CN117187763A - Binary compound preparation method - Google Patents
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- CN117187763A CN117187763A CN202311111610.4A CN202311111610A CN117187763A CN 117187763 A CN117187763 A CN 117187763A CN 202311111610 A CN202311111610 A CN 202311111610A CN 117187763 A CN117187763 A CN 117187763A
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- 150000001875 compounds Chemical class 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title abstract description 26
- 239000010408 film Substances 0.000 claims abstract description 148
- 239000000758 substrate Substances 0.000 claims abstract description 67
- 239000010409 thin film Substances 0.000 claims abstract description 44
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims description 35
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 239000010453 quartz Substances 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 238000005566 electron beam evaporation Methods 0.000 claims description 5
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 5
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 4
- 238000007747 plating Methods 0.000 claims description 3
- 230000008859 change Effects 0.000 abstract description 6
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 28
- 239000000463 material Substances 0.000 description 17
- 238000006243 chemical reaction Methods 0.000 description 13
- 230000015572 biosynthetic process Effects 0.000 description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 229910052723 transition metal Inorganic materials 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 238000010587 phase diagram Methods 0.000 description 4
- 239000011669 selenium Substances 0.000 description 4
- 230000007704 transition Effects 0.000 description 4
- 238000000576 coating method Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- -1 transition metal chalcogenide Chemical class 0.000 description 3
- 239000011364 vaporized material Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 150000001787 chalcogens Chemical group 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910052714 tellurium Inorganic materials 0.000 description 2
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 229910052798 chalcogen Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- XSOKHXFFCGXDJZ-UHFFFAOYSA-N telluride(2-) Chemical compound [Te-2] XSOKHXFFCGXDJZ-UHFFFAOYSA-N 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
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Abstract
The embodiment of the application provides a preparation method of a binary compound, which comprises the following steps: step S1: forming a first thin film and a second thin film on a substrate; step S2: the first film and the second film are subjected to chemical vapor deposition to generate binary compounds with different phase proportions, wherein in step S1, the content of the first film and the second film is controlled by the thickness of the first film and the second film, and in step S2, the generation of the binary compounds with different phase proportions is controlled by controlling the thickness proportion of the first film and the second film. The preparation method of the binary compound provided by the embodiment of the application can realize large-area controllable phase change of the binary compound.
Description
Technical Field
The application belongs to the technical field of semiconductor materials, and particularly relates to a preparation method of a binary compound.
Background
With the rapid development of modern electronic information technology, the silicon-based integrated circuit industry enters the "post-molar age", and the size miniaturization and performance improvement of transistors face various technical barriers, so that development and research on new materials and new processes are needed.
Two-dimensional semiconductor materials are one of the promising materials for the development of next-generation electronic and optoelectronic devices, and have the characteristics of atomic-level thickness, proper band gap, high mobility and the like. The preparation method of the two-dimensional transition metal chalcogenide mainly comprises a top-down path and a bottom-up path. The two-dimensional material is prepared by a physical or chemical synthesis method from bottom to top, wherein chemical vapor deposition is a mainstream two-dimensional material preparation method at present, and the two-dimensional material prepared by the chemical vapor deposition method has the advantages of wide synthesis range, controllable layer number, capability of realizing wafer-level size preparation and the like, and can be compatible with silicon base, thereby being a necessary material synthesis method in the next-generation semiconductor technology.
According to the phase diagram, many transition metal chalcogenides have rich phases, but are limited to common phases, and because of high requirements on temperature and element proportion, many phases do not realize controllable preparation.
Therefore, how to controllably prepare each phase in a material system by a chemical vapor deposition method is a problem to be solved in the current controllable phase growth of two-dimensional materials and large-area preparation.
Disclosure of Invention
Aiming at the problems in the related art, the application provides a preparation method of a binary compound, which can realize large-area controllable phase change of the binary compound.
