CN114457426B - Ti-doped monolayer molybdenum disulfide single crystal and preparation method and application thereof - Google Patents
Ti-doped monolayer molybdenum disulfide single crystal and preparation method and application thereof Download PDFInfo
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- CN114457426B CN114457426B CN202111389147.0A CN202111389147A CN114457426B CN 114457426 B CN114457426 B CN 114457426B CN 202111389147 A CN202111389147 A CN 202111389147A CN 114457426 B CN114457426 B CN 114457426B
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Abstract
The invention discloses a Ti-doped monolayer molybdenum disulfide single crystal and a preparation method and application thereof, wherein the preparation method comprises the following steps: preparing a quartz tube with two open ends, wherein the two ends of the quartz tube are respectively a raw material end and a substrate end, placing a substrate in the substrate end of the quartz tube, placing a raw material and a transport agent in the raw material end of the quartz tube, vacuumizing the quartz tube, and sealing the quartz tube to ensure that the pressure in the quartz tube is 10 ‑6 ～10 ‑3 And Pa, heating the raw material end and the substrate end of the quartz tube for 0.5-1 h simultaneously, cooling to room temperature of 20-25 ℃, and obtaining the Ti-doped monolayer molybdenum disulfide monocrystal on the substrate. The preparation method of the invention can ensure single-layer MoS 2 Realizing the single-layer MoS of transition element Ti on the premise of single crystal crystallization quality 2 Single crystal in-plane substitutional doping and MoS realization 2 A large increase in photoluminescence intensity.
Description
Technical Field
The invention belongs to the technical field of molybdenum disulfide single crystals, and particularly relates to a Ti-doped single-layer molybdenum disulfide single crystal and a preparation method and application thereof.
Background
Two-dimensional chalcogenide materials have great potential applications in flexible transistors, optoelectronic sensors, and information storage. However, the two-dimensional material has more intrinsic defect states, captures a large number of carriers, and has weak luminous efficiency, and the luminous performance of the two-dimensional material can be improved by selecting proper doping atoms under the condition of not changing the intrinsic band gap of the two-dimensional material.
However, the existing doping methods are not many, and the single-layer MoS cannot be maintained after doping 2 The single crystal has high crystallization quality, poor crystallinity, easy pollution and large interference from the outside.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a Ti-doped single-layer molybdenum disulfide single crystal, which can ensure single-layer MoS 2 On the premise of high crystallization quality of single crystal, the single-layer MoS is realized by Ti element 2 And realize MoS 2 The photoluminescence enhancement solves the problem of Ti-doped two-dimensional single-layer MoS 2 The technical problem is that the photoluminescence efficiency of the obtained Ti-doped monolayer molybdenum disulfide single crystal is greatly improved, and support is provided for realizing a high-performance photoelectric detector.
The purpose of the invention is realized by the following technical scheme.
A preparation method of a Ti-doped monolayer molybdenum disulfide single crystal comprises the following steps:
1) Preparing a quartz tube with two open ends, wherein the two ends of the quartz tube are respectively a raw material end and a substrate end, placing a substrate in the substrate end of the quartz tube, placing a raw material and a transport agent in the raw material end of the quartz tube, vacuumizing the quartz tube, and sealing the quartz tube to ensure that the pressure in the quartz tube is 10 -6 ～10 -3 Pa, wherein the raw material is MoO with the mass part of 1.5-2.5 3 0.36-0.42 mass portion of S powder and 0.2-1.0 mass portion of TiO 2 The transport agent is elemental iodine;
in the step 1), the substrate is mica or graphite.
In the step 1), the length of the quartz tube is 15-40 cm, and the inner diameter is 10-20mm.
In the step 1), the ratio of the raw material to the transport agent is (2-6) by mass: (3-8).
