CN114808117A - Crystallization vulcanization method - Google Patents
Crystallization vulcanization method Download PDFInfo
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- CN114808117A CN114808117A CN202210243792.XA CN202210243792A CN114808117A CN 114808117 A CN114808117 A CN 114808117A CN 202210243792 A CN202210243792 A CN 202210243792A CN 114808117 A CN114808117 A CN 114808117A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
Abstract
The application relates to the field of material growth treatment, in particular to a crystallization and vulcanization method, which is characterized in that a material to be crystallized is placed in a sulfur atmosphere to be heated to a preset temperature so as to realize the crystallization and vulcanization of the material to be crystallized to obtain a crystallized material, wherein the material to be crystallized is a molybdenum-containing substance, and the sulfur atmosphere contains a gaseous organic sulfur source. The material to be crystallized is heated in the sulfur atmosphere of the organic sulfur source, so that the escape of sulfur can be reduced, sulfur vacancies in the crystallized crystal are filled, the crystallized material with few sulfur vacancy defects is obtained, and the pollution of other sulfur sources to the molybdenum disulfide crystal, such as sulfur powder, is also avoided; meanwhile, the organic sulfur source has lower toxicity in the use process; the obtained crystalline material has high crystallization rate and crystal uniformity, and reduces crystal defects, thereby having good electrical properties including high conductivity.
Description
Technical Field
The application relates to the field of material growth treatment, in particular to a crystallization and vulcanization method.
Background
Compared with a two-dimensional layered material, the molybdenum disulfide has obvious advantages in many aspects such as physics, materials, electrons and the like. Molybdenum disulfide has a unique layered structure and properties that show great potential for nanoelectronic and optical applications, such as a band gap transition from an indirect band gap to a direct band gap when the size of molybdenum disulfide is reduced from three-dimensional to two-dimensional.
At normal temperature, the molybdenum disulfide is a metal luster black gray solid powder, the thermal stability is good, and the molybdenum disulfide can start to sublimate when the temperature reaches 450 ℃. In terms of chemical stability, molybdenum disulfide does not react in water and dilute acid, does not react in concentrated sulfuric acid, and shows very good stability. However, when molybdenum disulfide is put into heated concentrated sulfuric acid, reaction occurs to affect the structure. Due to the lack of the energy band gap, the application of the graphene on photoelectric devices becomes relatively narrow, and the molybdenum disulfide has the energy band gap which can be regulated, so that the molybdenum disulfide can be widely concerned and applied in various fields such as photoelectric devices and the like. In comparison with the three-dimensional bulk material, namely silicon material, molybdenum disulfide has an energy band gap and has a nanometer scale which is not possessed by the silicon material. These favorable conditions have allowed molybdenum disulfide to be used with great potential for the manufacture of smaller scale, more efficient electronic chips and semiconductors. The nano-scale organic light emitting diode is gradually dominant in the application of nano-electronic equipment in the future.
At present, the commonly used preparation methods of single crystal molybdenum disulfide mainly comprise a mechanical stripping method, a lithium ion intercalation method, a liquid phase ultrasonic method, an atomic layer deposition method (ALD), a chemical vapor deposition method (CVD) and the like. The mechanical stripping, the lithium ion intercalation method and the liquid phase ultrasonic method are all prepared by physical methods, and can prepare the molybdenum disulfide material with high crystallization quality, but the molybdenum disulfide material with high crystallization quality is difficult to prepare large-area materials. The ALD technology and the CVD technology can obtain a large-area molybdenum disulfide film, but the film with better crystallization quality needs to reduce the escape of sulfur element at high temperature so as to inhibit the generation of sulfur vacancy.
Currently, sulfur powder or hydrogen sulfide is mainly used as a sulfur source for treating molybdenum disulfide or molybdenum trioxide in vulcanization, so that a molybdenum disulfide material with high crystallization performance is obtained, but the sulfur powder is low in uniformity and many in product impurities in the vulcanization process; the hydrogen sulfide has high toxicity and has high potential safety hazard in the use process.
Disclosure of Invention
The application provides a crystallization and vulcanization method, which aims to solve the technical problem that the existing molybdenum disulfide is low in crystallinity.
In a first aspect, the present application provides a crystalline vulcanization process comprising the steps of:
and heating a material to be crystallized in a sulfur atmosphere to a preset temperature so as to realize crystallization and vulcanization of the material to be crystallized, thereby obtaining a crystallized material, wherein the material to be crystallized is a molybdenum-containing substance, and the sulfur atmosphere contains a gaseous organic sulfur source.
Optionally, the preset temperature is 50-1000 ℃.
