Method for manufacturing chalcogenide-based compound thin film

Abstract

The present invention relates to a method for manufacturing a chalcogenide-based compound thin film. According to an embodiment of the present invention, provided is a method for manufacturing a chalcogenide-based compound thin film, the method comprising: a deposition step of obtaining a chalcogenide-based compound thin film having a preset composition by simultaneously depositing an electropositive material and a chalcogen material on a deposition substrate through a simultaneous deposition process using a simultaneous deposition device.

Description

Method for manufacturing a thin film of a chalcogenide compound

[0001] The present invention relates to a method for manufacturing a chalcogenide compound thin film.

[0002] "The present invention is derived from research conducted as part of the Ministry of Science and ICT's individual basic research (Project unique number: 1711194081, Subproject number: 00208311, Research project name: Research on building a band structure control system for one-dimensional linear structure transition metal-chalcogenide M2N3X8 series compound semiconductor materials, Host organization: Ajou University Industry-Academic Cooperation Foundation, Research period: 2023.03.01 ~ 2024.02.29)."

[0003] A chalcogenide is a compound composed of at least one chalcogen ion (an element from group 16 (VIA) of the periodic table, such as sulfur (S), selenium (Se), and tellurium (Te)) and at least one electropositive element.

[0004] Chalcogenide compounds, which are composed of compounds of binary or higher systems, are known to have various properties that can easily change from crystalline to amorphous, semiconductor to metallic, ionic to electronic conductors, etc., by external electrical stimulation, heat, and light energy stimulation. Due to these material characteristics with various properties, they are widely used as thin film materials for information storage / processing, thin film materials for solar cells, thin film materials for ionic conductors, and thin film materials for information recognition / display.

[0005] Known methods used to synthesize chalcogenide compound thin films include Chemical Vapor Deposition (CVD), Chemical Vapor Transport (CVT), and Molecular Beam Epitaxy (MBE).

[0006] However, the above-mentioned synthetic methods are difficult to apply industrially due to difficult process conditions and contact resistance problems.

[0007] Specifically, in the case of CVD and CVT, high energy is required for the evaporation of positive elements, so it is a high-temperature synthesis process. If the synthesis temperature is lowered through organic precursors, catalysts, etc., the quality deteriorates due to the mixing of impurities, and there is a limitation that large-area growth is difficult.

[0008] In addition, in the case of MBE, an ultra-high vacuum must be maintained, and a raw material supply device such as a Knudsen cell must be used for each material, resulting in high equipment costs and limitations such as a low growth rate.

[0009] Accordingly, for the industrialization of calogenide compounds, research on a manufacturing method that can achieve large-scale growth at low cost, rapid growth rate, and excellent quality is essential.

[0010] A method for manufacturing a chalcogenide compound thin film according to an embodiment of the present invention is proposed to solve the above problems, and ensures compatibility by using equipment used in existing semiconductor processes, enables large-area synthesis, and enables synthesis even at low temperatures (below 250°C), thereby minimizing the impact of low heat costs and thermal limitations between semiconductor processes.

[0011] In addition, since only the substances that make up the composition of the compound are used in a high vacuum, high-purity, high-quality thin film synthesis is possible, and by easily changing the types of positive elements and chalcogen elements, various combinations of chalcogenide compound thin films can be easily synthesized.

[0012] According to one embodiment, a method for manufacturing a chalcogenide-based compound thin film using a simultaneous deposition device including a deposition chamber that maintains a preset vacuum level; a deposition rotation unit provided with a deposition substrate and disposed within the deposition chamber; an E-beam evaporation unit that is disposed within the deposition chamber and evaporates a positively charged material as a raw material; a thermal evaporation unit that is disposed within the deposition chamber and evaporates a chalcogen material as a raw material; and a deposition sensor that senses the deposition amount and deposition speed of the positively charged material and the chalcogen material deposited on the deposition substrate; a method for manufacturing a chalcogenide-based compound thin film can be provided, the method including a deposition step of simultaneously depositing the positively charged material and the chalcogen material on the deposition substrate through a simultaneous deposition process using the simultaneous deposition device to obtain a chalcogenide-based compound thin film having a preset composition.

[0013] In addition, in the deposition step, a method for manufacturing a chalcogenide compound thin film can be provided, wherein the positive material is at least one material selected from the group consisting of Ti, Ni, Cu, Ge, Mo, Sn, Sb, and Bi, the chalcogen material is at least one material selected from the group consisting of S, Se, and Te, and the positive material and the chalcogen material are single-element materials composed of only one type of element.

[0014] In addition, the above deposition step is performed within the deposition chamber, and the vacuum level within the deposition chamber is 10 -6 ~ 10 -5 A method for manufacturing a chalcogenide compound thin film satisfying a range of Torr can be provided.

[0015] In addition, a method for manufacturing a chalcogenide compound thin film can be provided, in which, in the deposition step, the chalcogenide compound thin film is deposited so as to satisfy a deposition rate range of 0.3 to 60 nm / min.

[0016] In addition, in the deposition step, a method for manufacturing a chalcogenide compound thin film can be provided in which the composition of the chalcogenide compound thin film is selectively controlled by controlling the deposition rate ratio of the positive material and the chalcogen material, and the deposition rate of the positive material and the chalcogen material satisfies a range of 0.05 to 10 Å / s.

[0017] In addition, a method for manufacturing a chalcogenide compound thin film can be provided, in which the deposition rate ratio of the positive material and the chalcogen material is 1 to 7:1 to 4.

[0018] In addition, a method for manufacturing a chalcogenide compound thin film can be provided, wherein the deposition step further includes a re-evaporation step of re-evaporating residual raw material by performing a deposition substrate heating process of heating the deposition substrate to satisfy a heating temperature range of 20 to 200°C.

[0019] In addition, the deposition step further includes, before the re-evaporation step, a step of deriving a heating temperature range for performing the deposition substrate heating process; wherein the step of deriving the heating temperature range includes: a step of obtaining a deposition rate value of a chalcogen material deposited on the deposition substrate through the deposition sensor; a step of obtaining a re-evaporation rate value of a chalcogen material re-evaporated on the deposition substrate by considering an adhesion coefficient of the deposition substrate, a vapor pressure of the chalcogen material, a vacuum level of the deposition chamber, and a heating temperature of the deposition substrate; and a step of deriving a heating temperature range of the deposition substrate such that the obtained re-evaporation rate value of the chalcogen material is greater than the obtained deposition rate value of the chalcogen material.

[0020] In addition, in the deposition step, the chalcogenide compound thin film includes at least one material selected from the group consisting of MoS2, NiS, Ni3S4, NiS2, SnS2, SnS, Ti2S, TiS, TiS2, TiS3, Cu2S, CuS, GeS, GeS2, Bi2S3, Sb2S3, MoSe2, NiSe, Ni3Se4, NiSe2, SnSe, SnSe2, TiSe2, Cu3Se2, CuSe, CuSe2, GeSe, GeSe2, Bi2Se, Bi4Se3, BiSe, Bi2Se3, Sb2Se3, MoTe2, Ni3Te2, NiTe, NiTe2, SnTe, Ti5Te4, TiTe, Ti3Te4, TiTe2, Cu7Te4, Cu2Te, CuTe, CuTe2, GeTe, Bi7Te3, Bi2Te, Bi4Te3, BiTe, Bi2Te3 and Sb2Te3. A method for manufacturing a chalcogenide compound thin film can be provided.