2) Simultaneously heating the raw material end and the substrate end of the quartz tube for 0.5-1 h, cooling to room temperature of 20-25 ℃, and obtaining the Ti-doped monolayer molybdenum disulfide monocrystal on the substrate, wherein the heating temperature of the raw material end is 750-900 ℃, and the heating temperature of the substrate end is 400-700 ℃.
In the step 2), the heating rate of heating to 750-900 ℃ is 25-50 ℃/min, and the heating rate of heating to 400-700 ℃ is 25-50 ℃/min.
In the step 2), the temperature gradient between the raw material end and the substrate end is 3-30 ℃/cm.
The Ti-doped monolayer molybdenum disulfide single crystal obtained by the preparation method.
The preparation method is applied to simultaneously realizing single-layer molybdenum disulfide photoluminescence enhancement and single-layer molybdenum disulfide single crystal preparation.
The preparation method of the invention can ensure single-layer MoS 2 Realizing the single-layer MoS of transition element Ti on the premise of single crystal crystallization quality 2 Single crystal in-plane substitutional doping and MoS realization 2 A large increase in photoluminescence intensity.
Drawings
FIG. 1 is an optical photograph of a Ti-doped single-layer molybdenum disulfide single crystal obtained in example 1, wherein a is the Ti-doped single-layer molybdenum disulfide single crystal obtained in example 2, b is the Ti-doped single-layer molybdenum disulfide single crystal obtained in example 3, and c is the Ti-doped single-layer molybdenum disulfide single crystal obtained in example 3;
FIG. 2 is an optical photograph of Ti-doped monolayer molybdenum disulfide single crystals obtained in comparative examples 1 and 2, wherein a is the Ti-doped monolayer molybdenum disulfide single crystal obtained in comparative example 1, and b is the Ti-doped monolayer molybdenum disulfide single crystal obtained in comparative example 2;
FIG. 3 is photoluminescence of a Ti-doped monolayer of molybdenum disulfide single crystal obtained in example 1 and a molybdenum disulfide single crystal obtained in comparative example 3;
FIG. 4 is a graph of photoluminescence of a Ti-doped monolayer of molybdenum disulfide single crystal obtained in comparative example 1 and molybdenum disulfide single crystal obtained in comparative example 3;
FIG. 5 is a photoluminescence of the Ti-doped monolayer of molybdenum disulfide single crystal obtained in comparative example 2 and the molybdenum disulfide single crystal obtained in comparative example 3;
FIG. 6 is Raman Mapping and PL Mapping graphs of the Ti-doped single-layer molybdenum disulfide single crystal obtained in example 1, wherein a is Raman Mapping and b is PL Mapping;
FIG. 7 is an AFM image of the Ti-doped single-layer molybdenum disulfide single crystal obtained in example 1, wherein a is an AFM image, and b is a height measurement image of the marked-out portion of the Ti-doped single-layer molybdenum disulfide single crystal in the image a;
FIG. 8 is an XPS data of Mo in the Ti-doped single-layer molybdenum disulfide single crystal obtained in example 1;
FIG. 9 is a XPS data of the S element in the Ti-doped single-layer molybdenum disulfide single crystal obtained in example 1;
FIG. 10 is a graph of XPS data for Ti element in a Ti-doped single-layer molybdenum disulfide single crystal obtained in example 1;
FIG. 11 is a low power TEM image of a Ti-doped monolayer molybdenum disulfide single crystal obtained in example 1;
FIG. 12 is a TEM-EDS elemental mapping of Mo in the Ti-doped single-layer molybdenum disulfide single crystal obtained in example 1;
FIG. 13 is a TEM-EDS elemental mapping of the S element in the Ti-doped single-layer molybdenum disulfide single crystal obtained in example 1;
FIG. 14 is a TEM-EDS elemental mapping of Ti element in the Ti-doped single-layer molybdenum disulfide single crystal obtained in example 1;
FIG. 15 shows the EDS energy spectra and the element contents of the elements in the Ti-doped single-layer molybdenum disulfide single crystal obtained in example 1;
FIG. 16 is a STEM of a single crystal of Ti-doped monolayer molybdenum disulfide obtained from example 1.
