Method for manufacturing chalcogenide-based compound thin films

Abstract

The present invention relates to a method for manufacturing a thin film of a chalcogenide compound. According to one embodiment, a method for manufacturing a chalcogenide compound thin film may be provided, comprising: a deposition step of simultaneously depositing a positively charged material and a chalcogenide material on a deposition substrate through a simultaneous deposition process using a simultaneous deposition apparatus to obtain a chalcogenide compound thin film having a preset composition.

Description

Technology Field

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

[0002] A chalcogenide is a compound composed of at least one chalcogen ion [an element of Group 16 (VIA) of the periodic table, e.g., sulfur (S), selenium (Se), and tellurium (Te)] and at least one electropositive element.

[0003] Chalcogenide compounds, composed of binary or higher compounds, are known as materials with diverse properties that easily transform from crystalline to amorphous, semiconductor to metallic, or ionic to electron conductors in response to external electrical stimulation, thermal energy stimulation, and light energy stimulation. Due to these diverse material characteristics, they are widely utilized in applications such as thin film materials for information storage / processing, solar cells, ion-conducting thin film materials, and information recognition / display thin film materials.

[0004] Known methods used to synthesize chalcogenide compound thin films include Chemical Vapor Deposition (CVD), Chemical Vapor Transport (CVT), and Molecular Beam Epitaxy (MBE).

[0005] However, the synthesis methods described above are difficult to apply industrially due to demanding process conditions and contact resistance issues.

[0006] Specifically, in the case of CVD and CVT, high energy is required for the evaporation of positively charged elements, resulting in high-temperature synthesis processes. Lowering the synthesis temperature through the use of organic precursors or catalysts leads to quality degradation due to the incorporation of impurities and presents limitations in achieving large-area growth.

[0007] In addition, MBE has limitations such as high equipment costs and low growth rates, as it requires maintaining an ultra-high vacuum and using a material supply device like a Knudsen cell for each material.

[0008] Accordingly, for the industrialization of calogenide compounds, research on manufacturing methods capable of large-area growth at low cost, rapid growth rates, and excellent quality is essential. The problem to be solved

[0009] A method for manufacturing a chalcogenide-based compound thin film according to one embodiment of the present invention ensures compatibility by using equipment utilized in existing semiconductor processes, enables large-area synthesis, and allows synthesis even at low temperatures (250°C or lower), thereby minimizing thermal costs and the impact of thermal limitations between semiconductor processes.

[0010] In addition, since only the materials constituting the composition of the compound are used in a high vacuum, high-purity, high-quality thin film synthesis is possible, and various combinations of chalcogenide-based compound thin films can be easily synthesized by easily changing the types of positive and chalcogen elements. means of solving the problem

[0011] According to one embodiment, a method for manufacturing a chalcogenide-based compound thin film using a simultaneous deposition apparatus comprising: a deposition chamber portion maintaining a preset vacuum level; a deposition rotating portion disposed within the deposition chamber portion and equipped with a deposition substrate; an E-beam evaporation portion disposed within the deposition chamber portion and evaporating a positively charged material which is a raw material; a thermal evaporation portion disposed within the deposition chamber portion and evaporating a chalcogenide material which is a raw material; and a deposition sensor that senses the deposition amount and deposition rate of the positively charged material and the chalcogenide material deposited on the deposition substrate; wherein the method comprises a deposition step of simultaneously depositing the positively charged material and the chalcogenide material on the deposition substrate through a simultaneous deposition process using the simultaneous deposition apparatus to obtain a chalcogenide-based compound thin film having a preset composition.

[0012] In addition, a method for manufacturing a chalcogenide compound thin film may be provided, wherein in the deposition step, the positively charged material is at least one material selected from the group consisting of Ti, Ni, Cu, Ge, Mo, Sn, Sb, and Bi, the chalcogenide material is at least one material selected from the group consisting of S, Se, and Te, and the positively charged material and the chalcogenide material are elemental materials composed of only one type of element.

[0013] In addition, the deposition step is performed within the deposition chamber, wherein the vacuum level within the deposition chamber is 10 -6 ~ 10 -5 A method for manufacturing a chalcogenide-based compound thin film satisfying the Torr range can be provided.

[0014] In addition, a method for manufacturing a chalcogenide compound thin film may be provided, wherein in the deposition step, the chalcogenide compound thin film is deposited to satisfy a deposition rate range of 0.3 to 60 nm / min.

[0015] In addition, a method for manufacturing a chalcogenide-based compound thin film can be provided, wherein, in the deposition step, the composition of the chalcogenide-based compound thin film is selectively controlled by adjusting the ratio of the deposition rates of the positively charged material and the chalcogenide material, and the deposition rates of the positively charged material and the chalcogenide material satisfy a range of 0.05 to 10 Å / s.

[0016] In addition, a method for manufacturing a chalcogenide-based compound thin film can be provided, wherein the deposition rate ratio of the positively charged material and the chalcogenide material is 1 to 7:1 to 4.

[0017] In addition, a method for manufacturing a chalcogenide-based compound thin film may be provided, wherein the deposition step further comprises a re-evaporation step in which a deposition substrate heating process is performed to heat the deposition substrate to a heating temperature range of 20 to 200°C to re-evaporate residual raw material.

[0018] Additionally, the deposition step further comprises a step of deriving a heating temperature range for performing a heating process of the deposition substrate prior to the re-evaporation step; wherein the step of deriving the heating temperature range comprises: a step of obtaining a deposition rate value of a chalcogenide material deposited on the deposition substrate through the deposition sensor; a step of obtaining a re-evaporation rate value of a chalcogenide material re-evaporated on the deposition substrate by considering the adhesion coefficient of the deposition substrate, the vapor pressure of the chalcogenide 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 such that the obtained re-evaporation rate value of the chalcogenide material is greater than the obtained deposition rate value of the chalcogenide material. A method for manufacturing a chalcogenide-based compound thin film may be provided.

[0019] In addition, in the deposition step, the chalcogenide compound thin film comprises at least one material selected from a chalcogenide compound of saturated composition and a chalcogenide compound of unsaturated composition, and the chalcogenide compound thin film comprises 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, A method for manufacturing a chalcogenide compound thin film comprising at least one material selected from the group consisting of Bi7Te3, Bi2Te, Bi4Te3, BiTe, Bi2Te3, and Sb2Te3 may be provided.

[0020] In addition, a method for manufacturing a chalcogenide-based compound thin film may be provided, wherein in the deposition step, the chalcogenide-based compound thin film is composed of a single layer or multiple layers. Effects of the invention

[0021] A method for manufacturing a chalcogenide-based compound thin film according to one embodiment of the present invention ensures compatibility by using equipment utilized in existing semiconductor processes, enables large-area synthesis, and allows synthesis even at low temperatures (250°C or lower), thereby having the effect of minimizing thermal costs and the impact of thermal limitations between semiconductor processes.