Optionally, the preset temperature is 100-
Optionally, the vacuum degree during heating is 10 -5 -10 -2 torr。
Optionally, the organic sulfur source comprises at least one of 1, 3-propanedithiol, ethanedithiol, 1, 5-pentanethiol, ethanethiol, tert-butanethiol, and 2, 3-butanedithiol.
Optionally, the sulfur atmosphere comprises an inert gas.
Optionally, the control manner of the amount of the gaseous organic sulfur source in the sulfur atmosphere includes: the flow rate is controlled by a pulsed valve and/or by a carrier gas carrying the organosulfur source.
Optionally, the molybdenum-containing substance includes any one of molybdenum disulfide, molybdenum trioxide, and elemental molybdenum.
Optionally, the crystalline material is stored in a deoxygenated manner.
Compared with the prior art, the technical scheme provided by the embodiment of the application has the following advantages:
according to the method provided by the embodiment of the application, the material to be crystallized is placed in a sulfur atmosphere and heated to the preset temperature, and the material to be crystallized is heated in the sulfur atmosphere of an organic sulfur source, so that the escape of sulfur can be reduced, sulfur vacancies in the crystallized crystals are filled, the crystallized material with few sulfur vacancy defects is obtained, and the pollution of other sulfur sources to the crystals of molybdenum disulfide, such as sulfur powder, is also avoided; meanwhile, the organic sulfur source has lower toxicity in the use process; the obtained crystalline material has high crystallization rate and crystal uniformity, and reduces crystal defects, thereby having good electrical properties including high conductivity.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description, serve to explain the principles of the invention.
In order to more clearly illustrate the embodiments or technical solutions in the prior art of the present invention, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious for those skilled in the art to obtain other drawings without inventive labor.
FIG. 1 is an x-ray photoelectron spectrum of an embodiment of the present application;
FIG. 2 is an x-ray photoelectron spectrum of a comparative example of the present application;
FIG. 3 is a Raman spectrum of an example of the present application;
fig. 4 is a raman spectrum of a comparative example of the present application.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The present application provides a crystallization vulcanization method, comprising the steps of:
and heating a material to be crystallized in a sulfur atmosphere to a preset temperature so as to realize crystallization and vulcanization of the material to be crystallized, thereby obtaining a crystallized material, wherein the material to be crystallized is a molybdenum-containing substance, and the sulfur atmosphere contains a gaseous organic sulfur source.
Specifically, after the vulcanization treatment is finished, the sample is naturally cooled to room temperature and then taken out, and the crystalline material can be placed in a vacuum drying oven for later use, wherein the crystalline material is molybdenum disulfide or a molybdenum disulfide film.
In some embodiments, the predetermined temperature is 50 to 1000 ℃. Preferably, the preset temperature is 100-900 DEG C
In an embodiment of the application, the preset temperature is controlled to be 50-1000 ℃, the crystallization and vulcanization can be effectively promoted, the heating temperatures are controlled to be different according to different materials to be crystallized, for example, the material to be crystallized is molybdenum disulfide containing impurities, the heating temperature is controlled to be 800-950 ℃, the positive effect of improving the crystallinity is achieved, and if the temperature is not in the range, the adverse effect of reducing the crystallinity is achieved; if the material to be vulcanized is molybdenum trioxide, the heating temperature is controlled to be 700-950 ℃, the positive effect of vulcanization is achieved, and if the temperature is not in the range, the adverse effect of vulcanization is achieved.
In one embodiment of the present application, the material to be crystallized may be heated alone, the gas in the sulfur atmosphere may be heated, or both may be heated simultaneously.
In some embodiments, the vacuum during heating is 10 degrees f -5 -10 -2 torr。
In one embodiment of the present application, the positive effect of controlling the environment to be a vacuum environment during heating is to increase the diffusivity of the organic sulfur source and reduce the impurity content, and the vacuum degree is controlled to be 10 -5 -10 -2 the positive effect of the torr is to eliminate the interference of oxygen in the air; if the material to be crystallized is molybdenum disulfide containing oxygen impurity, controlling vacuum degree to be 10 -5 -10 -2 the positive effect of the torr is to reduce the interference of impurities in the air and has the function of sulfurationIf the degree of vacuum is out of this range, there is an adverse effect of increasing the oxygen content; if the material to be crystallized is molybdenum trioxide, controlling the vacuum degree to be 10 -5 -10 -2 the positive effect of torr is to eliminate the interference of oxygen in the air, with the positive effect of sulfidation, and with the negative effect of increasing oxygen content if the vacuum is not within this range.