Detailed Description
The technical scheme of the invention is further explained by combining specific examples.
MoO 3 Purity is more than or equal to 99.9 percent and Beijing Haog;
and (2) S powder: the purity is more than or equal to 99.999 percent and the sigma;
I 2 : the purity is more than or equal to 99.999 percent, and Alfa Aesar;
TiO 2 : purity is more than or equal to 99.99 percent, beijing HaoKe;
OLYMPUS-bx53 m-microscope;
WITec confocal Raman coupled atomic force microscopy (Raman-AFM) systems;
the quartz tube heating uses a tube furnace.
The quartz tubes used in the following examples and comparative examples had a length of 15cm and an inner diameter of 11mm.
Examples 1 to 3
A preparation method of Ti-doped monolayer molybdenum disulfide single crystal comprises the following steps:
1) Preparing a quartz tube with two open ends, wherein the two ends of the quartz tube are respectively a raw material end and a substrate end, placing a substrate in the substrate end of the quartz tube, placing raw materials and a transport agent in the raw material end of the quartz tube, vacuumizing the quartz tube by using a vacuum tube sealing device, and sealing the quartz tube by using flame gun flame to ensure that the pressure in the quartz tube is 3.5 x 10 -4 Pa, ensuring that other elements except Ti are not introduced, wherein the raw material is MoO 3 S powder and TiO 2 The transport agent is elementary iodine;
2) Simultaneously heating a raw material end and a substrate end of a quartz tube for 0.5h, naturally cooling to room temperature of 20-25 ℃ along with a furnace, and obtaining the Ti-doped monolayer molybdenum disulfide monocrystal on the substrate, wherein the heating temperature of the raw material end is T1 ℃, the heating temperature of the substrate end is T2 ℃, the heating rate of heating to T1 ℃ is T1 ℃/min, the heating rate of heating to T2 ℃ is T2 ℃/min, and the temperature gradient between the raw material end and the substrate end is x ℃/cm.
TABLE 1
Comparative examples 1 to 2
A preparation method of Ti-doped monolayer molybdenum disulfide single crystal comprises the following steps:
1) Preparing a quartz tube with two open ends, wherein the two ends of the quartz tube are respectively a raw material end and a substrate end, placing mica as a substrate in the substrate end of the quartz tube, placing raw materials and a transport agent in the raw material end of the quartz tube, vacuumizing the quartz tube by using a vacuum tube sealing device, and sealing the quartz tube by using flame of a flame gun to ensure that the pressure in the quartz tube is 3.5 x 10 -4 Pa, ensuring that other elements except Ti are not introduced, wherein the raw material is MoO 3 S powder and TiO 2 The transport agent is elementary iodine;
2) Simultaneously heating a raw material end and a substrate end of a quartz tube for 0.5h, naturally cooling the raw material end and the substrate end along with a furnace to room temperature of 20-25 ℃, and obtaining the Ti-doped monolayer molybdenum disulfide monocrystal on the substrate, wherein the heating temperature of the raw material end is 850 ℃, the heating temperature of the substrate end is 600 ℃, the heating rate of heating to 850 ℃ is 42.5 ℃/min, the heating rate of heating to 600 ℃ is 30 ℃/min, and the temperature gradient between the raw material end and the substrate end is 16 ℃/cm.