[0021] In addition, a method for manufacturing a chalcogenide compound thin film can be provided, wherein, in the deposition step, the chalcogenide compound thin film is formed as a single layer or multiple layers.

[0022] The method for manufacturing a chalcogenide compound thin film according to one embodiment of the present invention secures compatibility by using equipment used in existing semiconductor processes, enables large-area synthesis, and enables synthesis even at low temperatures (250°C or lower), thereby having the effect of minimizing the influence of low heat costs and thermal limitations between semiconductor processes.

[0023] In addition, since only the substances that make up the composition of the compound are used in a high vacuum, high-purity, high-quality thin film synthesis is possible, and by easily changing the types of positive elements and chalcogen elements, it is possible to easily synthesize chalcogenide compound thin films of various combinations.

[0024] FIG. 1 is a drawing for explaining a simultaneous deposition device according to one embodiment of the present invention.

[0025] Figure 2 is a flow chart for explaining a method for manufacturing a chalcogenide compound thin film according to one embodiment of the present invention.

[0026] FIG. 3 is a drawing for briefly explaining a chalcogenide compound thin film according to one embodiment of the present invention.

[0027] Figure 4 shows the results of evaluating the characteristics of a chalcogenide compound thin film according to Example 1 of the present invention.

[0028] Figure 5 shows the results of evaluating the characteristics of a chalcogenide compound thin film according to Example 2 of the present invention.

[0029] Figure 6 shows the results of evaluating the characteristics of a chalcogenide compound thin film according to Example 3 of the present invention.

[0030] Figure 7 shows the results of evaluating the characteristics of a chalcogenide compound thin film according to Example 4 of the present invention.

[0031] Figure 8 shows the results of evaluating the characteristics of a chalcogenide compound thin film according to Example 5 of the present invention.

[0032] Figure 9 shows the results of evaluating the characteristics of a chalcogenide compound thin film according to Example 6 of the present invention.

[0033] Figure 10 shows the results of evaluating the characteristics of a chalcogenide compound thin film according to Example 7 of the present invention.

[0034] Figure 11 shows the results of evaluating the characteristics of a chalcogenide compound thin film according to Example 8 of the present invention.

[0035] In order to fully understand the configuration and effect of the present invention, a preferred embodiment of the present invention will be described in detail with reference to the attached drawings.

[0036] The present invention is not limited to the embodiments disclosed below, but can be implemented in various forms and subject to various modifications and changes. However, the description of these embodiments is provided to ensure that the disclosure of the present invention is complete and to fully inform those skilled in the art of the present invention of the scope of the invention. In the attached drawings, components are illustrated in enlarged size for convenience of explanation, and the proportions of each component may be exaggerated or reduced.

[0037] The terminology used herein is for the purpose of describing embodiments and is not intended to limit the present invention. In addition, the terms used herein can be interpreted as having the meaning commonly known to those of ordinary skill in the art, unless otherwise defined. In this specification, the singular also includes the plural unless specifically stated in the phrase. As used herein, the words "comprises" and / or "comprising" do not exclude the presence or addition of one or more other components, steps, operations, and / or elements mentioned.

[0038] When a layer is referred to herein as being "on" another layer, it may be formed directly on the surface of the other layer, or a third layer may be interposed therebetween. Although terms such as first, second, etc. are used herein to describe various regions, layers, etc., these regions and layers should not be limited by such terms. These terms are used merely to distinguish a given region or layer from another region or layer. Thus, a part referred to as a first part in one embodiment may be referred to as a second part in another embodiment. The embodiments described and illustrated herein also include complementary embodiments thereof. Parts denoted by the same reference numerals throughout the specification represent like elements.

[0039] The present invention provides a method for synthesizing a low-cost, high-quality, and large-area chalcogenide compound thin film by utilizing an e-beam evaporator and a thermal evaporator used in a semiconductor process.

[0040] Specifically, the present invention is designed to simultaneously deposit a positive material and a chalcogen material, while controlling the deposition rate ratio between each material, thereby obtaining a chalcogenide compound thin film having various compositions.

[0041] In addition, the present invention is designed to obtain a high-quality chalcogenide compound thin film by effectively removing residual raw materials by controlling the temperature of the deposition substrate.

[0042]

[0043] <Method for manufacturing chalcogenide compound thin films>

[0044] FIG. 1 is a drawing for explaining a simultaneous deposition device according to one embodiment of the present invention, and FIG. 2 is a flowchart for explaining a method for manufacturing a chalcogenide compound thin film according to one embodiment of the present invention.

[0045] Referring to FIGS. 1 and 2, a method for manufacturing a chalcogenide compound thin film according to an embodiment of the present invention (S10) may utilize a simultaneous deposition device (10) including a deposition chamber (100) that maintains a preset vacuum level; a deposition rotation unit (200) provided with a deposition substrate (210) and disposed within the deposition chamber (100); an E-beam evaporation unit (300) that is disposed within the deposition chamber (100) and evaporates a positively charged material as a raw material; a thermal evaporation unit (400) that is disposed within the deposition chamber (100) and evaporates a chalcogen material as a raw material; and a deposition sensor (not shown) that senses the deposition amount and deposition speed of the positively charged material and the chalcogen material deposited on the deposition substrate (210).

[0046] In addition, a method for manufacturing a chalcogenide compound thin film according to one embodiment of the present invention (S10) includes a deposition step (S100) of simultaneously depositing a positive material and a chalcogen material on the deposition substrate (210) through a simultaneous deposition process utilizing the simultaneous deposition device (10) to obtain a chalcogenide compound thin film having a preset composition.

[0047] First, referring to FIG. 1, the simultaneous deposition device (10) may be a device that independently and simultaneously evaporates a positive element and a chalcogen element (S, Se, Te) by utilizing an E-beam and a thermal evaporator, respectively, inside a chamber maintained at high vacuum, so that they are synthesized on a heated substrate.

[0048] That is, the simultaneous deposition device (10) may be a device for synthesizing a chalcogenide, which is a compound composed of at least one group 16 (chalcogen) element and one or more positive elements.

[0049] Specifically, only pure positively charged substances and chalcogen substances are used in a high vacuum environment, and each raw material can be stored within a high vacuum chamber, thereby preventing oxidation and adsorption, enabling the synthesis of high-purity chalcogenide compounds.

[0050] In addition, since the vapor pressure of chalcogenide is high at about 1 mTorr at 200°C, the substrate temperature can be increased to effectively prevent the residue of chalcogen material that did not participate in the synthesis.

[0051] In addition, since the E-beam and thermal sources can be controlled independently, the deposition rate of the positive material and chalcogen material can be controlled during synthesis, and the temperature of the substrate can be controlled to easily synthesize high-quality thin films with various composition ratios on the phase diagram.

[0052] Furthermore, by arranging multiple positively charged materials inside the e-bema, it is possible to synthesize heterogeneous chalcogenide compounds in situ within the process or to synthesize multiple layers of chalcogenide compound thin films with different composition ratios, making it versatile and highly expandable.

[0053] Meanwhile, the deposition substrate (210) may be any one substrate selected from among a p-Si substrate, an Al2O3 substrate, a Si / SiO2 substrate, and a SiO2 substrate, but is not limited thereto.

[0054] Next, referring to FIG. 2, the method for manufacturing the chalcogenide compound thin film (S10) can be performed through a simultaneous deposition process using the simultaneous deposition device (10) described above.

[0055] The above simultaneous deposition process may be a process for synthesizing a chalcogenide compound thin film having various composition ratios by utilizing an evaporation source placed inside a chamber to evaporate a positive material and a chalcogen material, maintaining a high vacuum inside the chamber, heating the substrate to a temperature required for compound formation, and controlling the deposition rate ratio of the positive material and the chalcogen material.