Therefore, the embodiment of the application provides a preparation method of a binary compound, which comprises the following steps:
step S1: forming a first thin film and a second thin film on a substrate;
step S2: the first film and the second film generate binary compounds with different phase proportions by a chemical vapor deposition method,
wherein, in step S1, the content of the first film and the second film is controlled by the thickness of the first film and the second film, and in step S21, the generation of the binary compound with different phase ratios is controlled by controlling the thickness ratio of the first film and the second film.
In some embodiments, the step S1 includes: and generating the first film and the second film on the substrate by a magnetron sputtering method.
In some embodiments, the step S1 includes: the first thin film and the second thin film are formed on the substrate by an electron beam evaporation plating method.
In some embodiments, the step S2 includes: and placing the substrates for growing the first film and the second film into a quartz boat, and then placing the quartz boat into a tube furnace for chemical vapor deposition.
In some embodiments, the substrate includes a first substrate and a second substrate, and the step S1 includes: generating the first thin film on the first substrate and generating the second thin film on the second substrate, wherein the step S2 includes: and placing the first film generated on the first substrate above the second film generated on the second substrate, and generating binary compound films with different phase proportions by a chemical vapor deposition method through the first film and the second film.
In some embodiments, the substrate includes a conductive layer and an insulating layer, the conductive layer disposed over the insulating layer.
In some embodiments, the first film is a Te film and the second film is a Pd film.
In some embodiments, the first film is a Te film and the second film is a Mo film.
In some embodiments, the first film is a Se film and the second film is a Pd film.
In some embodiments, the substrate is a silicon/silicon oxide substrate.
According to the preparation method of the binary compound, the first film and the second film are generated on the substrate, the contents of two elements participating in the reaction are controlled by controlling the thickness proportion of the first film and the second film, and the generation of binary compounds with different phases can be controlled at the same reaction temperature, namely, the preparation method of the binary compound can realize large-area controllable phase change of the two-dimensional binary compound.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the related art, the drawings that are required to be used in the embodiments or the related technical descriptions will be briefly described, and it is apparent that the drawings in the following description are only some embodiments of the present application, and other drawings may be obtained from the structures shown in the drawings without inventive effort to those skilled in the art.
FIG. 1 is a schematic flow chart of a preparation method of a binary compound provided by an embodiment of the application;
FIG. 2 is a schematic diagram of a process for preparing a binary compound according to an embodiment of the present application;
fig. 3 is a schematic diagram of a simulated reaction of a method for preparing a binary compound according to the second embodiment of the present application.
The achievement of the objects, functional features and advantages of the present application will be further described with reference to the accompanying drawings, in conjunction with the embodiments.
Detailed Description
The following description of the embodiments of the present application will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
It should be understood that the terms "comprises" and "comprising," when used in this specification and the appended claims, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
It is also to be understood that the terminology used in the description of the application herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used in this specification and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art according to the specific circumstances.
In the existing preparation method of the binary compound, firstly, a two-dimensional Pd (palladium) film is grown on a substrate, and then a Te (tellurium) simple substance is taken as a tellurium source, and the palladium telluride film is formed on the substrate by a chemical vapor deposition method. However, from the phase diagram, pdTE is known 2 Is the material with the highest Te content in Pd-Te phase, other phases, such as Pd 9 Te 4 、Pd 20 Te 7 The Pd/Te amounts of PdTE and the like are smaller than that of PdTE 2 Moreover, the formation temperatures between the phases of Pd-Te are very close, and it is difficult to achieve controlled growth of the phases by controlling the temperatures individually. Therefore, how to control the trace Te to participate in the reaction, thereby obtaining other phases is needed to be solvedTechnical problems of (2).
