulfur powder in an upstream constant temperature area.
And step two, introducing hydrogen-containing carrier gas into the double-temperature-zone tubular furnace, controlling the temperature of the upstream constant-temperature zone to be higher than 200 ℃ so as to volatilize sulfur powder into sulfur steam, and controlling the temperature of the downstream constant-temperature zone to be 750 ℃ so as to vulcanize the metal Pd film, thereby finally obtaining a palladium-sulfur product PdS.
Wherein the hydrogen-containing carrier gas comprises Ar and H 2 . Flow rate of Ar of20sccm，H 2 The flow rate of (2) was 1sccm, and the vulcanization time was 40min. The characteristic peaks of Raman scattering of the palladium sulphur product PdS are shown in figure 6.
The invention also provides a large-area palladium sulfide film, wherein the large-area palladium sulfide film is prepared by applying the preparation process of the large-area palladium sulfide film, and the large-area palladium sulfide film comprises PdS and PdS 2 And PdS 3 。
The invention also provides application of the large-area palladium sulfide film, wherein the large-area palladium sulfide film is prepared by the preparation process of the large-area palladium sulfide film, and PdS is prepared by the large-area palladium sulfide film 2 A MOS transistor.
Wherein, the semiconductor characteristic PdS is generated by the sulfurization reaction at 450-550 DEG C 2 Film, and the carrier mobility is measured to reach 10.4cm 2 V -1 s -1 The material has good carrier mobility, and is expected to be applied to a semiconductor process (as shown in FIG. 7). Theoretical study of PdS at two-dimensional limits 2 Is a narrow bandgap semiconductor, so the synthesized PdS 2 The film can also be used in the field of infrared detectors.
The invention provides a large-area palladium sulfide film, a preparation process and application thereof, the prepared palladium sulfide film has larger area, and a plurality of substrates of selectable metal Pd films, including silicon wafers, sapphires, metals and the like, are expected to be applied to the fields of catalysis, electronic devices, photoelectricity and the like. The preparation process of the invention has no complicated operation steps, simple equipment, simple and easy operation and good reproducibility.
Finally, it should be noted that: the above-mentioned embodiments are only specific embodiments of the present invention, which are used for illustrating the technical solutions of the present invention and not for limiting the same, and the protection scope of the present invention is not limited thereto, although the present invention is described in detail with reference to the foregoing embodiments, those skilled in the art should understand that: any person skilled in the art can modify or easily conceive the technical solutions described in the foregoing embodiments or equivalent substitutes for some technical features within the technical scope of the present disclosure; such modifications, changes or substitutions do not depart from the spirit and scope of the embodiments of the present invention, and they should be construed as being included therein. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. The preparation process of the large-area palladium sulfide film is characterized by being realized by applying a double-temperature-area tube furnace, wherein an upstream constant-temperature area and a downstream constant-temperature area are arranged in the double-temperature-area tube furnace, the upstream constant-temperature area and the downstream constant-temperature area are respectively provided with a heating device, a magnetic boat filled with sulfur powder is placed in the upstream constant-temperature area, the magnetic boat filled with a substrate of a metal Pd film is placed in the downstream constant-temperature area, and the preparation process comprises the following steps:
preparing a metal Pd film by using an electron beam evaporation instrument, then placing a magnetic boat of a substrate filled with the metal Pd film in a downstream constant temperature area of a double-temperature-area tube furnace, and placing the magnetic boat filled with sulfur powder in an upstream constant temperature area;
and (3) introducing hydrogen-containing carrier gas into the double-temperature-zone tubular furnace, controlling the temperature of the upstream constant-temperature zone to be higher than 200 ℃ so as to volatilize sulfur powder into sulfur steam, and controlling the temperature range of the downstream constant-temperature zone to be 350-750 ℃ so as to vulcanize the metal Pd film, thereby finally obtaining a palladium-sulfur product.
2. The process of claim 1, wherein the hydrogen-containing carrier gas comprises Ar and H 2 Ar flow rate of 20sccm, H 2 The flow rate of (2) is 1sccm.
3. The process of claim 2, wherein the step of sulfidizing the Pd membrane is performed for a corresponding sulfidizing time of 40min.
4. The process according to claim 3, wherein in the step of preparing the Pd film by electron beam evaporation, the Pd is in bulk and has a particle size of 2.5mm, and the thickness of the Pd film is controlled within 10 nm.
5. The process according to claim 4, wherein the mass ratio of the added sulfur powder to the metal Pd film in the dual-temperature-zone tube furnace is greater than 10000.
6. The process for preparing a large-area palladium sulfide thin film according to claim 5, wherein the sulfidation time required for preparing a 1-10 nm palladium sulfide thin film is 20-60 min.
7. The process according to claim 6, wherein in the step of sulfidizing the metal Pd membrane, when the sulfidizing temperature of the metal Pd membrane is 350 ℃, the corresponding product is PdS 3 (ii) a When the sulfurization temperature of the metal Pd membrane is 450 ℃, the corresponding product is PdS 2 (ii) a When the vulcanization temperature of the metal Pd membrane is 550 ℃, the corresponding product is PdS 2 。
8. The process according to claim 6, wherein in the step of sulfidizing the metal Pd membrane, when the sulfidizing temperature of the metal Pd membrane is 650 ℃, the corresponding product is PdS; when the sulfidation temperature of the metal Pd film is 750 ℃, the corresponding product is PdS.
9. A large-area palladium sulfide thin film, which is prepared by the preparation process of the large-area palladium sulfide thin film as claimed in any one of claims 1 to 8, wherein the large-area palladium sulfide thin film comprises PdS and PdS 2 And PdS 3 。
10. Use of a large-area palladium sulfide film, wherein the large area is characterized in thatThe palladium sulfide film is prepared by the preparation process of the large-area palladium sulfide film as claimed in any one of claims 1 to 8, and PdS is prepared by the preparation process of the large-area palladium sulfide film 2 A MOS transistor.
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