[0056] Specifically, in the deposition step (S100), the positive material may be at least one material selected from the group consisting of Ti, Ni, Cu, Ge, Mo, Sn, Sb, and Bi, and the chalcogen material may be at least one material selected from the group consisting of S, Se, and Te.

[0057] In addition, in the deposition step (S100), the positive material and the chalcogen material are simple element materials composed of only one type of element.

[0058] In a method (S10) for manufacturing a chalcogenide compound thin film according to one embodiment of the present invention, unlike conventional deposition equipment, a simultaneous deposition device (10) is utilized, thereby overcoming the limitation of having to use a metal compound as a metal precursor to evaporate a positive material having a high evaporation temperature, and having the advantage of being able to use a pure positive material as a metal precursor.

[0059] In addition, the deposition step (S100) is performed within the deposition chamber (100), and the vacuum level within the deposition chamber (100) is 10 -6 ~ 10 -5 It can satisfy the range of Torr.

[0060] Specifically, in the above deposition step (S100), the deposition chamber part (100) is 10 -6 ~ 10 -5 Maintaining a vacuum level that satisfies the range of Torr, this vacuum level range can lower the temperature at which the chalcogenide material can exist in the gas phase.

[0061] More specifically, the vacuum level in the deposition chamber (100) is 10 -6 If it is lower than Torr, the problem arises that the cost for maintaining vacuum increases rapidly, and the vacuum level in the deposition chamber (100) is 10 -5 Above Torr, the temperature range in which the chalcogenide can remain in a gaseous state may become too high, which may cause problems.

[0062] In addition, in the deposition step (S100), the chalcogenide compound thin film can be deposited so as to satisfy a deposition rate range of 0.3 to 60 nm / min, and in a preferred embodiment of the present invention, the deposition rate of the chalcogenide compound thin film is 0.3 to 30 nm / min.

[0063] If the deposition rate of the above chalcogenide compound thin film is lower than 0.3 nm / min, the productivity decreases rapidly, and if the deposition rate is higher than 60 nm / min, there is a problem in that it is difficult to obtain a large-area thin film of excellent quality.

[0064] In addition, in the deposition step (S100), the composition of the chalcogenide compound thin film can be selectively controlled by adjusting the deposition rate ratio of the positive material and the chalcogen material.

[0065] That is, when the composition ratio of the chalcogenide compound changes depending on the process requirements, various process requirements can be responded to by simply changing the deposition rate ratio of the positive material and the chalcogen material without the need to add separate process conditions.

[0066] Furthermore, by changing the types of positive and negative substances, chalcogenide compounds with various composition ratios can be easily synthesized.

[0067] Specifically, in the deposition step (S100), the deposition speed of the positive material and the chalcogen material can satisfy a range of 0.05 to 10 Å / s, and in a preferred embodiment of the present invention, the deposition speed of the positive material and the chalcogen material satisfies a range of 0.05 to 5 Å / s.

[0068] More specifically, the deposition rate ratio of the positive material and the chalcogen material may be 1 to 7:1 to 4.

[0069] In a method (S10) for manufacturing a chalcogenide compound thin film according to one embodiment of the present invention, the deposition step (S100) may further include a re-evaporation step (S110) of performing a deposition substrate heating process for heating the deposition substrate (210) to satisfy a heating temperature range of 20 to 200°C to re-evaporate residual raw materials.

[0070] Specifically, the above re-evaporation step (S110) is performed to prevent surface adsorption of raw materials, and is a step to suppress residual raw materials that do not participate in the synthesis reaction by preventing surface adsorption.

[0071] In the method for manufacturing a chalcogenide compound thin film according to one embodiment of the present invention (S10), the reaction mechanism of the raw material including the positive material and the chalcogen material can be explained by the Eley-Rideal Reaction.

[0072] Specifically, the Eley-Rideal Reaction is the adsorption rate (J) of the raw material chalcogenide. Abs ) is less than 0, and more specifically, it can occur when the re-evaporation rate of the chalcogen substance is greater than the deposition rate of the chalcogen substance.

[0073] Here, the adsorption rate of the chalcogen substance (J Abs ) is the deposition rate of the chalcogenide material (J Inc ) value of the re-evaporation rate of the chalcogenide (J T Vap ) is the value minus the value.

[0074] Through this Eley-Rideal Reaction, residual chalcogen material is prevented from being adsorbed on the substrate surface, and adsorption of the product after the gas phase reaction occurs, thereby obtaining a chalcogenide compound thin film with excellent composition ratio and surface homogeneity.

[0075] Furthermore, by deriving a heating temperature range of the substrate to induce an Eley-Rideal Reaction and setting the deposition substrate (210) to be heated within the derived heating temperature range, a gas phase reaction of the chalcogen material can be induced to obtain a high-quality thin film.

[0076] In a method (S10) for manufacturing a chalcogenide compound thin film according to one embodiment of the present invention, the deposition step (S100) may further include a step (S120) of deriving a heating temperature range for performing the deposition substrate heating process prior to the re-evaporation step (S110).

[0077] The step (S120) of deriving the above heating temperature range may be a step of deriving the heating temperature range of the deposition substrate (210) so that the re-evaporation rate value of the chalcogenide material is greater than the deposition rate value of the chalcogenide material, in order to obtain a chalcogenide compound thin film having a specific composition ratio according to process requirements, as described above.

[0078] That is, the step (S120) of deriving the above heating temperature range is the adsorption rate (J) of the raw material, the chalcogen substance. Abs ) may be a step of deriving a heating temperature range of the deposition substrate (210) so that the temperature is less than 0.

[0079] More specifically, the step (S120) of deriving the heating temperature range is to determine the deposition rate value (J) of the chalcogen material deposited on the deposition substrate (210) through the deposition sensor. Inc ) obtaining step (S211), adhesion coefficient (α) of the deposition substrate (210), vapor pressure (P) of the chalcogen material T Vap ), the vacuum level (P) of the above deposition chamber (100) Cham ) and the heating temperature (T) of the deposition substrate (210), the re-evaporation rate value (J) of the chalcogen material re-evaporated on the deposition substrate (210) T Vap) may include a step (S212) of obtaining a chalcogenide material, and a step (S213) of deriving a range of a heating temperature (T) of the deposition substrate (210) so that the re-evaporation rate value of the obtained chalcogenide material is greater than the deposition rate value of the obtained chalcogenide material.

[0080] The adsorption rate of the raw material, chalcogenide, can be expressed by the following mathematical formula 1.

[0081] [Mathematical Formula 1]

[0082] J Abs =J Inc -J T Vap

[0083] (J Abs : Adsorption rate of the substance, J Inc : Deposition rate of material, J T Vap : re-evaporation rate of the substance)

[0084]

[0085] At this time, J T Vap can be expressed as a function of the adhesion coefficient of the deposition substrate, the vapor pressure of the material, the chamber pressure, and the temperature, and can be expressed by the following mathematical expression 2.