In some embodiments, the organic sulfur source comprises at least one of 1, 3-propanedithiol, ethanedithiol, 1, 5-pentanethiol, ethanethiol, tert-butanethiol, and 2, 3-butanedithiol.
In one embodiment of the present application, 1, 3-propanedithiol, ethanedithiol, 1, 5-pentanethiol, etc. have saturated vapor pressures in the range of 1-5mmHg, and have a sufficiently positive effect on diffusion of crystallization vulcanization.
In one embodiment of the present application, the positive effect of controlling the concentration of the gaseous organic sulfur source in the sulfur atmosphere is to diffuse rapidly, increase the contact area with the sample, improve the vulcanization efficiency, and if the concentration is outside this range, have the adverse effect of insufficient vulcanization and reduced vulcanization efficiency.
In some embodiments, the sulfur atmosphere comprises an inert gas.
In some embodiments, the amount of gaseous organic sulfur source in the sulfur atmosphere is controlled in a manner comprising: the flow rate is controlled by a pulsed valve and/or by a carrier gas carrying the organosulfur source.
In one embodiment of the present application, the pulse valve may be an ALD pulse valve with a response speed of millisecond order. The pulse valve can be set to be 0.001-4s, and the sulfur source is briefly and discontinuously introduced into the chamber, so that the sulfur source is quickly diffused in the vacuum chamber to form a sulfur atmosphere environment; the sulfur source can enter the chamber through multiple pulses, and the amount of the gaseous organic sulfur source in the sulfur atmosphere can be controlled through the carrier gas flow bearing the organic sulfur source, so that the sulfur source can be rapidly diffused in the vacuum chamber, and the purpose of rapid and uniform vulcanization can be achieved.
In some embodiments, the molybdenum-containing element or the molybdenum compound comprises any one of molybdenum disulfide, molybdenum trioxide, and an element of molybdenum.
In one embodiment of the present application, any molybdenum containing compound can be used to crystallize the sulfide and yield a crystalline material.
In some embodiments, the crystalline material is stored in a deoxygenated storage.
In one embodiment of the present application, the final product, that is, molybdenum disulfide with high crystallinity, and conventional unsulfurized molybdenum disulfide is amorphous or polycrystalline, and contains a higher oxygen element, and since the electronegativity of the sulfur element is lower than that of the oxygen element, the sulfur element is easily oxidized in air, which causes an adverse effect of replacing the sulfur element with the oxygen element, and needs to be deoxidized for preservation during preservation.
The process of the present invention will be described in detail below with reference to examples, comparative examples and experimental data.
Example 1
The present application provides a crystallization vulcanization method, comprising the steps of:
and heating a material to be crystallized in a sulfur atmosphere to a preset temperature so as to realize crystallization and vulcanization of the material to be crystallized, thereby obtaining a crystallized material, wherein the material to be crystallized is a molybdenum-containing substance, and the sulfur atmosphere contains a gaseous organic sulfur source.
The method specifically comprises the following steps:
a. putting molybdenum disulfide containing impurities into a vulcanization chamber, vacuumizing the vulcanization chamber, and starting to heat a sample and the chamber, wherein the vacuum degree is 10 -5 -10 -2 torr；
b. Filling 1, 3-propanedithiol into a liquid source bottle in a glove box, placing the source bottle at room temperature, setting pulse time for 0.001-4s, and testing until the vapor pressure of each pulse is stable, wherein the 1, 3-propanedithiol is liquid at room temperature, but the saturated vapor pressure is higher and is 20mmHg at 25 ℃, so that heating is not needed for use, enough vapor pressure pulses enter a carrier gas system at room temperature, and finally, the carrier gas is transported to a vacuum vulcanization chamber.
c. And after the substrate temperature of the molybdenum disulfide reaches the preset value of 800-: 1, 3-propanedithiol is introduced into the vacuum vulcanization chamber in a pulse mode, and the pulse time is 1-4 s; the 1, 3-propanedithiol is freely diffused in the chamber to fill the whole chamber; waiting for 10-300s, reducing the concentration of the sulfur atmosphere in the chamber, and then pulsing 1, 3-propanedithiol again; the carrier gas flow is 10sccm, the vulcanization time is determined according to the thickness of the molybdenum disulfide film, and the control is carried out through the pulse time, the pulse times and the interval time.
Example 2
The present embodiment is different from embodiment 1 in that: the material to be sulfurized and crystallized is molybdenum trioxide.
Example 3
The present embodiment is different from embodiment 1 in that: the material to be vulcanized is a molybdenum simple substance.
Comparative example 1
The present embodiment is different from embodiment 1 in that: the sulfur source uses sulfur powder with the particle size of 500nm, has poor diffusion, so the vulcanization effect is poor and is not easy to control.