[0022] In addition, since only the materials constituting 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 and chalcogen elements, various combinations of chalcogenide-based compound thin films can be easily synthesized. Brief explanation of the drawing

[0023] FIG. 1 is a drawing for explaining a simultaneous deposition apparatus according to one embodiment of the present invention. FIG. 2 is a flowchart illustrating a method for manufacturing a chalcogenide-based compound thin film according to one embodiment of the present invention. FIG. 3 is a diagram briefly illustrating a chalcogenide-based compound thin film according to one embodiment of the present invention. Figure 4 is the result of the characteristic evaluation of a chalcogenide-based compound thin film according to Example 1 of the present invention. Figure 5 is the result of the characteristic evaluation of a chalcogenide-based compound thin film according to Example 2 of the present invention. Figure 6 is the result of the characteristic evaluation of a chalcogenide-based compound thin film according to Example 3 of the present invention. Figure 7 is the result of the characteristic evaluation of a chalcogenide-based compound thin film according to Example 4 of the present invention. Figure 8 is the result of the characteristic evaluation of a chalcogenide-based compound thin film according to Example 5 of the present invention. Figure 9 is the result of the characteristic evaluation of a chalcogenide-based compound thin film according to Example 6 of the present invention. Figure 10 is the result of the characteristic evaluation of a chalcogenide-based compound thin film according to Example 7 of the present invention. Figure 11 is the result of the characteristic evaluation of a chalcogenide-based compound thin film according to Example 8 of the present invention. Specific details for implementing the invention

[0024] In order to fully understand the structure and effects of the present invention, preferred embodiments of the present invention will be described in detail with reference to the attached drawings.

[0025] 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. The description of the embodiments is provided merely to ensure that the disclosure of the present invention is complete and to fully inform those skilled in the art of the scope of the invention. In the attached drawings, the components are depicted enlarged from their actual size for convenience of explanation, and the proportions of each component may be exaggerated or reduced.

[0026] The terms used in this specification are for describing embodiments and are not intended to limit the invention. Furthermore, unless otherwise defined, the terms used in this specification may be interpreted in the sense commonly known to those skilled in the art. In this specification, the singular form includes the plural form unless specifically stated otherwise in the text. As used in this specification, 'comprises' and / or 'comprising' do not exclude the presence or addition of one or more other components, steps, actions, and / or elements to the mentioned components, steps, actions, and / or elements.

[0027] Where in this specification a layer is referred to as being 'on' another layer, it may be formed directly on the surface of the other layer or a third layer may be interposed between them. Although terms such as first, second, etc., have been used in this specification to describe various regions, layers, etc., these regions and layers should not be limited by such terms. These terms are used merely to distinguish one specific region or layer from another region or layer. Accordingly, a part referred to as the first part in one embodiment may be referred to as the second part in another embodiment. The embodiments described and illustrated herein also include their complementary embodiments. Throughout the specification, parts indicated by the same reference numeral represent the same components.

[0028] The present invention provides a method for synthesizing low-cost, high-quality, and large-area chalcogenide compound thin films by utilizing a beam evaporator and a thermal evaporator used in semiconductor processes.

[0029] Specifically, the present invention is designed to obtain chalcogenide-based compound thin films having various compositions by simultaneously depositing a positively charged material and a chalcogenide material and controlling the deposition rate ratio between each material.

[0030] In addition, the present invention is designed to obtain a high-quality chalcogenide compound thin film by effectively removing residual raw materials through controlling the temperature of the deposition substrate.

[0032] Method for manufacturing a chalcogenide compound thin film

[0033] FIG. 1 is a drawing for explaining a simultaneous deposition apparatus according to one embodiment of the present invention, and FIG. 2 is a flowchart for explaining a method for manufacturing a chalcogenide-based compound thin film according to one embodiment of the present invention.

[0034] Referring to FIGS. 1 and 2, a method (S10) for manufacturing a chalcogenide-based compound thin film according to one embodiment of the present invention may utilize a simultaneous deposition apparatus (10) comprising: a deposition chamber (100) that maintains a preset vacuum level; a deposition rotation unit (200) disposed within the deposition chamber (100) and equipped with a deposition substrate (210); an E-beam evaporation unit (300) disposed within the deposition chamber (100) and evaporating a positively charged material which is a raw material; a thermal evaporation unit (400) disposed within the deposition chamber (100) and evaporating a chalcogenide material which is a raw material; and a deposition sensor (not shown) that senses the deposition amount and deposition rate of the positively charged material and chalcogenide material deposited on the deposition substrate (210).

[0035] In addition, a method (S10) for manufacturing a chalcogenide-based compound thin film according to one embodiment of the present invention comprises a deposition step (S100) of simultaneously depositing a positively charged material and a chalcogenide material on a deposition substrate (210) through a simultaneous deposition process utilizing the simultaneous deposition apparatus (10) to obtain a chalcogenide-based compound thin film having a preset composition.

[0036] First, referring to FIG. 1, the simultaneous deposition apparatus (10) may be a device that utilizes an E-beam and a thermal evaporator, respectively, inside a chamber maintained at a high vacuum to independently evaporate positively charged elements and chalcogen elements (S, Se, Te) so that they can be synthesized on a heated substrate.

[0037] That is, the above simultaneous deposition apparatus (10) may be an apparatus for synthesizing chalcogenides, which are compounds composed of at least one group 16 (chalcogen) element and one or more positively charged elements.

[0038] Specifically, by using only pure cationic and chalcogen materials in a high vacuum environment and storing each raw material within a high vacuum chamber, oxidation and adsorption can be prevented, thereby enabling the synthesis of high-purity chalcogenide compounds.

[0039] In addition, since the vapor pressure of chalcogenides is high at about 1 mTorr at 200°C, increasing the substrate temperature can effectively prevent the retention of chalcogen materials that did not participate in the synthesis.

[0040] In addition, since the E-beam and thermal source can be controlled independently, the deposition rates of positively charged and chalcogenide materials can be controlled during synthesis, and the substrate temperature can be controlled to easily synthesize high-quality thin films with various compositional ratios on the phase diagram.

[0041] Furthermore, by arranging multiple positively charged materials inside the e-beam, heterogeneous chalcogenide compounds can be synthesized in-situ within the process, or chalcogenide compound thin films with different compositional ratios can be synthesized in multiple layers, making it versatile and highly scalable.

[0042] Meanwhile, the deposition substrate (210) may be any one of a p-Si substrate, an Al2O3 substrate, a Si / SiO2 substrate, and a SiO2 substrate, but is not limited thereto.

[0043] Next, referring to FIG. 2, the method (S10) for manufacturing the chalcogenide-based compound thin film can be performed through a simultaneous deposition process using the simultaneous deposition apparatus (10) described above.

[0044] The above simultaneous deposition process may be a process for synthesizing chalcogenide compound thin films with various compositional ratios by utilizing an evaporation source placed inside a chamber to evaporate a positively charged material and a chalcogenide material, maintaining the vacuum level inside the chamber at a high vacuum, heating the substrate to a temperature required for compound formation, and controlling the deposition rate ratio of the positively charged material and the chalcogenide material.