TABLE 2
Comparative example 3
A preparation method of molybdenum disulfide single crystal comprises the following steps:
1) Preparing a quartz tube with two open ends, wherein the two ends of the quartz tube are respectively a raw material end and a substrate end, placing mica as a substrate in the substrate end of the quartz tube, placing raw materials and transport agents in the raw material end of the quartz tube, vacuumizing the quartz tube by using a vacuum tube sealing device, and sealing the quartz tube by using flame of a flame gun to ensure that the pressure in the quartz tube is 3.5 x 10 -4 Pa, wherein the starting material is 2.7mg of MoO 3 And 0.4mg of S powder, the transport agent is 3mg of elemental iodine;
2) Heating the raw material end and the substrate end of the quartz tube for 0.5h simultaneously, naturally cooling to room temperature of 20-25 ℃ along with the furnace, and obtaining molybdenum disulfide single crystal on the substrate, wherein the heating temperature of the raw material end is 850 ℃, the heating temperature of the substrate end is 600 ℃, the heating rate of heating to 8501 ℃ is 42.5 ℃/min, the heating rate of heating to 6002 ℃ is 30 ℃/min, and the temperature gradient between the raw material end and the substrate end is 16 ℃/cm.
Fig. 1 shows a, b, and c are optical micrographs of Ti-doped monolayer molybdenum disulfide single crystals grown on different substrates in examples 1 to 3 of the present invention, respectively, which indicate that the Ti-doped monolayer molybdenum disulfide single crystal obtained by the preparation method of the present invention can be applied to the growth of various substrates, has a wide growth temperature range, and can maintain a monolayer MoS after doping 2 The triangular shape of (1).
In fig. 2, a and b are optical photographs of Ti doped monolayer molybdenum disulfide single crystal grown under the doping amounts of comparative example 1 and comparative example 2, respectively. Comparative example 1 has a comparative example compared to example 1The doping amount is smaller in the embodiment 1, and the growth morphology is almost unchanged; comparative example 2 has a larger doping amount than example 1, the growth morphology is significantly deformed, and the center nucleation is severe, so that an ideal single-layer MoS cannot be obtained 2 And (3) single crystal.
FIG. 3 is a photoluminescence of the Ti-doped monolayer molybdenum disulfide single crystal obtained in example 1 and the molybdenum disulfide single crystal obtained in comparative example 3, showing that the Ti-doping is compared to the undoped monolayer MoS 2 The photoluminescence of the single crystal is greatly enhanced. The inset is the comparison of the luminescence peak position after the luminescence intensity is normalized, which shows that the peak position is blue-shifted after doping Ti element.
FIG. 4 is a graph showing photoluminescence of a Ti-doped single-layer molybdenum disulfide single crystal obtained in comparative example 1 and a molybdenum disulfide single crystal obtained in comparative example 3, and a single-layer MoS was found at a smaller doping amount 2 The photoluminescence property enhancement effect of the single crystal is not significant.
FIG. 5 is a plot of photoluminescence of the Ti-doped monolayer of molybdenum disulfide single crystal obtained in comparative example 2 and the molybdenum disulfide single crystal obtained in comparative example 3, where a monolayer of MoS was found at higher doping levels 2 The photoluminescence enhancement effect of the single crystal is not obvious, and the crystallinity of the single crystal is influenced due to a large number of defects introduced by excessive doping.
FIG. 6 is a Raman Mapping and PL Mapping plot of isolated triangular morphology samples of Ti-doped monolayer molybdenum disulfide single crystal obtained in example 1 of the present invention showing the doped MoS 2 Still has uniformity of crystal quality and uniformity of light emitting properties.
FIG. 7 is an AFM picture of a Ti-doped single-layer molybdenum disulfide single crystal obtained in example 1 of the present invention, and a graph b corresponds to a height variation curve of a line drawn in FIG. 1, showing that the thickness of the Ti-doped single-layer molybdenum disulfide single crystal grown is about 0.8nm, which is equivalent to a single-layer MoS 2 The thickness of (A) was kept consistent, indicating that MoS was obtained by the preparation method of the present invention 2 Is a single layer of material.
FIGS. 8 to 10 are XPS data graphs of Ti-doped monolayer molybdenum disulfide single crystals obtained in example 1 of the present invention, and analysis of the data shows that Ti atoms successfully enter MoS 2 In the crystal lattice and form Ti-S bonds.