Example 1
Accordingly, referring to fig. 1 and 2, an embodiment of the present application provides a method for preparing a binary compound, including:
step S1: forming a first thin film 102 and a second thin film 103 on a substrate 100;
step S2: the first film 102 and the second film 103 are formed into binary compound films with different phase ratios by a chemical vapor deposition method,
wherein, in step S1, the amounts of the first film 102 and the second film 103 are controlled by the thicknesses of the first film 102 and the second film 103; in step S2, the formation of binary compounds with different phase ratios is controlled by controlling the thickness ratio of the first film 102 and the second film 103.
Specifically, as shown in fig. 2, when the first film 102 and the second film 103 are formed on the substrate 101, the surface areas of the first film 102 and the second film 103 covered on the substrate 100 are equal, and therefore, the preparation method of the embodiment of the present application can control the contents of the first film 102 and the second film 103 by controlling the thicknesses of the first film 102 and the second film 103, respectively. The surface areas of the first film 102 and the second film 103 covered on the substrate 100 may be set according to specific needs.
As can be seen from the phase diagrams, the formation temperatures of the different phases of the binary compound are very close, and it is difficult to achieve controllable growth of the phases by controlling the temperatures alone, whereas in some embodiments according to the present application, the formation of the binary compound of the different phases can be controlled by controlling the contents of the two elements participating in the reaction by controlling the thickness of the first thin film 102 and the second thin film 103, i.e., the preparation method of the binary compound according to the embodiment of the present application can achieve a large-area controllable phase change of the two-dimensional binary compound.
The binary compounds mentioned above are typically transition metal sulfides (Transition Metal Dichalcogenides, TMDs), which are layered structures, similar to single-atomic-layer graphene structures, with two layers of chalcogen atoms sandwiching a layer of transition metal atoms to form a sandwich-like form (X-M-X)A layered structure. TMDs of the formula MX 2 M refers to a transition metal element, and X represents a chalcogen element (e.g., O, S, se, te, etc.).
It should be noted that the stacking sequence of the first film 102 and the second film 103 does not affect the preparation of the binary compound, that is, the first film 102 may be disposed above the second film 103, and the first film 102 may be disposed below the second film 103.
Further, step S1 includes: a first thin film 102 and a second thin film 103 are formed over a substrate 100 by a magnetron sputtering method. The magnetron sputtering method is far away from the target surface by utilizing interaction of a magnetic field and an electric field to enable electrons to spirally run near the target surface, so that the probability that the electrons strike argon to generate ions is increased, and the generated ions strike the target surface under the action of the electric field to sputter the target material. In some embodiments of the present application, the first thin film 102 is generated by a magnetron sputtering method, which has advantages of simple equipment, easy control, large coating area, strong adhesion, etc.
Further, step S1 includes: a first thin film 102 and a second thin film 103 are formed on a substrate 100 by an electron beam evaporation plating method. The electron beam evaporation coating method is a vacuum coating method, and solves the problem that the film material and the evaporation source material are in direct contact and easy to mix in a resistance heating mode. The vaporized material is heated by the electron beam to vaporize and transport the vaporized material to the substrate, and the vaporized material is condensed on the substrate to form a thin film. In some embodiments of the present application, the first film 102 is formed by an electron beam evaporation coating method, which has the advantage of providing higher heat for the material to be evaporated, so that the evaporation rate is also faster, the electron beam positioning is accurate, and evaporation and pollution of the crucible material can be avoided.
In some embodiments according to the application, step S2 comprises: the substrate 100 on which the first film 102 and the second film 103 are grown is placed in a quartz boat, and then the quartz boat is placed in a tube furnace for chemical vapor deposition. The tube furnace is usually an atmospheric tube furnace, so the binary compound is generated according to the method, the operation is simple, and the production cost is low.
Wherein the substrate 100 includes a conductive layer and an insulating layer, and the conductive layer is disposed over the insulating layer. The substrate 100 is the underlying material of all semiconductor chips and primarily serves the physical support, thermal and electrical conductivity. The structure of the mechanical support of the chip module needs to withstand different working environments, and needs to have enough thermal conductivity to quickly transfer out the heat generated by the chip and the like, and meanwhile, in a specific working environment, the substrate 100 has an electric conduction function, so that the substrate 100 can realize the physical support, heat conduction and electric conduction functions through the arrangement.