[0045] Specifically, in the deposition step (S100), the positively charged 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.

[0046] In addition, in the deposition step (S100), the positively charged material and the chalcogen material are elemental materials composed of only one type of element.

[0047] In the method (S10) for manufacturing a chalcogenide-based compound thin film according to one embodiment of the present invention, by utilizing a simultaneous deposition apparatus (10) unlike conventional deposition equipment, the limitation of having to use a metal compound as a metal precursor to evaporate a positively charged material having a high evaporation temperature can be overcome, and the advantage of being able to use a pure positively charged material as a metal precursor is achieved.

[0048] Additionally, the deposition step (S100) is performed within the deposition chamber (100), wherein the vacuum level within the deposition chamber (100) is 10 -6 ~ 10 -5 It can satisfy the range of Torr.

[0049] Specifically, in the deposition step (S100), the deposition chamber part (100) is 10 -6 ~ 10 -5 It maintains a vacuum level satisfying the Torr range, and this vacuum level range can lower the temperature at which chalcogenide can exist in the gaseous state.

[0050] More specifically, the vacuum level in the deposition chamber (100) is 10 -6 If it is lower than Torr, a problem arises where the cost of maintaining the vacuum increases rapidly, and the vacuum level in the deposition chamber (100) is 10 -5 If it is higher than Torr, a problem may arise where the temperature range in which chalcogenide can be maintained in a gaseous state becomes too high.

[0051] In addition, in the deposition step (S100), the chalcogenide-based compound thin film can be deposited 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-based compound thin film is 0.3 to 30 nm / min.

[0052] If the deposition rate of the above chalcogenide-based compound thin film is lower than 0.3 nm / min, productivity decreases rapidly, and if the deposition rate is higher than 60 nm / min, there is a problem that it is difficult to obtain a large-area thin film of excellent quality.

[0053] In addition, in the deposition step (S100), the composition of the chalcogenide-based compound thin film can be selectively controlled by adjusting the deposition rate ratio of the positively charged material and the chalcogenide material.

[0054] In other words, when the composition ratio of chalcogenide compounds varies according to process requirements, various process requirements can be met by simply changing the deposition rate ratio of the cationic material and the chalcogen material without the need to add separate process conditions.

[0055] Furthermore, by changing the types of cationic and chalcogen materials, chalcogenide compounds with various compositional ratios can be easily synthesized.

[0056] Specifically, in the deposition step (S100), the deposition rate of the positively charged material and the chalcogenide material may satisfy a range of 0.05 to 10 Å / s, and in a preferred embodiment of the present invention, the deposition rate of the positively charged material and the chalcogenide material satisfies a range of 0.05 to 5 Å / s.

[0057] More specifically, the deposition rate ratio of the positively charged material and the chalcogenide material may be 1 to 7:1 to 4.

[0058] In a method (S10) for manufacturing a chalcogenide-based compound thin film according to one embodiment of the present invention, the deposition step (S100) may further include a re-evaporation step (S110) in which a deposition substrate heating process is performed to heat the deposition substrate (210) to satisfy a heating temperature range of 20 to 200°C to re-evaporate residual raw material.

[0059] Specifically, the re-evaporation step (S110) is performed to prevent surface adsorption of raw materials, and is a step to suppress residual raw materials that did not participate in the synthesis reaction by preventing surface adsorption.

[0060] In a method (S10) for manufacturing a chalcogenide-based compound thin film according to one embodiment of the present invention, the reaction mechanism of the raw material including the positively charged material and the chalcogen material can be explained by the Eley-Rideal Reaction.

[0061] Specifically, the Eley-Rideal Reaction is the adsorption rate (J) of the raw material, the chalcogenide. Abs This is a reaction that occurs when ) is less than 0, and more specifically, it can occur when the redevaporation rate of the chalcogenide is greater than the deposition rate of the chalcogenide.

[0062] Here, the adsorption rate of the chalcogen substance (J Abs ) is the deposition rate of chalcogenide material (J Inc The re-evaporation rate of chalcogenide (J) at the ) value T Vap It is the value minus the ) value.

[0063] Through this Eley-Rideal Reaction, residual chalcogenide material is prevented from adsorbing onto the substrate surface, and adsorption of the product occurs after the gas phase reaction, thereby obtaining a chalcogenide compound thin film with excellent compositional ratio and surface homogeneity.

[0064] Furthermore, a heating temperature range of the substrate to induce the Eley-Rideal Reaction is derived, and by setting the deposition substrate (210) to be heated to the derived heating temperature range, a vapor phase reaction of the chalcogen material can be induced to obtain a high-quality thin film.

[0065] In a method (S10) for manufacturing a chalcogenide-based 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 a heating process of the deposition substrate prior to the re-evaporation step (S110).

[0066] The step of deriving the heating temperature range (S120) may be a step of deriving the heating temperature range of the deposition substrate (210) such that the re-evaporation rate of the chalcogenide material is greater than the deposition rate of the chalcogenide material, in order to obtain a chalcogenide compound thin film having a specific composition ratio according to process requirements as previously described.

[0067] That is, the step (S120) of deriving the above heating temperature range is the adsorption rate (J) of the chalcogen material, which is the raw material. Abs The step may be to derive a heating temperature range of the deposition substrate (210) such that ) is less than 0.

[0068] More specifically, the step (S120) of deriving the heating temperature range is the deposition rate value (J) of the chalcogen material deposited on the deposition substrate (210) through the deposition sensor. Inc Step (S211) of obtaining ) adhesion coefficient (α) of the deposition substrate (210), vapor pressure (P) of the chalcogen material T Vap ), vacuum level (P) of the deposition chamber (100) Cham Considering the heating temperature (T) of the deposition substrate (210) and the re-evaporation rate value (J) of the chalcogen material re-evaporated on the deposition substrate (210) T VapIt may include a step (S212) of obtaining ) and a step (S213) of deriving a heating temperature (T) range of the deposition substrate (210) such that the re-evaporation rate value of the obtained chalcogen material is greater than the deposition rate value of the obtained chalcogen material.

[0069] The adsorption rate of the raw material chalcogen can be expressed by the following mathematical formula 1.

[0070] [Mathematical Formula 1]

[0071] J Abs =J Inc -J T Vap

[0072] (J Abs : Adsorption rate of a substance, J Inc : Deposition rate of material, J T Vap : Re-evaporation rate of a substance)

[0074] At this time, J T Vap It 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 formula 2.

[0075] [Mathematical Formula 2]

[0076]

[0077] (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])

[0079] Adsorption rate of chalcogen substances (J AbsIf ) is greater than 0, the chalcogenide is adsorbed onto the substrate surface, and the adsorption rate of the chalcogenide (J Abs If ) is less than 0, the chalcogen material cannot be adsorbed onto 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 material, and the chamber pressure are determined, the heating temperature of the deposition substrate (210) is controlled to control the adsorption rate (J) of the chalcogen material. Abs The size and sign of ) can be controlled.