[0086] [Equation 2]

[0087]

[0088] (N: Number of gas molecules, A: Surface Area [m 2 ], α: Sticking coefficient(0≤α≤1), N A : Avogadro constant[mol -1 ], P Cham : Chamber Pressure[Pa], P T Vap : Vapor pressure of element at (T) K[Pa], M: Molar mass[kg mol -1 ], T: Temperature[K])

[0089]

[0090] Adsorption rate of chalcogenide (J Abs ) is greater than 0, the chalcogen substance is adsorbed on the substrate surface, and the adsorption rate of the chalcogen substance (J Abs ) is less than 0, the chalcogen substance is not adsorbed on the substrate surface and exists in a gaseous state. That is, when the adhesion coefficient of the deposition substrate, the vapor pressure of the chalcogen substance, and the chamber pressure are determined, the adsorption rate (J) of the chalcogen substance is controlled by adjusting the heating temperature of the deposition substrate (210). Abs ) can control the size and sign.

[0091] In other words, the step (S120) of deriving the above heating temperature range is the adsorption rate (J) of the chalcogen substance. Abs ) may be a step of finding a heating temperature range of the deposition substrate (210) so that it is less than 0.

[0092] In a method for manufacturing a chalcogenide compound thin film according to another embodiment of the present invention (S10), the re-evaporation step (S110) may be a step of re-evaporating residual raw material by performing a deposition substrate heating process that heats the deposition substrate (210) to satisfy a heating temperature range of 200 to 500°C.

[0093] In a method for manufacturing a chalcogenide compound thin film according to another embodiment of the present invention (S10), the reaction mechanism of the raw material including the positive material and the chalcogen material can be explained as a gas-phase reaction.

[0094] Specifically, the gas-phase reaction is the adsorption rate (J) of the raw materials, positive substances and chalcogen substances. Abs ) is a reaction that occurs when all are less than 0.

[0095] Through this gas-phase reaction, residual raw materials are prevented from being adsorbed on the substrate surface, and adsorption of the product after the gas-phase reaction occurs, thereby obtaining a chalcogenide compound thin film with excellent composition ratio and surface homogeneity.

[0096] Looking at the heating temperature range of the substrate for inducing a gas-phase reaction, the range for a positive material is 200 to 500°C, and the range for a chalcogen material is 20 to 200°C. Therefore, by setting the heating temperature range based on the positive material, both the positive material and the chalcogen material can induce a gas-phase reaction, thereby obtaining a high-quality thin film.

[0097] In addition, in the method (S10) for manufacturing a chalcogenide compound thin film according to another embodiment of the present invention, the step (S120) of deriving the heating temperature range may be a step of deriving the heating temperature range of the deposition substrate (210) so that the re-evaporation rate value of the positive material is greater than the deposition rate value of the positive material in order to obtain a chalcogenide compound thin film having a specific composition ratio according to process requirements.

[0098] That is, the step (S120) of deriving the above heating temperature range is the adsorption rate (J) of the positive substance. Abs ) may be a step of deriving a heating temperature range of the deposition substrate (210) so that the temperature is less than 0.

[0099] More specifically, the step (S120) of deriving the heating temperature range is to obtain the deposition rate value (J) of the positive material deposited on the deposition substrate (210) through the deposition sensor. Inc ) and the adhesion coefficient (α) of the deposition substrate (210), the vapor pressure (P) of the positive material T Vap ), the vacuum level (P) of the above deposition chamber (100) Cham ) and the heating temperature (T) of the deposition substrate (210), the re-evaporation rate value (J) of the positive material re-evaporated on the deposition substrate (210) T Vap ) and a step of deriving a heating temperature (T) range of the deposition substrate (210) so that the re-evaporation rate value of the obtained positive material is greater than the deposition rate value of the obtained positive material.

[0100] Adsorption rate of positive substances (J Abs ) is greater than 0, the positive material is adsorbed on the substrate surface, and the adsorption rate of the positive material (J Abs ) is less than 0, the positive material is not adsorbed on the substrate surface and exists in a gaseous state. That is, when the adhesion coefficient of the deposition substrate, the vapor pressure of the positive material, and the chamber pressure are determined, the adsorption rate (J) of the positive material is controlled by adjusting the heating temperature of the deposition substrate (210). Abs ) can control the size and sign.

[0101] In other words, the step (S120) of deriving the above heating temperature range is the adsorption rate (J) of the positive substance. Abs ) may be a step of finding a heating temperature range of the deposition substrate (210) so that it is less than 0.

[0102] In addition, in the deposition step (S100), the chalcogenide compound thin film may include at least one material selected from a saturated composition chalcogenide compound and a non-saturated composition chalcogenide compound.

[0103] Specifically, the chalcogenide compound thin film may include at least one material selected from the group consisting of MoS2, NiS, Ni3S4, NiS2, SnS2, SnS, Ti2S, TiS, TiS2, TiS3, Cu2S, CuS, GeS, GeS2, Bi2S3, Sb2S3, MoSe2, NiSe, Ni3Se4, NiSe2, SnSe, SnSe2, TiSe2, Cu3Se2, CuSe, CuSe2, GeSe, GeSe2, Bi2Se, Bi4Se3, BiSe, Bi2Se3, Sb2Se3, MoTe2, Ni3Te2, NiTe, NiTe2, SnTe, Ti5Te4, TiTe, Ti3Te4, TiTe2, Cu7Te4, Cu2Te, CuTe, CuTe2, GeTe, Bi7Te3, Bi2Te, Bi4Te3, BiTe, Bi2Te3, and Sb2Te3.

[0104] In addition, in the deposition step (S100), the chalcogenide compound thin film may be formed as a single layer or multiple layers.

[0105] Specifically, in the method (S10) for manufacturing a chalcogenide compound thin film according to one embodiment of the present invention, the deposition step (S100) may be repeated multiple times, and for example, a different raw material may be used each time the deposition step (S100) is repeated multiple times, that is, the simultaneous deposition process may be repeated while changing the raw material.

[0106] Accordingly, through the present invention, two or more chalcogenide compound thin films having different compositions can be laminated, i.e., a chalcogenide compound thin film composed of multiple layers can be obtained.

[0107] FIG. 3 is a drawing for briefly explaining a chalcogenide compound thin film according to one embodiment of the present invention.

[0108] Figure 3a) is a drawing showing a 3D schematic diagram of TMDC, and Figure 3b) is a diagram showing the composition ratio that can be formed through a combination of each element in the periodic table showing positive elements and chalcogen elements.

[0109] Referring to FIG. 3a), the chalcogenide compound thin film of the present invention may include TMDC, and the TMDC is a material formed through the bonding of a transition metal atom (M) and a chalcogen atom (X), and may have various physical properties such as a semimetal and a semiconductor depending on the combination of the transition metal and the chalcogen.

[0110] Most TMDCs have a two-dimensional layered structure, and the bonds between each layer are maintained through weak van der Waals bonds. This weak bonding energy allows them to be easily separated into two-dimensional sheets, and the band gap can be easily controlled by varying the number of layers.

[0111] In particular, semiconductor TMDCs such as MoS2 and WSe2 have higher carrier mobility than conventional silicon and have a thin thickness of several nm, so research into next-generation semiconductor devices is actively being conducted.

[0112] Referring to Fig. 3b), it can be confirmed that the formation of chalcogen compounds with various combinations and composition ratios is possible. Specifically, it is shown that various combinations between the chalcogen element indicated with an orange background and the positive element with a blue background can be formed, and depending on the type of positive element, the chalcogen compounds that can be formed are indicated above each positive element with a 1:1 composition in light blue, a 1:2 composition in red, and a 2:3 composition in blue, confirming that the synthesis of various compositions is possible.

[0113]

[0114] Hereinafter, the present invention will be described in more detail through drawings and examples, but the present invention is not limited thereto.