Comparative example 2
The present embodiment is different from embodiment 1 in that: the sulfur source uses hydrogen sulfide, and the diffusibility is good, so that the sulfur source has a good vulcanization effect, but the hydrogen sulfide is high in toxicity and high in cost.
Experimental detection
Examination of the vulcanized materials of examples and comparative examples and determination of the vulcanized materials of examples and comparative examples on X-ray photoelectron Spectroscopy (XPS) As shown in FIGS. 1 and 2, it can be seen that MoS vulcanized by the present method 2 The ratio of Mo to S elements of the samples is closer to 1: 2, and the content of O elements is far less than that of the comparative example group, which shows that the method of the application has the advantages of reducing impurity oxygen elements and improving MoS 2 The advantage of purity.
The crystalline materials of examples and comparative examples were examined by raman spectroscopy, and the crystalline properties of the examples were measured as shown in fig. 3; the crystalline properties of the comparative example are shown in fig. 4. In the figure, the example is at 385cm -1 And 406cm -1 There is a distinct characteristic peak, the comparative example has no distinct peak at the two beam positions, and the comparison shows thatThe crystallinity of the sample after vulcanization crystallization is improved.
In conclusion, the method performs crystallization and vulcanization treatment by using the organic sulfur source with better diffusivity, low toxicity or no toxicity, is simple to operate, and is beneficial to promoting the preparation, treatment and application of molybdenum disulfide; the molybdenum disulfide film treated by the crystallization and vulcanization method has good electrical properties, and reduces the crystal defects of the film
It is noted that, in this document, relational terms such as "first" and "second," and the like, may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The foregoing are merely exemplary embodiments of the present invention, which enable those skilled in the art to understand or practice the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. A crystalline vulcanization process characterized by the steps of:
and heating a material to be crystallized in a sulfur atmosphere to a preset temperature so as to realize crystallization and vulcanization of the material to be crystallized, thereby obtaining a crystallized material, wherein the material to be crystallized is a molybdenum-containing substance, and the sulfur atmosphere contains a gaseous organic sulfur source.
2. The method according to claim 1, wherein the preset temperature is 50-1000 ℃.
3. The method as claimed in claim 1, wherein the predetermined temperature is 100-900 ℃.
4. The method of claim 1, wherein the heating is performed at a vacuum level of 10% -5 -10 -2 torr。
5. The method of claim 1, wherein the organic sulfur source comprises at least one of 1, 3-propanedithiol, ethanedithiol, 1, 5-pentanethiol, ethanethiol, tert-butanethiol, and 2, 3-butanedithiol.
6. The method of claim 1, wherein the sulfur atmosphere comprises an inert gas.
7. The method of claim 1, wherein the amount of gaseous organic sulfur source in the sulfur atmosphere is controlled in a manner comprising: the flow rate is controlled by a pulsed valve and/or by a carrier gas carrying the organosulfur source.
8. The method according to claim 1, wherein the molybdenum-containing substance comprises any one of molybdenum disulfide, molybdenum trioxide and elemental molybdenum.
9. The method of claim 1, wherein the crystalline material is stored in a deoxygenated manner.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109378341A (en) * | 2018-09-20 | 2019-02-22 | 复旦大学 | A kind of molybdenum disulfide tunneling transistor and preparation method thereof |
| CN110747448A (en) * | 2019-11-04 | 2020-02-04 | 江南大学 | NbS grown by atomic layer deposition technologyxMethod for making thin film |
| CN111893456A (en) * | 2020-07-09 | 2020-11-06 | 清华-伯克利深圳学院筹备办公室 | Two-dimensional transition metal chalcogenide compound and preparation method and device thereof |
| CN113088932A (en) * | 2021-03-30 | 2021-07-09 | 天津理工大学 | Wafer-level molybdenum sulfide with controllable layer number and preparation method thereof |
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- 2022-03-10 CN CN202210243792.XA patent/CN114808117A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109378341A (en) * | 2018-09-20 | 2019-02-22 | 复旦大学 | A kind of molybdenum disulfide tunneling transistor and preparation method thereof |
| CN110747448A (en) * | 2019-11-04 | 2020-02-04 | 江南大学 | NbS grown by atomic layer deposition technologyxMethod for making thin film |
| CN111893456A (en) * | 2020-07-09 | 2020-11-06 | 清华-伯克利深圳学院筹备办公室 | Two-dimensional transition metal chalcogenide compound and preparation method and device thereof |
| CN113088932A (en) * | 2021-03-30 | 2021-07-09 | 天津理工大学 | Wafer-level molybdenum sulfide with controllable layer number and preparation method thereof |
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