[0080] In other words, the step (S120) of deriving the heating temperature range above is the adsorption rate (J of the chalcogenide material) Abs The step may be to find a heating temperature range of the deposition substrate (210) such that ) is less than 0.

[0081] In a method (S10) for manufacturing a chalcogenide-based compound thin film according to another embodiment of the present invention, the re-evaporation step (S110) may be a step of re-evaporating residual raw material by performing a deposition substrate heating process to heat the deposition substrate (210) to satisfy a heating temperature range of 200 to 500°C.

[0082] In a method (S10) for manufacturing a chalcogenide-based compound thin film according to another embodiment of the present invention, the reaction mechanism of the raw material including the positively charged material and the chalcogen material can be explained as a gas-phase reaction.

[0083] Specifically, the gas-phase reaction is the adsorption rate (J) of the raw materials, namely cationic and chalcogen materials. Abs This is a reaction that occurs when both are less than 0.

[0084] Through such a gas-phase reaction, residual raw materials are prevented from being adsorbed onto the substrate surface, and adsorption of the product occurs after the gas-phase reaction, thereby enabling the production of a chalcogenide-based thin film with excellent compositional ratio and surface homogeneity.

[0085] Looking at the heating temperature range of the substrate to induce a gas-phase reaction, the range for the cationic material is 200 to 500°C and the range for the chalcogenide material is 20 to 200°C. Therefore, by setting the heating temperature range based on the cationic material, both the cationic material and the chalcogenide material can undergo a gas-phase reaction to obtain a high-quality thin film.

[0086] In addition, in a method (S10) for manufacturing a chalcogenide-based 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) such that the re-evaporation rate value of the positively charged material is greater than the deposition rate value of the positively charged material in order to obtain a chalcogenide-based compound thin film having a specific composition ratio according to process requirements.

[0087] That is, the step (S120) of deriving the heating temperature range above is the adsorption rate (J of the positively charged substance) Abs The step may be to derive a heating temperature range of the deposition substrate (210) such that ) is less than 0.

[0088] More specifically, the step (S120) of deriving the heating temperature range is the deposition rate value (J) of the positively charged material deposited on the deposition substrate (210) through the deposition sensor. Inc A step of obtaining ); and the adhesion coefficient (α) of the deposition substrate (210), and the vapor pressure (P) of the positively charged material. T Vap ), vacuum level (P) of the deposition chamber (100) Cham Considering the heating temperature (T) of the deposition substrate (210) and the re-evaporation rate value (J) of the positively charged material re-evaporated on the deposition substrate (210) T Vap The method may include the step of obtaining ) and the step of deriving a heating temperature (T) range of the deposition substrate (210) such that the re-evaporation rate value of the obtained positively charged material is greater than the deposition rate value of the obtained positively charged material.

[0089] Adsorption rate of cationic substances (J Abs If ) is greater than 0, the positively charged material is adsorbed onto the substrate surface, and the adsorption rate of the positively charged material (J Abs If ) is less than 0, the positively charged material cannot be adsorbed onto the substrate surface and exists in a gaseous state. That is, when the adhesion coefficient of the deposition substrate, the vapor pressure of the positively charged material, and the chamber pressure are determined, the heating temperature of the deposition substrate (210) is controlled to control the adsorption rate (J) of the positively charged material. Abs The size and sign of ) can be controlled.

[0090] In other words, the step (S120) of deriving the heating temperature range above is the adsorption rate (J of the positively charged substance). Abs The step may be to find a heating temperature range of the deposition substrate (210) such that ) is less than 0.

[0091] Additionally, in the deposition step (S100), the chalcogenide compound thin film may include at least one material selected from a chalcogenide compound of saturated composition and a chalcogenide compound of unsaturated composition.

[0092] Specifically, the chalcogenide compound thin film may comprise 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.

[0093] In addition, in the deposition step (S100), the chalcogenide-based compound thin film may be composed of a single layer or multiple layers.

[0094] Specifically, in a method (S10) for manufacturing a chalcogenide-based compound thin film according to one embodiment of the present invention, the deposition step (S100) may be repeated multiple times, and for example, different raw materials 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 materials.

[0095] Accordingly, through the present invention, two or more chalcogenide-based compound thin films having different compositions can be stacked, that is, a chalcogenide-based compound thin film consisting of multiple layers can be obtained.

[0096] FIG. 3 is a diagram briefly illustrating a chalcogenide-based compound thin film according to one embodiment of the present invention.

[0097] Figure 3a) is a 3D schematic diagram of TMDC, and Figure 3b) is a diagram showing the composition ratios that can be formed through the combination of each element in the periodic table showing positive and chalcogen elements.

[0098] Referring to FIG. 3a), the chalcogenide-based 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 properties such as semimetal and semiconductor depending on the combination of the transition metal and chalcogen.

[0099] Most TMDCs have a two-dimensional layered structure, and the bonds between layers can be maintained through weak van der Waals bonds. Due to these weak bond energies, they can be easily separated into two-dimensional sheets, and the band gap can be easily adjusted based on the number of layers.

[0100] In particular, semiconductor TMDCs such as MoS2 and WSe2 have higher carrier mobility than conventional silicon and have a thin thickness of several nanometers, so research is actively being conducted on them as next-generation semiconductor devices.

[0101] Referring to Fig. 3b), it can be seen that chalcogen compounds of various combinations and compositional ratios can be formed. Specifically, it shows that various combinations can be formed between chalcogen elements indicated by an orange background and positronic elements with a blue background. It can be seen that the synthesis of various compositions is possible by indicating the chalcogen compounds that can be formed depending on the type of positronic element in light blue for a 1:1 composition, red for a 1:2 composition, and blue for a 2:3 composition above each positronic element.

[0103] The present invention will be described in more detail below through drawings and embodiments, but the present invention is not limited thereto.

[0105] Example 1: Chalcogenide compound thin film (TiSe 2 Manufacture of ) 1

[0106] A simultaneous deposition apparatus was prepared comprising a deposition chamber, a deposition rotating part equipped with a deposition substrate, an e-beam evaporation part, a thermal evaporation part, and a deposition sensor.

[0107] Afterwards, the vacuum level inside the deposition chamber is 10 -6 The temperature was maintained at Torr, the heating temperature of the deposition substrate was maintained at 500℃, and the beam evaporator and thermal evaporator were operated to evaporate the positively charged material Ti and the chalcogen material Se, and the deposition rate ratio of the said Ti and the said Se was satisfied at 1:2.

[0108] Here, the deposition substrate is a 4-inch silicon (Si) substrate.

[0109] In addition, the deposition rate of the thin film was set to satisfy 3.4 nm / min, and the film was deposited for 7 minutes and 30 seconds to obtain a chalcogenide compound thin film having a TiSe2 composition (Example 1).