[0115]

[0116] Example 1: Preparation of a chalcogenide compound thin film (TiSe2) 1

[0117] A simultaneous deposition device including a deposition chamber, a deposition rotation unit equipped with a deposition substrate, an E-beam evaporation unit, a thermal evaporation unit, and a deposition sensor was prepared.

[0118] Afterwards, the vacuum level inside the deposition chamber was 10 -6 The pressure was maintained at 10 Torr, the heating temperature of the deposition substrate was maintained at 500°C, and the e-beam evaporator and the thermal evaporator were operated to evaporate Ti, a positive material, and Se, a chalcogen material, and the deposition rate ratio of Ti and Se was set to 1:2.

[0119] Here, the deposition substrate is a 4-inch silicon (Si) substrate.

[0120] In addition, the deposition rate of the thin film was set to 3.4 nm / min, and the deposition was performed for 7 minutes and 30 seconds to obtain a chalcogenide compound thin film having a TiSe2 composition (Example 1).

[0121]

[0122] Example 2: Preparation of a chalcogenide compound thin film (NiSe2) 2

[0123] A simultaneous deposition device including a deposition chamber, a deposition rotation unit equipped with a deposition substrate, an E-beam evaporation unit, a thermal evaporation unit, and a deposition sensor was prepared.

[0124] Afterwards, the vacuum level inside the deposition chamber was 10 -6 The pressure was maintained at 10 Torr, the heating temperature of the deposition substrate was maintained at 200°C, and the e-beam evaporator and the thermal evaporator were operated to evaporate Ni, a positive material, and Se, a chalcogen material, and the deposition rate ratio of Ni and Se was set to 1:2.

[0125] Here, the deposition substrate is a 4-inch silicon (Si) / silicon oxide (SiO2) substrate.

[0126] In addition, the deposition rate of the thin film was set to 1.75 nm / min, and the deposition was performed for 23 minutes to obtain a chalcogenide compound thin film having a NiSe2 composition (Example 2).

[0127]

[0128] Example 3: Preparation of a chalcogenide compound thin film (Bi2Se3) 3

[0129] A simultaneous deposition device including a deposition chamber, a deposition rotation unit equipped with a deposition substrate, an E-beam evaporation unit, a thermal evaporation unit, and a deposition sensor was prepared.

[0130] Afterwards, the vacuum level inside the deposition chamber was 10 -6The temperature was maintained at 1 Torr, the heating temperature of the deposition substrate was maintained at 15°C, 100°C, or 200°C, and the e-beam evaporator and the thermal evaporator were operated to evaporate Bi, a positive material, and Se, a chalcogen material, and the deposition rate ratio of Bi and Se was set to 2:3.

[0131] Here, the deposition substrate is an aluminum oxide (Al2O3) substrate or a silicon (Si) / silicon oxide (SiO2) substrate.

[0132] In addition, a chalcogenide compound thin film having a Bi2Se3 composition was obtained by depositing for 7 minutes so that the deposition rate of the thin film satisfies 4.7 nm / min (Example 3).

[0133] Here, the thin film obtained by using an Al2O3 substrate and maintaining the heating temperature of the deposition substrate at 15°C is sample A of Example 3, the thin film obtained by using an Al2O3 substrate and maintaining the heating temperature of the deposition substrate at 100°C is sample B of Example 3, and the thin film obtained by using an Al2O3 substrate and maintaining the heating temperature of the deposition substrate at 200°C is sample C of Example 3.

[0134] In addition, a thin film obtained by using a SiO2 substrate and maintaining the heating temperature of the deposition substrate at 15°C is sample D of Example 3, a thin film obtained by using a SiO2 substrate and maintaining the heating temperature of the deposition substrate at 100°C is sample E of Example 3, and a thin film obtained by using a SiO2 substrate and maintaining the heating temperature of the deposition substrate at 200°C is sample F of Example 3.

[0135]

[0136] Example 4: Preparation of a chalcogenide compound thin film (Bi4Se3) 4

[0137] A simultaneous deposition device including a deposition chamber, a deposition rotation unit equipped with a deposition substrate, an E-beam evaporation unit, a thermal evaporation unit, and a deposition sensor was prepared.

[0138] Afterwards, the vacuum level inside the deposition chamber was 10 -6The pressure was maintained at 10 Torr, the heating temperature of the deposition substrate was maintained at 200°C, and the e-beam evaporator and the thermal evaporator were operated to evaporate Bi, a positive material, and Se, a chalcogen material, and the deposition rate ratio of Bi and Se was set to 4:3.

[0139] Here, the deposition substrate is an aluminum oxide (Al2O3) substrate, a silicon (Si) substrate, or a silicon (Si) / silicon oxide (SiO2) substrate.

[0140] In addition, the deposition rate of the thin film was set to 6.85 nm / min, and the deposition was performed for 3 minutes and 40 seconds to obtain a chalcogenide compound thin film having a Bi4Se3 composition (Example 4).

[0141]

[0142] Example 5: Preparation of a chalcogenide compound thin film (Bi2Te3) 5

[0143] A simultaneous deposition device including a deposition chamber, a deposition rotation unit equipped with a deposition substrate, an E-beam evaporation unit, a thermal evaporation unit, and a deposition sensor was prepared.

[0144] Afterwards, the vacuum level inside the deposition chamber was 10 -6 The temperature was maintained at 1 Torr, the heating temperature of the deposition substrate was maintained at 15°C, 100°C, or 200°C, and the two-beam evaporator and the thermal evaporator were operated to evaporate Bi, a positive material, and Te, a chalcogen material, and the deposition rate ratio of Bi and Te was set to 2:3.

[0145] Here, the deposition substrate is an aluminum oxide (Al2O3) substrate or a silicon (Si) / silicon oxide (SiO2) substrate.

[0146] In addition, a chalcogenide compound thin film having a Bi2Te3 composition was obtained by depositing for 8 minutes and 20 seconds so that the deposition rate of the thin film satisfies 5.52 nm / min (Example 5).

[0147] Here, the thin film obtained by using an Al2O3 substrate and maintaining the heating temperature of the deposition substrate at 15°C is sample A of Example 5, the thin film obtained by using an Al2O3 substrate and maintaining the heating temperature of the deposition substrate at 100°C is sample B of Example 5, and the thin film obtained by using an Al2O3 substrate and maintaining the heating temperature of the deposition substrate at 200°C is sample C of Example 5.

[0148] In addition, a thin film obtained by using a SiO2 substrate and maintaining the heating temperature of the deposition substrate at 15°C is sample D of Example 5, a thin film obtained by using a SiO2 substrate and maintaining the heating temperature of the deposition substrate at 100°C is sample E of Example 5, and a thin film obtained by using a SiO2 substrate and maintaining the heating temperature of the deposition substrate at 200°C is sample F of Example 5.

[0149]

[0150] Example 6: Preparation of a chalcogenide compound thin film (Cu2Te) 6

[0151] A simultaneous deposition device including a deposition chamber, a deposition rotation unit equipped with a deposition substrate, an E-beam evaporation unit, a thermal evaporation unit, and a deposition sensor was prepared.

[0152] Afterwards, the vacuum level inside the deposition chamber was 10 -6 The pressure was maintained at 100 Torr, the heating temperature of the deposition substrate was maintained at 100°C, and the e-beam evaporator and the thermal evaporator were operated to evaporate Cu, a positive material, and Te, a chalcogen material, and the deposition rate ratio of Cu and Te was made to satisfy 2:1.

[0153] Here, the deposition substrate is an aluminum oxide (Al2O3) substrate or a silicon (Si) / silicon oxide (SiO2) substrate.