Furthermore, in some embodiments according to the application, the first film 102 is a Te film and the second film 103 is a Pd film. Therefore, in some embodiments according to the present application, the contents of two elements participating in the reaction are controlled by controlling the thickness of the Te thin film and the Pd thin film, that is, the generation of binary compounds of different phases can be controlled, that is, the preparation method of binary compounds according to embodiments of the present application can realize large-area controllable phase transition of two-dimensional binary compounds.
In particular, experimental data shows that, for example, when the Pd film thickness on the substrate 100 is 10nm, the Te film thickness is 18nm, and the Pd film is located above the Te film, the binary compound generated is PdTe; when the Pd film thickness on the substrate 100 is 20nm, the Te film thickness is 42nm, and the Pd film is positioned above the Te film, the binary compound is also PdTE; when the Pd film thickness on the substrate 100 is 10nm, the Te film thickness is 42nm, and the Pd film is located above the Te film, the binary compound is PdTE 2 The method comprises the steps of carrying out a first treatment on the surface of the When the Pd film thickness on the substrate 100 is 20nm, the Te film thickness is 12nm, and the Pd film is located above or below the Te film, the binary compound is Pd 20 Te 7 。
The above data are only used as examples, and in some embodiments of the present application, the contents of two elements participating in the reaction are controlled by controlling the thickness of the Te thin film and the Pd thin film, so that the generation of binary compounds with different phases can be controlled, that is, the preparation method of binary compounds according to the embodiments of the present application can realize large-area controllable phase change of two-dimensional binary compounds.
Further, the first film is a Te film, and the second film is a Mo (molybdenum) film. Therefore, in some embodiments according to the present application, the contents of two elements participating in the reaction are controlled by controlling the thickness of the Te thin film and the Mo thin film, that is, the generation of binary compounds of different phases can be controlled, that is, the preparation method of binary compounds according to embodiments of the present application can realize large-area controllable phase transition of two-dimensional binary compounds.
Further, the first film is a Se (selenium) film, and the second film is a Pd film. Therefore, in some embodiments according to the present application, the contents of two elements participating in the reaction are controlled by controlling the thickness of the Te thin film and the Se thin film, that is, the generation of binary compounds of different phases can be controlled, that is, the preparation method of binary compounds according to embodiments of the present application can realize large-area controllable phase transition of two-dimensional binary compounds.
In addition, the substrate 100 is a silicon/silicon oxide substrate, and the substrate 100 is a bottom material of all semiconductor chips, and mainly plays roles of physical support, heat conduction and electric conduction. The silicon/silicon oxide substrate can better meet the working requirements in terms of environmental resistance, heat conduction and electric conductivity.
Example two
Referring to fig. 3, which shows a schematic diagram of a simulated reaction of a method for preparing a binary compound according to a second embodiment of the present application, unlike the first embodiment described above, referring to fig. 3, a substrate 201 includes a first substrate 21 and a second substrate 22, and step S1 includes: a first thin film 202 is grown on the first substrate 21, and a second thin film 203 is grown on the second substrate 22, step S2 includes: the first film 202 formed on the first substrate 21 is placed over the second film 203 formed on the second substrate 22, and the first film 202 and the second film 203 are formed into binary compounds with different phase ratios by a chemical vapor deposition method.
Specifically, compared with the first embodiment, in the embodiment of the present application, by forming the first film 202 and the second film 203 on different substrates 21, 22, interference generated during the formation of the first film and the second film can be avoided, and the subsequent chemical vapor deposition reaction is affected, so that the formation of binary compounds with different phase ratios is further ensured.