[0111] Example 2: Chalcogenide compound thin film (NiSe 2 Manufacturing of ) 2

[0112] A simultaneous deposition apparatus was prepared comprising a deposition chamber, a deposition rotating part equipped with a deposition substrate, an e-beam evaporation part, a thermal evaporation part, and a deposition sensor.

[0113] Afterwards, the vacuum level inside the deposition chamber is 10 -6 The temperature was maintained at Torr, the heating temperature of the deposition substrate was maintained at 200°C, and the beam evaporator and thermal evaporator were operated to evaporate the positively charged material Ni and the chalcogenide material Se, and the deposition rate ratio of Ni and Se was satisfied to be 1:2.

[0114] Here, the deposition substrate is a 4-inch silicon (Si) / silicon oxide (SiO2) substrate.

[0115] In addition, the deposition rate of the thin film was set to satisfy 1.75 nm / min, and the film was deposited for 23 minutes to obtain a chalcogenide compound thin film having a NiSe2 composition (Example 2).

[0117] Example 3: Chalcogenide compound thin film (Bi 2 Se 3 Manufacturing 3 of )

[0118] A simultaneous deposition apparatus was prepared comprising a deposition chamber, a deposition rotating part equipped with a deposition substrate, an e-beam evaporation part, a thermal evaporation part, and a deposition sensor.

[0119] Afterwards, the vacuum level inside the deposition chamber is 10 -6 The temperature was maintained at Torr, the heating temperature of the deposition substrate was maintained at 15℃, 100℃, or 200℃, and the beam evaporator and thermal evaporator were operated to evaporate the positively charged material Bi and the chalcogenide material Se, and the deposition rate ratio of the Bi and Se was satisfied to be 2:3.

[0120] Here, the deposition substrate is an aluminum oxide (Al2O3) substrate or a silicon (Si) / silicon oxide (SiO2) substrate.

[0121] In addition, a chalcogenide compound thin film having a Bi2Se3 composition was obtained by depositing for 7 minutes to satisfy a thin film deposition rate of 4.7 nm / min (Example 3).

[0122] Here, the thin film obtained by using an Al2O3 substrate and maintaining the heating temperature of the deposition substrate at 15℃ 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℃ 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℃ is Sample C of Example 3.

[0123] In addition, the thin film obtained by using a SiO2 substrate and maintaining the heating temperature of the deposition substrate at 15℃ is Sample D of Example 3, the thin film obtained by using a SiO2 substrate and maintaining the heating temperature of the deposition substrate at 100℃ is Sample E of Example 3, and the thin film obtained by using a SiO2 substrate and maintaining the heating temperature of the deposition substrate at 200℃ is Sample F of Example 3.

[0125] Example 4: Chalcogenide compound thin film (Bi 4 Se 3 Manufacturing 4 of )

[0126] A simultaneous deposition apparatus was prepared comprising a deposition chamber, a deposition rotating part equipped with a deposition substrate, an e-beam evaporation part, a thermal evaporation part, and a deposition sensor.

[0127] Afterwards, the vacuum level inside the deposition chamber is 10 -6 The temperature was maintained at Torr, the heating temperature of the deposition substrate was maintained at 200℃, and the beam evaporator and thermal evaporator were operated to evaporate the positively charged material Bi and the chalcogenide material Se, and the deposition rate ratio of the Bi and Se was satisfied at 4:3.

[0128] Here, the deposition substrate is an aluminum oxide (Al2O3) substrate, a silicon (Si) substrate, or a silicon (Si) / silicon oxide (SiO2) substrate.

[0129] In addition, the deposition rate of the thin film was set to satisfy 6.85 nm / min, and the film was deposited for 3 minutes and 40 seconds to obtain a chalcogenide compound thin film having a Bi4Se3 composition (Example 4).

[0131] Example 5: Chalcogenide compound thin film (Bi 2 Te 3 Manufacturing 5 of )

[0132] A simultaneous deposition apparatus was prepared comprising a deposition chamber, a deposition rotating part equipped with a deposition substrate, an e-beam evaporation part, a thermal evaporation part, and a deposition sensor.

[0133] Afterwards, the vacuum level inside the deposition chamber is 10 -6 The temperature was maintained at Torr, the heating temperature of the deposition substrate was maintained at 15℃, 100℃, or 200℃, and the beam evaporator and thermal evaporator were operated to evaporate the positively charged material Bi and the chalcogenide material Te, and the deposition rate ratio of the Bi and Te was satisfied to be 2:3.

[0134] Here, the deposition substrate is an aluminum oxide (Al2O3) substrate or a silicon (Si) / silicon oxide (SiO2) substrate.

[0135] In addition, a chalcogenide compound thin film having a Bi2Te3 composition was obtained by depositing for 8 minutes and 20 seconds to satisfy a thin film deposition rate of 5.52 nm / min (Example 5).

[0136] Here, the thin film obtained by using an Al2O3 substrate and maintaining the heating temperature of the deposition substrate at 15℃ 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℃ 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℃ is Sample C of Example 5.

[0137] In addition, the thin film obtained by using a SiO2 substrate and maintaining the heating temperature of the deposition substrate at 15℃ is Sample D of Example 5, the thin film obtained by using a SiO2 substrate and maintaining the heating temperature of the deposition substrate at 100℃ is Sample E of Example 5, and the thin film obtained by using a SiO2 substrate and maintaining the heating temperature of the deposition substrate at 200℃ is Sample F of Example 5.

[0139] Example 6: Chalcogenide compound thin film (Cu 2 Preparation of Te) 6

[0140] A simultaneous deposition apparatus was prepared comprising a deposition chamber, a deposition rotating part equipped with a deposition substrate, an e-beam evaporation part, a thermal evaporation part, and a deposition sensor.

[0141] Afterwards, the vacuum level inside the deposition chamber is 10 -6 The temperature was maintained at Torr, the heating temperature of the deposition substrate was maintained at 100°C, and the beam evaporator and thermal evaporator were operated to evaporate the positively charged material Cu and the chalcogenide material Te, and the deposition rate ratio of the Cu and Te was satisfied at 2:1.

[0142] Here, the deposition substrate is an aluminum oxide (Al2O3) substrate or a silicon (Si) / silicon oxide (SiO2) substrate.

[0143] In addition, the deposition rate of the thin film was set to satisfy 10.2 nm / min, and the film was deposited for 10 minutes and 30 seconds to obtain a chalcogenide compound thin film having a Cu2Te composition (Example 6).

[0145] Example 7: Chalcogenide compound thin film (MoSe 2 Manufacturing 7 of )

[0146] A simultaneous deposition apparatus was prepared comprising a deposition chamber, a deposition rotating part equipped with a deposition substrate, an e-beam evaporation part, a thermal evaporation part, and a deposition sensor.