[0154] In addition, the deposition rate of the thin film was set to 10.2 nm / min, and the thin film was deposited for 10 minutes and 30 seconds to obtain a chalcogenide compound thin film having a Cu2Te composition (Example 6).

[0155]

[0156] Example 7: Preparation of a chalcogenide compound thin film (MoSe2) 7

[0157] A simultaneous deposition device including a deposition chamber, a deposition rotation unit equipped with a deposition substrate, an E-beam evaporation unit, a thermal evaporation unit, and a deposition sensor was prepared.

[0158] Afterwards, the vacuum level inside the deposition chamber was 10 -6 The pressure was maintained at 10 Torr, the heating temperature of the deposition substrate was maintained at 200°C, and the e-beam evaporator and the thermal evaporator were operated to evaporate the positive material Mo and the chalcogen material Se, and the deposition rate ratio of the Mo and the Se was set to 1:2.

[0159] Here, the deposition substrate is an aluminum oxide (Al2O3) substrate, a silicon (Si) / silicon oxide (SiO2) substrate, or a germanium (Ge) / graphene (Gr) substrate.

[0160] In addition, the deposition rate of the thin film was set to 0.69 nm / min, and the deposition was performed for 11 minutes and 40 seconds to obtain a chalcogenide compound thin film having a MoSe2 composition (Example 7).

[0161]

[0162] Example 8: Preparation of a double-layer chalcogenide compound thin film (TiSe2 / SnSe2)

[0163] A simultaneous deposition device including a deposition chamber, a deposition rotation unit equipped with a deposition substrate, an E-beam evaporation unit, a thermal evaporation unit, and a deposition sensor was prepared.

[0164] Afterwards, the vacuum level inside the deposition chamber was 10 -6 The pressure was maintained at 10 Torr, the heating temperature of the deposition substrate was maintained at 500°C, and the e-beam evaporator and the thermal evaporator were operated to evaporate Ti, a positive material, and Se, a chalcogen material, and the deposition rate ratio of Ti and Se was set to 1:2.

[0165] Here, the deposition substrate is an aluminum oxide (Al2O3) substrate.

[0166] In addition, a chalcogenide compound thin film with a TiSe2 composition was synthesized by depositing for 13 minutes so that the deposition rate of the thin film satisfies 0.84 nm / min.

[0167] Afterwards, the vacuum level inside the deposition chamber was 10 -6 The pressure was maintained at 10 Torr, the heating temperature of the deposition substrate was maintained at 200°C or 300°C, and the e-beam evaporator and the thermal evaporator were operated to evaporate the positive material Sn and the chalcogen material Se, and the deposition rate ratio of the Sn and the Se was made to satisfy 1:2.

[0168] In addition, a double-layer chalcogenide compound thin film having a TiSe2 / SnSe2 composition was obtained by depositing (in-situ epitaxial growth) on the chalcogenide compound thin film having the TiSe2 composition for 12 minutes and 20 seconds so that the deposition rate of the thin film satisfies 0.93 nm / min (Example 8).

[0169] Here, the thin film obtained by maintaining the heating temperature of the deposition substrate at 200°C is sample A of Example 8, and the thin film obtained by maintaining the heating temperature of the deposition substrate at 300°C is sample B of Example 8.

[0170]

[0171] Experimental Example 1: Crystal Growth Analysis

[0172] In a method for manufacturing a chalcogenide compound thin film according to one embodiment of the present invention, in order to confirm the crystal growth of the chalcogenide compound thin film (TiSe2) according to Example 1, actual analysis, XRD analysis, and XRR analysis were performed, and the results are shown in FIG. 4.

[0173] Figure 4 shows the results of evaluating the characteristics of a chalcogenide compound thin film according to Example 1 of the present invention.

[0174] FIG. 4a) is an actual photograph of a chalcogenide compound thin film (TiSe2) according to Example 1, FIG. 4b) is an XRD analysis result for each point of a chalcogenide compound thin film (TiSe2) according to Example 1, FIG. 4c) is a drawing in which XRD graphs for each point of a chalcogenide compound thin film (TiSe2) according to Example 1 are superimposed, and FIG. 4d) is an XRR analysis result for each point of a chalcogenide compound thin film (TiSe2) according to Example 1.

[0175] As illustrated in Fig. 4, a TiSe2 thin film with a thickness of approximately 25 nm was simultaneously deposited and obtained on a 4-inch silicon (Si) substrate. It was confirmed that the TiSe2 thin film grew in a vdW layered structure along the ab-plane.

[0176] Additionally, the overlapping XRD graphs are confirmed to be within a 5% error range, so it is judged to be homogeneously deposited.

[0177] In addition, when looking at the overlapping XRR graph, the thickness at point 1 was confirmed to be 24.5 nm, the thickness at point 2 was 25.2 nm, the thickness at point 3 was 25.3 nm, the thickness at point 4 was 25.3 nm, and the thickness at point 5 was 25.9 nm, which was confirmed to be within the 3% error range.

[0178]

[0179] Experimental Example 2: XPS analysis, work function-hole concentration analysis

[0180] In a method for manufacturing a chalcogenide compound thin film according to one embodiment of the present invention, actual analysis, XRD analysis, XPS analysis, and hole concentration analysis of the chalcogenide compound thin film (NiSe2) according to Example 2 were performed, and the results are shown in FIG. 5.

[0181] Figure 5 shows the results of evaluating the characteristics of a chalcogenide compound thin film according to Example 2 of the present invention.

[0182] FIG. 5a) is a real photograph of a patterned chalcogenide compound thin film (NiSe2) according to Example 2, FIG. 5b) is an XRD analysis result of a chalcogenide compound thin film (NiSe2) according to Example 2, FIG. 5c) is a full-range XPS analysis result of a chalcogenide compound thin film (NiSe2) according to Example 2, FIG. 5d) is an oxygen region XPS analysis result of a chalcogenide compound thin film (NiSe2) according to Example 2, FIG. 5e) is a graph showing the hole concentration verified through repeated measurements of a chalcogenide compound thin film (NiSe2) according to Example 2, and FIG. 5f) is a drawing showing the work function-hole concentration comparison result of a chalcogenide compound thin film (NiSe2) according to Example 2.

[0183] As shown in Fig. 5, a NiSe2 thin film having a preset pattern was simultaneously deposited on a 4-inch silicon (Si) / silicon oxide (SiO2) substrate, and the NiSe2 thin film was determined to be homogeneously deposited as it was confirmed to be within the error range of 3.39% hole concentration, 0.42% resistivity, and 2.52% thickness.

[0184] Additionally, XRD analysis confirmed that polycrystalline NiSe2 was well grown.

[0185] In addition, the XPS analysis results showed that no elements other than Ni and Se that participated in the bonding were identified, and the trace amount of oxygen detected was not formed by bonding with the material, but was an element adsorbed on the surface, confirming that oxidation of NiSe2 did not occur.

[0186] It was also confirmed that it has the highest hole concentration among metals with high work functions.

[0187] Therefore, NiSe2 with excellent physical properties at low temperatures was synthesized as a result of the present invention.

[0188]

[0189] Experimental Example 3: Crystal Growth and Electron Mobility Analysis

[0190] In a method for manufacturing a chalcogenide compound thin film according to one embodiment of the present invention, XRD analysis, electron mobility analysis, and SEM analysis of the chalcogenide compound thin film (Bi2Se3) according to Example 3 were performed, and the results are shown in FIG. 6.