Specifically, as shown in fig. 3, a first thin film 202 is formed on a first substrate 21, a second thin film 203 is formed on a second substrate 22, and the surface areas of the first thin film 202 and the second thin film 203 respectively covered on the substrates 21 and 22 are equal, so that the preparation method of the embodiment of the application can respectively control the content of the first thin film 202 and the second thin film 203 by controlling the thickness of the first thin film 202 and the second thin film 203. The surface area of the first film 202 and the second film 203 covered on the substrate 200 may be set according to specific needs.
As can be seen from the phase diagrams, the formation temperatures of the different phases of the binary compound are very close, and it is difficult to achieve controllable growth of the phases by controlling the temperatures alone, whereas in some embodiments according to the present application, the formation of the binary compound of the different phases can be controlled by controlling the contents of the two elements participating in the reaction by controlling the thickness of the first film 202 and the second film 203, i.e., the preparation method of the binary compound according to the embodiment of the present application can achieve large-area controllable phase transition of the two-dimensional binary compound.
For example, the film formed on the first substrate 21 is a Te film 202, the film formed on the second substrate 22 is a Pd film 203, the Te film 202 is disposed above the Pd film 203, and when the Pd film thickness is 20nm and the Te film thickness is 30nm, the binary compound formed is Pd 9 Te 4 。
The above data are only used as examples, and in some embodiments of the present application, the contents of two elements participating in the reaction are controlled by controlling the thickness of the Te thin film and the Pd thin film, so that the generation of binary compounds with different phases can be controlled, that is, the preparation method of binary compounds according to the embodiments of the present application can realize large-area controllable phase change of two-dimensional binary compounds.
While the application has been described with reference to certain preferred embodiments, it will be understood by those skilled in the art that various changes and substitutions of equivalents may be made and equivalents will be apparent to those skilled in the art without departing from the scope of the application. Therefore, the protection scope of the application is subject to the protection scope of the claims.
Claims (10)
1. A method for preparing a binary compound, comprising:
step S1: forming a first thin film and a second thin film on a substrate;
step S2: the first film and the second film generate binary compounds with different phase proportions by a chemical vapor deposition method,
wherein, in step S1, the content of the first film and the second film is controlled by the thickness of the first film and the second film, and in step S21, the generation of the binary compound with different phase ratios is controlled by controlling the thickness ratio of the first film and the second film.
2. The method according to claim 1, wherein the step S1 includes: and generating the first film and the second film on the substrate by a magnetron sputtering method.
3. The method according to claim 1, wherein the step S1 includes: the first thin film and the second thin film are formed on the substrate by an electron beam evaporation plating method.
4. A method according to any one of claims 1 to 3, wherein said step S2 comprises: and placing the substrates for growing the first film and the second film into a quartz boat, and then placing the quartz boat into a tube furnace for chemical vapor deposition.
5. The method of claim 4, wherein the substrate comprises a first substrate and a second substrate, and wherein the step S1 comprises: generating the first thin film on the first substrate and generating the second thin film on the second substrate, wherein the step S2 includes: and placing the first film generated on the first substrate above the second film generated on the second substrate, and generating the binary compound with different phase proportions by a chemical vapor deposition method through the first film and the second film.
6. The method of claim 5, wherein the substrate comprises a conductive layer and an insulating layer, the conductive layer disposed over the insulating layer.
7. The method of claim 6, wherein the first film is a Te film and the second film is a Pd film.
8. The method of claim 6, wherein the first film is a Te film and the second film is a Mo film.
9. The method of claim 6, wherein the first film is a Se film and the second film is a Pd film.
10. The method of any of claims 4 to 9, wherein the substrate is a silicon/silicon oxide substrate.
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| CN202311111610.4A CN117187763A (en) | 2023-08-30 | 2023-08-30 | Binary compound preparation method |
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| CN202311111610.4A CN117187763A (en) | 2023-08-30 | 2023-08-30 | Binary compound preparation method |
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