[0147] Afterwards, the vacuum level inside the deposition chamber is 10 -6The temperature was maintained at Torr, the heating temperature of the deposition substrate was maintained at 200°C, and the beam evaporator and thermal evaporator were operated to evaporate Mo, a positively charged material, and Se, a chalcogenide material, and the deposition rate ratio of Mo and Se was satisfied at 1:2.

[0148] Here, the deposition substrate is an aluminum oxide (Al2O3) substrate, a silicon (Si) / silicon oxide (SiO2) substrate, or a germanium (Ge) / graphene (Gr) substrate.

[0149] In addition, the deposition rate of the thin film was set to satisfy 0.69 nm / min, and the film was deposited for 11 minutes and 40 seconds to obtain a chalcogenide compound thin film having a MoSe2 composition (Example 7).

[0151] Example 8: Double-layer chalcogenide compound thin film (TiSe 2 / SnSe 2 Manufacturing of )

[0152] A simultaneous deposition apparatus was prepared comprising a deposition chamber, a deposition rotating part equipped with a deposition substrate, an e-beam evaporation part, a thermal evaporation part, and a deposition sensor.

[0153] Afterwards, the vacuum level inside the deposition chamber is 10 -6 The temperature was maintained at Torr, the heating temperature of the deposition substrate was maintained at 500℃, and the beam evaporator and thermal evaporator were operated to evaporate the positively charged material Ti and the chalcogen material Se, and the deposition rate ratio of the said Ti and the said Se was satisfied at 1:2.

[0154] Here, the deposition substrate is an aluminum oxide (Al2O3) substrate.

[0155] In addition, a chalcogenide compound thin film with a TiSe2 composition was synthesized by depositing for 13 minutes to satisfy a thin film deposition rate of 0.84 nm / min.

[0156] Afterwards, the vacuum level inside the deposition chamber is 10 -6The temperature was maintained at Torr, the heating temperature of the deposition substrate was maintained at 200°C or 300°C, and the beam evaporator and thermal evaporator were operated to evaporate Sn, a positively charged material, and Se, a chalcogenide material, and the deposition rate ratio of Sn and Se was satisfied at 1:2.

[0157] 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).

[0158] 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.

[0160] Experimental Example 1: Crystal Growth Analysis

[0161] In a method for manufacturing a chalcogenide-based compound thin film according to one embodiment of the present invention, in order to confirm the crystal growth of the chalcogenide-based compound thin film (TiSe2) according to Example 1, physical analysis, XRD analysis, and XRR analysis were performed, and the results are shown in FIG. 4.

[0162] Figure 4 is the result of the characteristic evaluation of a chalcogenide-based compound thin film according to Example 1 of the present invention.

[0163] Figure 4a) is a real photograph of a chalcogenide-based compound thin film (TiSe2) according to Example 1, Figure 4b) is the XRD analysis result for each point of the chalcogenide-based compound thin film (TiSe2) according to Example 1, Figure 4c) is a superimposed diagram of the XRD graph for each point of the chalcogenide-based compound thin film (TiSe2) according to Example 1, and Figure 4d) is the XRR analysis result for each point of the chalcogenide-based compound thin film (TiSe2) according to Example 1.

[0164] As shown in Fig. 4, a TiSe2 thin film with a thickness of about 25 nm was obtained by simultaneous deposition on a 4-inch silicon (Si) substrate. It was confirmed that the TiSe2 thin film grew into a vdW layered structure along the ab-plane.

[0165] In addition, looking at the superimposed XRD graph, it is confirmed to be within a 5% error range, so it is determined that it was deposited homogeneously.

[0166] In addition, looking at the superimposed XRR graph, it was confirmed that the thickness at point 1 was 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, and it was confirmed that they were within a 3% margin of error.

[0168] Experimental Example 2: XPS Analysis, Work Function-Hole Concentration Analysis

[0169] In a method for manufacturing a chalcogenide-based compound thin film according to one embodiment of the present invention, physical analysis, XRD analysis, XPS analysis, and hole concentration analysis were performed on a chalcogenide-based compound thin film (NiSe2) according to Example 2, and the results are shown in FIG. 5.

[0170] Figure 5 is the result of the characteristic evaluation of a chalcogenide-based compound thin film according to Example 2 of the present invention.

[0171] FIG. 5a) is a real photograph of a patterned chalcogenide compound thin film (NiSe2) according to Example 2, FIG. 5b) is the XRD analysis result of the chalcogenide compound thin film (NiSe2) according to Example 2, FIG. 5c) is the full-region XPS analysis result of the chalcogenide compound thin film (NiSe2) according to Example 2, FIG. 5d) is the oxygen region XPS analysis result of the chalcogenide compound thin film (NiSe2) according to Example 2, FIG. 5e) is a graph showing the hole concentration verified through repeated measurements of the chalcogenide compound thin film (NiSe2) according to Example 2, and FIG. 5f) is a diagram showing the work function-hole concentration comparison result of the chalcogenide compound thin film (NiSe2) according to Example 2.

[0172] As shown in Fig. 5, a NiSe2 thin film with a preset pattern was obtained by simultaneous deposition on a 4-inch silicon (Si) / silicon oxide (SiO2) substrate, and since the NiSe2 thin film was found to be within the error range of a hole concentration of 3.39%, a resistivity of 0.42%, and a thickness of 2.52%, it is determined that it was deposited homogeneously.

[0173] In addition, XRD analysis confirmed that polycrystalline NiSe2 was successfully grown.

[0174] Furthermore, XPS analysis results confirmed that no elements other than Ni and Se, which participated in the bonding, were identified, and the detected trace amounts of oxygen were proven to be elements adsorbed on the surface rather than formed through bonding with the material, thereby confirming that no oxidation of NiSe2 occurred.

[0175] In addition, it was confirmed that it has the highest hole concentration among metals with a high work function.

[0176] Therefore, NiSe2 with excellent properties at low temperatures was synthesized as a result of the effects of the present invention.

[0178] Experimental Example 3: Crystal Growth and Electron Mobility Analysis

[0179] In a method for manufacturing a chalcogenide-based compound thin film according to one embodiment of the present invention, XRD analysis, electron mobility analysis, and SEM analysis were performed on a chalcogenide-based compound thin film (Bi2Se3) according to Example 3, and the results are shown in FIG. 6.

[0180] Figure 6 is the result of the characteristic evaluation of a chalcogenide-based compound thin film according to Example 3 of the present invention.

[0181] FIG. 6a) shows the XRD analysis results of chalcogenide compound thin films (Bi2Se3) according to samples A, B, and C of Example 3 at different heating temperatures; FIG. 6b) shows the XRD analysis results of chalcogenide compound thin films (Bi2Se3) according to samples D, E, and F of Example 3 at different heating temperatures; FIG. 6c) shows the electron mobility analysis results of chalcogenide compound thin films (Bi2Se3) according to samples A, B, and C of Example 3 at different heating temperatures; FIG. 6d) shows the electron mobility analysis results of chalcogenide compound thin films (Bi2Se3) according to samples D, E, and F of Example 3 at different heating temperatures; FIG. 6e) shows the SEM analysis results of the chalcogenide compound thin film (Bi2Se3) according to sample C of Example 3; and FIG. 6f) shows the SEM of the chalcogenide compound thin film (Bi2Se3) according to sample F of Example 3. This is the analysis result.