[0191] Figure 6 shows the results of evaluating the characteristics of a chalcogenide compound thin film according to Example 3 of the present invention.

[0192] FIG. 6a) is an XRD analysis result of chalcogenide compound thin films (Bi2Se3) according to sample A, sample B, and sample C of Example 3 depending on the heating temperature, FIG. 6b) is an XRD analysis result of chalcogenide compound thin films (Bi2Se3) according to sample D, sample E, and sample F of Example 3 depending on the heating temperature, FIG. 6c) is an electron mobility analysis result of chalcogenide compound thin films (Bi2Se3) according to sample A, sample B, and sample C of Example 3 depending on the heating temperature, FIG. 6d) is an electron mobility analysis result of chalcogenide compound thin films (Bi2Se3) according to sample D, sample E, and sample F of Example 3 depending on the heating temperature, FIG. 6e) is an SEM analysis result of chalcogenide compound thin films (Bi2Se3) according to sample C of Example 3, and FIG. 6f) is an XRD analysis result of chalcogenide compound thin films (Bi2Se3) according to sample F of Example 3. This is the SEM analysis result of the thin film (Bi2Se3).

[0193] As shown in Fig. 6, it was confirmed that high crystallinity and excellent mobility of Bi2Se3 thin film can be achieved at an optimal temperature of 200°C and on an Al2O3 substrate.

[0194] Specifically, it was confirmed through XRD that the Bi2Se3 thin film had the best crystallinity when the substrate was Al2O3 at 200℃, and through Hall measurement, it was confirmed that Al2O3 had the highest carrier mobility at 200℃. In addition, it was confirmed through SEM surface analysis that the surface roughness of the chalcogenide compound thin film (Bi2Se3) grown on the Al2O3 substrate at 200℃ was low. Accordingly, it was confirmed that the finally obtained chalcogenide compound thin film (Bi2Se3) had the best quality when the substrate was Al2O3 at 200℃.

[0195]

[0196] Experimental Example 4: Crystal Growth Analysis

[0197] In a method for manufacturing a chalcogenide compound thin film according to one embodiment of the present invention, in order to confirm the crystal growth of the chalcogenide compound thin film (Bi4Se3) according to Example 4, XRD analysis was performed, and the results are shown in Fig. 7.

[0198] Figure 7 shows the results of evaluating the characteristics of a chalcogenide compound thin film according to Example 4 of the present invention.

[0199] Fig. 7a) is an XRD analysis result for each substrate of a chalcogenide compound thin film (Bi4Se3) according to Example 4, and Fig. 7b) is an enlarged view of the 5-10 degree region of the Al2O3 substrate among the XRD graphs of the chalcogenide compound thin film (Bi4Se3) according to Example 4.

[0200] As illustrated in Fig. 7, a Bi4Se3 thin film with a thickness of approximately 35 nm was obtained by simultaneous deposition on aluminum oxide (Al2O3), a silicon (Si) substrate, and a silicon (Si) / silicon oxide (SiO2) substrate. It was confirmed that the Bi4Se3 thin film had high crystallinity on the aluminum oxide (Al2O3) substrate and grew in a vdW layered structure along the ab-plane.

[0201] Additionally, a periodic pattern (laue oscillation) repeating at 6 to 8 degrees was confirmed, confirming that epitaxial growth had occurred.

[0202]

[0203] Experimental Example 5: Crystal Growth and Electron Mobility Analysis

[0204] In a method for manufacturing a chalcogenide compound thin film according to one embodiment of the present invention, XRD analysis and electron mobility analysis of the chalcogenide compound thin film (Bi2Te3) according to Example 5 were performed, and the results are shown in FIG. 8.

[0205] Figure 8 shows the results of evaluating the characteristics of a chalcogenide compound thin film according to Example 5 of the present invention.

[0206] FIG. 8a) shows the XRD analysis results of chalcogenide compound thin films (Bi2Te3) according to sample A, sample B, and sample C of Example 5 depending on the heating temperature, FIG. 8b) shows the XRD analysis results of chalcogenide compound thin films (Bi2Te3) according to sample D, sample E, and sample F of Example 5 depending on the heating temperature, FIG. 8c) shows the electron mobility analysis results of chalcogenide compound thin films (Bi2Te3) according to sample A, sample B, and sample C of Example 5 depending on the heating temperature, and FIG. 8d) shows the electron mobility analysis results of chalcogenide compound thin films (Bi2Te3) according to sample D, sample E, and sample F of Example 5 depending on the heating temperature.

[0207] As shown in Fig. 8, it was confirmed that high mobility of Bi2Te3 thin film can be realized at an optimal temperature of 200°C and on an Al2O3 substrate.

[0208] Specifically, it was confirmed through XRD that the Bi2Te3 thin film had the best crystallinity when the substrate was Al2O3 at 200℃, and through Hall measurement, it was confirmed that Al2O3 had the highest carrier mobility at 200℃. However, when synthesized at 15℃ on a SiO2 substrate, the mobility could not be properly measured. Accordingly, it was confirmed that the finally obtained chalcogenide compound thin film (Bi2Te3) had the best quality when the substrate was Al2O3 at 200℃.

[0209]

[0210] Experimental Example 6: Crystal Growth Analysis

[0211] In a method for manufacturing a chalcogenide compound thin film according to one embodiment of the present invention, in order to confirm the crystal growth of the chalcogenide compound thin film (Cu2Te) according to Example 6, XRD analysis and SEM analysis were performed, and the results are shown in Fig. 9.

[0212] Figure 9 shows the results of evaluating the characteristics of a chalcogenide compound thin film according to Example 6 of the present invention.

[0213] Figure 9a) is an XRD analysis result for each substrate of a chalcogenide compound thin film (Cu2Te) according to Example 6, and Figure 9b) is an SEM analysis result of a chalcogenide compound thin film (Cu2Te) synthesized on a SiO2 substrate according to Example 6.

[0214] As illustrated in Fig. 9, a Cu2Te thin film having a thickness of approximately 108.7 nm was obtained by simultaneous deposition on aluminum oxide (Al2O3) and silicon (Si) / silicon oxide (SiO2) substrates. It was confirmed that the Cu2Te thin film had high crystallinity on the aluminum oxide (Al2O3) substrate and thus had excellent quality.

[0215]

[0216] Experimental Example 7: Crystal Growth Analysis

[0217] In a method for manufacturing a chalcogenide compound thin film according to one embodiment of the present invention, in order to confirm the crystal growth of the chalcogenide compound thin film (MoSe2) according to Example 7, XRD analysis, Phi scan analysis, and SEM analysis were performed, and the results are shown in FIG. 10.

[0218] Figure 10 shows the results of evaluating the characteristics of a chalcogenide compound thin film according to Example 7 of the present invention.

[0219] FIG. 10a) is an XRD analysis result for each substrate of a chalcogenide compound thin film (MoSe2) according to Example 7, FIG. 10b) is a Phi scan analysis result for a chalcogenide compound thin film (MoSe2) synthesized on a Ge / Gr substrate according to Example 7, FIG. 10c) is an SEM analysis result for a chalcogenide compound thin film (MoSe2) synthesized on a Ge / Gr substrate according to Example 7, and FIG. 10d) is an SEM analysis result for a chalcogenide compound thin film (MoSe2) synthesized on a SiO2 substrate according to Example 7.

[0220] As illustrated in Fig. 10, a MoSe2 thin film with a thickness of about 8 nm was simultaneously deposited on an aluminum oxide (Al2O3) substrate, a silicon (Si) / silicon oxide (SiO2) substrate, or a germanium (Ge) / graphene (Gr) substrate. The MoSe2 thin film was confirmed to exhibit excellent crystal growth with very high crystallinity on a germanium (Ge) / graphene (Gr) substrate, but high surface roughness was observed. On the silicon (Si) / silicon oxide (SiO2) substrate, it was confirmed to have excellent quality with both excellent crystallinity and low surface roughness despite a low thickness of 8 nm.

[0221]

[0222] Experimental Example 8: Crystal Growth Analysis

[0223] In a method for manufacturing a chalcogenide compound thin film according to one embodiment of the present invention, in order to confirm the crystal growth of the double-layer chalcogenide compound thin film (TiSe2 / SnSe2) according to Example 8, XRD analysis, In-plane XRD analysis, TEM analysis, and XRR analysis were performed, and the results are shown in FIG. 11.

[0224] Figure 11 shows the results of evaluating the characteristics of a chalcogenide compound thin film according to Example 8 of the present invention.

[0225] FIG. 11a) is the XRD analysis result of the chalcogenide compound thin film (TiSe2 / SnSe2) according to sample A of example 8, FIG. 11b) is the in-plane XRD analysis result of the chalcogenide compound thin film (TiSe2 / SnSe2) according to sample A of example 8, FIG. 11c) is the cross-section TEM analysis result of the chalcogenide compound thin film (TiSe2 / SnSe2) according to sample A of example 8, FIG. 11d) is the cross-section TEM analysis result of the chalcogenide compound thin film (TiSe2 / SnSe2) according to sample B of example 8, FIG. 11e) is the XRR analysis result of the chalcogenide compound thin film (TiSe2 / SnSe2) according to sample A of example 8, and FIG. 11f) is the XRR of the chalcogenide compound thin film (TiSe2 / SnSe2) according to sample B of example 8. This is the analysis result.

[0226] As shown in Fig. 11, it was confirmed that heteroepitaxial growth of TiSe2 / SnSe2 thin films could be achieved at an optimal temperature of 200°C.

[0227] Specifically, a SnSe2 thin film was additionally epitaxially grown on an epitaxially grown TiSe2 thin film, and the epitaxial orientation was confirmed through in-plane XRD, and the epitaxial growth was confirmed to be formed by vdW bonding between the two layers. In addition, a clear epitaxial interface was confirmed at 200°C through TEM and XRR. Accordingly, it was confirmed that the finally obtained double-layer chalcogenide compound thin film (TiSe2 / SnSe2) had the best quality at 200°C.

[0228] Although the method for manufacturing a chalcogenide compound thin film according to the above embodiments of the present invention has been described as a specific embodiment, this is merely an example, and the present invention is not limited thereto, and should be interpreted as having the widest scope according to the basic idea disclosed in this specification. Those skilled in the art may implement embodiments not specified by combining or replacing the disclosed embodiments, but this also does not exceed the scope of the present invention. In addition, those skilled in the art may easily change or modify the disclosed embodiments based on this specification, and it is clear that such changes or modifications also fall within the scope of the present invention.

Claims

1. A method for manufacturing a chalcogenide compound thin film using a simultaneous deposition device including a deposition chamber unit that maintains a preset vacuum level; a deposition rotation unit provided with a deposition substrate and disposed within the deposition chamber unit; an E-beam evaporation unit that evaporates a positive material as a raw material; a thermal evaporation unit that evaporates a chalcogen material as a raw material; and a deposition sensor that senses the deposition amount and deposition speed of the positive material and the chalcogen material deposited on the deposition substrate. A deposition step for simultaneously depositing a positive material and a chalcogen material on the deposition substrate through a simultaneous deposition process using the simultaneous deposition device, thereby obtaining a chalcogenide compound thin film having a preset composition; including; Method for manufacturing a thin film of a chalcogenide compound.

2. In paragraph 1, In the above deposition step, The positive material is at least one material selected from the group consisting of Ti, Ni, Cu, Ge, Mo, Sn, Sb, and Bi, The above chalcogen material is at least one material selected from the group consisting of S, Se and Te, The above-mentioned positive material and the above-mentioned chalcogen material are simple element materials composed of only one type of element. Method for manufacturing a thin film of a chalcogenide compound.

3. In paragraph 1, The above deposition step is, It is performed within the above deposition chamber, and the vacuum level within the deposition chamber is 10 -6 ~ 10 -5 Satisfying the range of Torr, Method for manufacturing a thin film of a chalcogenide compound.

4. In paragraph 1, In the above deposition step, The above chalcogenide compound thin film is deposited so as to satisfy a deposition rate range of 0.3 to 60 nm / min. Method for manufacturing a thin film of a chalcogenide compound.

5. In paragraph 1, In the above deposition step, By controlling the deposition rate ratio of the positive material and the chalcogen material, the composition of the chalcogenide compound thin film is selectively controlled. The deposition rate of the positive material and the chalcogen material satisfies the range of 0.05 to 10 Å / s. Method for manufacturing a thin film of a chalcogenide compound.

6. In paragraph 5, The deposition rate ratio of the positive material and the chalcogen material is 1 to 7:1 to 4. Method for manufacturing a thin film of a chalcogenide compound.

7. In paragraph 1, The above deposition step is, Further comprising a re-evaporation step of re-evaporating residual raw materials by performing a deposition substrate heating process that heats the deposition substrate to satisfy a heating temperature range of 20 to 200°C; Method for manufacturing a thin film of a chalcogenide compound.

8. In paragraph 7, The above deposition step is, Before the above re-evaporation step, a step of deriving a heating temperature range for performing the deposition substrate heating process is further included; The step of deriving the above heating temperature range is: A step of obtaining a deposition rate value of a chalcogen material deposited on the deposition substrate through the deposition sensor; A step of obtaining a re-evaporation rate value of a chalcogen material re-evaporated on the deposition substrate by considering the adhesion coefficient of the deposition substrate, the vapor pressure of the chalcogen material, the vacuum level of the deposition chamber, and the heating temperature of the deposition substrate; and A step of deriving a heating temperature range of the deposition substrate so that the re-evaporation rate value of the obtained chalcogen material is greater than the deposition rate value of the obtained chalcogen material; including; Method for manufacturing a thin film of a chalcogenide compound.

9. In paragraph 1, In the above deposition step, The above chalcogenide compound thin film comprises at least one material selected from a saturated composition chalcogenide compound and a non-saturated composition chalcogenide compound, The above chalcogenide compound thin film comprises at least one material selected from the group consisting of MoS2, NiS, Ni3S4, NiS2, SnS2, SnS, Ti2S, TiS, TiS2, TiS3, Cu2S, CuS, GeS, GeS2, Bi2S3, Sb2S3, MoSe2, NiSe, Ni3Se4, NiSe2, SnSe, SnSe2, TiSe2, Cu3Se2, CuSe, CuSe2, GeSe, GeSe2, Bi2Se, Bi4Se3, BiSe, Bi2Se3, Sb2Se3, MoTe2, Ni3Te2, NiTe, NiTe2, SnTe, Ti5Te4, TiTe, Ti3Te4, TiTe2, Cu7Te4, Cu2Te, CuTe, CuTe2, GeTe, Bi7Te3, Bi2Te, Bi4Te3, BiTe, Bi2Te3 and Sb2Te3. Method for manufacturing a thin film of a chalcogenide compound.

10. In paragraph 9, In the above deposition step, The above chalcogenide compound thin film is composed of a single layer or multiple layers. Method for manufacturing a thin film of a chalcogenide compound.

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