[0182] As shown in Fig. 6, it was confirmed that high crystallinity and excellent mobility of the Bi2Se3 thin film can be achieved at an optimal temperature of 200°C on an Al2O3 substrate.

[0183] Specifically, XRD confirmed that the Bi2Se3 thin film exhibited the best crystallinity at 200°C on an Al2O3 substrate, and Hall measurements confirmed that it had the highest carrier mobility at 200°C on Al2O3. Additionally, SEM surface analysis confirmed that the surface roughness of the chalcogenide compound thin film (Bi2Se3) grown on an Al2O3 substrate was low at 200°C. Accordingly, it was confirmed that the finally obtained chalcogenide compound thin film (Bi2Se3) had the best quality at 200°C on an Al2O3 substrate.

[0185] Experimental Example 4: Crystal Growth Analysis

[0186] In a method for manufacturing a chalcogenide-based compound thin film according to one embodiment of the present invention, XRD analysis was performed to confirm the crystal growth of the chalcogenide-based compound thin film (Bi4Se3) according to Example 4, and the results are shown in FIG. 7.

[0187] Figure 7 is the result of the characteristic evaluation of a chalcogenide-based compound thin film according to Example 4 of the present invention.

[0188] Figure 7a) shows the XRD analysis results for each substrate of the chalcogenide compound thin film (Bi4Se3) according to Example 4, and Figure 7b) is an enlarged view of the 5-10 degree region of the Al2O3 substrate in the XRD graph of the chalcogenide compound thin film (Bi4Se3) according to Example 4.

[0189] As shown in Fig. 7, a Bi4Se3 thin film with a thickness of about 35 nm was obtained by simultaneously depositing it on an 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 into a vdW layered structure along the ab-plane.

[0190] In addition, a repeating periodic pattern (laue oscillation) was observed at 6–8 degrees, confirming that epitaxial growth had occurred.

[0192] Experimental Example 5: Crystal Growth and Electron Mobility Analysis

[0193] In a method for manufacturing a chalcogenide-based compound thin film according to one embodiment of the present invention, XRD analysis and electron mobility analysis were performed on a chalcogenide-based compound thin film (Bi2Te3) according to Example 5, and the results are shown in FIG. 8.

[0194] Figure 8 is the result of the characteristic evaluation of a chalcogenide-based compound thin film according to Example 5 of the present invention.

[0195] FIG. 8a) shows the XRD analysis results of chalcogenide compound thin films (Bi2Te3) according to samples A, B, and C of Example 5 at different heating temperatures, FIG. 8b) shows the XRD analysis results of chalcogenide compound thin films (Bi2Te3) according to samples A, B, and C of Example 5 at different heating temperatures, FIG. 8c) shows the electron mobility analysis results of chalcogenide compound thin films (Bi2Te3) according to samples D, E, and F of Example 5 at different heating temperatures, and FIG. 8d) shows the electron mobility analysis results of chalcogenide compound thin films (Bi2Te3) according to samples D, E, and F of Example 5 at different heating temperatures.

[0196] As shown in Fig. 8, it was confirmed that high mobility of the Bi2Te3 thin film on an Al2O3 substrate can be achieved at an optimal temperature of 200°C.

[0197] Specifically, XRD confirmed that the Bi2Te3 thin film exhibited the best crystallinity at 200°C on an Al2O3 substrate, and Hall measurements confirmed that it had the highest carrier mobility at 200°C on Al2O3. However, mobility could not be properly measured when synthesized at 15°C on a SiO2 substrate. Accordingly, it was confirmed that the finally obtained chalcogenide compound thin film (Bi2Te3) had the best quality at 200°C on an Al2O3 substrate.

[0199] Experimental Example 6: Crystal Growth Analysis

[0200] In a method for manufacturing a chalcogenide-based compound thin film according to one embodiment of the present invention, XRD analysis and SEM analysis were performed to confirm the crystal growth of the chalcogenide-based compound thin film (Cu2Te) according to Example 6, and the results are shown in FIG. 9.

[0201] Figure 9 is the result of the characteristic evaluation of a chalcogenide-based compound thin film according to Example 6 of the present invention.

[0202] Figure 9a) shows the XRD analysis results of the chalcogenide compound thin film (Cu2Te) according to Example 6 for each substrate, and Figure 9b) shows the SEM analysis results of the chalcogenide compound thin film (Cu2Te) synthesized on a SiO2 substrate according to Example 6.

[0203] As shown in Fig. 9, a Cu2Te thin film with a thickness of about 108.7 nm was obtained by simultaneously depositing it on aluminum oxide (Al2O3) and silicon (Si) / silicon oxide (SiO2) substrates. It was confirmed that the Cu2Te thin film has excellent quality with high crystallinity on the aluminum oxide (Al2O3) substrate.

[0205] Experimental Example 7: Crystal Growth Analysis

[0206] In a method for manufacturing a chalcogenide-based compound thin film according to one embodiment of the present invention, XRD analysis, Phi scan analysis, and SEM analysis were performed to confirm the crystal growth of the chalcogenide-based compound thin film (MoSe2) according to Example 7, and the results are shown in FIG. 10.

[0207] Figure 10 is the result of the characteristic evaluation of a chalcogenide-based compound thin film according to Example 7 of the present invention.

[0208] FIG. 10a) is the XRD analysis result of the chalcogenide compound thin film (MoSe2) according to Example 7 for each substrate, FIG. 10b) is the Phi scan analysis result of the chalcogenide compound thin film (MoSe2) synthesized on a Ge / Gr substrate according to Example 7, FIG. 10c) is the SEM analysis result of the chalcogenide compound thin film (MoSe2) synthesized on a Ge / Gr substrate according to Example 7, and FIG. 10d) is the SEM analysis result of the chalcogenide compound thin film (MoSe2) synthesized on a SiO2 substrate according to Example 7.

[0209] As shown in Fig. 10, a MoSe2 thin film with a thickness of about 8 nm was obtained by simultaneously depositing it on an aluminum oxide (Al2O3) substrate, a silicon (Si) / silicon oxide (SiO2) substrate, or a germanium (Ge) / graphene (Gr) substrate. It was confirmed that the MoSe2 thin film exhibited excellent crystal growth with very high crystallinity on the germanium (Ge) / graphene (Gr) substrate, but high surface roughness was observed. On the silicon (Si) / silicon oxide (SiO2) substrate, it was confirmed that the film had excellent quality with low surface roughness along with excellent crystallinity despite the low thickness of 8 nm.

[0211] Experimental Example 8: Crystal Growth Analysis

[0212] In a method for manufacturing a chalcogenide-based compound thin film according to one embodiment of the present invention, in order to confirm the crystal growth of a double-layer chalcogenide-based 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.

[0213] Figure 11 is the result of the characteristic evaluation of a chalcogenide-based compound thin film according to Example 8 of the present invention.

[0214] FIG. 11a) is the XRD analysis result of a chalcogenide compound thin film (TiSe2 / SnSe2) according to Sample A in Example 8, FIG. 11b) is the in-plane XRD analysis result of a chalcogenide compound thin film (TiSe2 / SnSe2) according to Sample A in Example 8, FIG. 11c) is the cross-section TEM analysis result of a chalcogenide compound thin film (TiSe2 / SnSe2) according to Sample A in Example 8, FIG. 11d) is the cross-section TEM analysis result of a chalcogenide compound thin film (TiSe2 / SnSe2) according to Sample B in Example 8, FIG. 11e) is the XRR analysis result of a chalcogenide compound thin film (TiSe2 / SnSe2) according to Sample A in Example 8, FIG. 11f) is the XRR analysis result of a chalcogenide compound thin film (TiSe2 / SnSe2) according to Sample B in Example 8.

[0215] As shown in Fig. 11, it was confirmed that heteroepitaxial growth of TiSe2 / SnSe2 thin films can be achieved at an optimal temperature of 200°C.

[0216] Specifically, an additional SnSe2 thin film was epitaxially grown on an epitaxially grown TiSe2 thin film, and the epitaxial orientation was confirmed via In-Plane XRD, confirming that the epitaxial growth consisted of vdW bonding between the two layers. In addition, it was confirmed via TEM and XRR that a clear epitaxial interface was present at 200°C. Accordingly, it was confirmed that the finally obtained double-layer chalcogenide compound thin film (TiSe2 / SnSe2) exhibited the best quality at 200°C.

[0218] Although a method for manufacturing a chalcogenide-based compound thin film according to an embodiment of the present invention has been described above as a specific embodiment, this is merely illustrative and the present invention is not limited thereto, and should be interpreted as having the broadest scope in accordance with the basic concept disclosed in this specification. Those skilled in the art may implement unspecified embodiments by combining or substituting the disclosed embodiments, and this also does not deviate from the scope of the present invention. Furthermore, those skilled in the art may easily change or modify the embodiments disclosed based on this specification, and it is evident that such changes or modifications also fall within the scope of the present invention. Explanation of the symbols

[0219] 10: Simultaneous deposition apparatus 100: Deposition chamber section 200: Deposition rotating part 210: Deposition substrate 300: E-beam evaporator 400: Heat evaporator

Claims

Claim 1 A method for manufacturing a chalcogenide-based compound thin film using a simultaneous deposition apparatus comprising: a deposition chamber section maintaining a preset vacuum level; a deposition rotating section disposed within the deposition chamber section and equipped with a deposition substrate; an E-beam evaporation section disposed within the deposition chamber section and evaporating a positively charged material which is a raw material; a thermal evaporation section disposed within the deposition chamber section and evaporating a chalcogenide material which is a raw material; and a deposition sensor sensing the deposition amount and deposition rate of the positively charged material and chalcogenide material deposited on the deposition substrate; wherein the method comprises a deposition step of simultaneously depositing a positively charged material and a chalcogenide material on the deposition substrate through a simultaneous deposition process utilizing the simultaneous deposition apparatus to obtain a chalcogenide-based compound thin film having a preset composition; wherein the deposition step comprises a deposition substrate heating process that heats the deposition substrate to satisfy a heating temperature range of 20 to 200°C to re-evaporate residual raw materials. A method for manufacturing a chalcogenide-based compound thin film, comprising: a re-evaporation step; further comprising, wherein the deposition step further comprises, prior to the re-evaporation step, a step of deriving a heating temperature range for performing a heating process of the deposition substrate; wherein the step of deriving the heating temperature range comprises: a step of obtaining a deposition rate value of a chalcogenide material deposited on the deposition substrate through the deposition sensor; a step of obtaining a re-evaporation rate value of a chalcogenide material re-evaporated on the deposition substrate by considering the adhesion coefficient of the deposition substrate, the vapor pressure of the chalcogenide material, the vacuum degree 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 such that the obtained re-evaporation rate value of the chalcogenide material is greater than the obtained deposition rate value of the chalcogenide material. Claim 2 A method for manufacturing a chalcogenide compound thin film according to claim 1, wherein in the deposition step, the positively charged material is at least one material selected from the group consisting of Ti, Ni, Cu, Ge, Mo, Sn, Sb, and Bi, the chalcogenide material is at least one material selected from the group consisting of S, Se, and Te, and the positively charged material and the chalcogenide material are elemental materials composed of only one type of element. Claim 3 In claim 1, the deposition step is performed within the deposition chamber, wherein the vacuum level within the deposition chamber is 10 -6 ~ 10 -5 Method for manufacturing a chalcogenide compound thin film satisfying the Torr range. Claim 4 A method for manufacturing a chalcogenide-based compound thin film according to claim 1, wherein in the deposition step, the chalcogenide-based compound thin film is deposited to satisfy a deposition rate range of 0.3 to 60 nm / min. Claim 5 A method for manufacturing a chalcogenide-based compound thin film according to claim 1, wherein, in the deposition step, the composition of the chalcogenide-based compound thin film is selectively controlled by adjusting the deposition rate ratio of the positively charged material and the chalcogenide material, and the deposition rates of the positively charged material and the chalcogenide material satisfy a range of 0.05 to 10 Å / s. Claim 6 A method for manufacturing a chalcogenide-based compound thin film according to claim 5, wherein the deposition rate ratio of the positively charged material and the chalcogenide material is 1 to 7:1 to 4. Claim 7 delete Claim 8 delete Claim 9 A method for manufacturing a chalcogenide compound thin film using a simultaneous deposition apparatus comprising: a deposition chamber section maintaining a preset vacuum level; a deposition rotating section disposed within the deposition chamber section and equipped with a deposition substrate; an E-beam evaporation section disposed within the deposition chamber section and evaporating a positively charged material which is a raw material; a thermal evaporation section disposed within the deposition chamber section and evaporating a chalcogenide material which is a raw material; and a deposition sensor that senses the deposition amount and deposition rate of the positively charged material and the chalcogenide material deposited on the deposition substrate; wherein the method comprises a deposition step of simultaneously depositing a positively charged material and a chalcogenide material on the deposition substrate through a simultaneous deposition process using the simultaneous deposition apparatus to obtain a chalcogenide compound thin film having a preset composition; wherein, in the deposition step, the chalcogenide compound thin film comprises at least one material selected from a chalcogenide compound with a saturated composition and a chalcogenide compound with an unsaturated composition The chalcogenide compound thin film comprises, wherein the 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. Manufacturing method. Claim 10 A method for manufacturing a chalcogenide compound thin film according to claim 9, wherein in the deposition step, the chalcogenide compound thin film is composed of a single layer or multiple layers.

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