FIG. 11E14 is a TEM-EDS elemental mapping chart of the Ti-doped monolayer molybdenum disulfide single crystal obtained in example 1 of the present invention, which more visually illustrates that the doping element is in MoS 2 Uniform distribution in the crystal.
FIG. 15 is a TEM-EDS spectrum of a single crystal of Ti-doped single-layer molybdenum disulfide obtained in example 1 of the present invention and the content ratio of each element, showing characteristic peaks of Ti-K, and the doping amount of Ti element is about 1.2%.
FIG. 16 is a STEM chart of a Ti-doped single-layer molybdenum disulfide single crystal obtained in example 1 of the present invention, from which it can be determined that Ti is in MoS 2 The original Mo position is replaced in the crystal lattice, thereby obtaining the transition element doped single-layer MoS 2 And (3) single crystal.
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (8)
1. A preparation method of a Ti-doped monolayer molybdenum disulfide single crystal is characterized by comprising the following steps:
1) Preparing a quartz tube with two open ends, wherein the two ends of the quartz tube are respectively a raw material end and a substrate end, placing a substrate in the substrate end of the quartz tube, placing a raw material and a transport agent in the raw material end of the quartz tube, vacuumizing the quartz tube, and sealing the quartz tube to ensure that the pressure in the quartz tube is 10 -6 ~10 -3 Pa, wherein the raw material is MoO with the mass portion of 2.3-2.5 3 0.36 to 0.42 mass portion of S powder and 0.35 mass portion of TiO 2 The transport agent is elemental iodine;
2) Heating the raw material end and the substrate end of the quartz tube for 0.5 to 1h at the same time, cooling to the room temperature of 20 to 25 ℃, and obtaining a Ti-doped monolayer molybdenum disulfide monocrystal on the substrate, wherein the heating temperature of the raw material end is 750 to 900 ℃, and the heating temperature of the substrate end is 400 to 700 ℃.
2. The method according to claim 1, wherein in the step 1), the substrate is mica or graphite.
3. The production method according to claim 1, wherein in the step 1), the quartz tube has a length of 15 to 40cm and an inner diameter of 10 to 20mm.
4. The production method according to claim 1, wherein in the step 1), the ratio of the raw material to the transporting agent is (2~6): (3-8).
5. The production method according to claim 1, wherein in the step 2), the heating rate is 25 to 50 ℃/min for heating to 750 to 900 ℃, and the heating rate is 25 to 50 ℃/min for heating to 400 to 700 ℃.
6. The preparation method according to claim 1, wherein in the step 2), the temperature gradient between the raw material end and the base end is 3 to 30 ℃/cm.
7. The Ti-doped monolayer molybdenum disulfide single crystal obtained by the process of any one of claims 1~6.
8. Use of the method of claim 1~6 in the simultaneous photoluminescence enhancement of a single layer of molybdenum disulfide and single crystal molybdenum disulfide production.
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| WO2014134524A1 (en) * | 2013-03-01 | 2014-09-04 | Massachusetts Institute Of Technology | Synthesis of transition metal disulfide layers |
| US9527062B2 (en) * | 2013-05-09 | 2016-12-27 | North Carolina State University | Process for scalable synthesis of molybdenum disulfide monolayer and few-layer films |
| US20150064471A1 (en) * | 2013-08-28 | 2015-03-05 | Massachusetts Institute Of Technology | Seed for Metal Dichalcogenide Growth by Chemical Vapor Deposition |
| IN2013CH04799A (en) * | 2013-10-24 | 2015-05-08 | Empire Technology Dev Llc | |
| CN109225274B (en) * | 2018-10-26 | 2020-08-14 | 苏州大学 | Fe-doped MoS2Nano material and preparation method and application thereof |
| US11114579B2 (en) * | 2019-06-19 | 2021-09-07 | University Of Electronic Science And Technology Of China | Method for preparing ultrathin two-dimensional nanosheets and applications thereof |
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| CN109633933A (en) * | 2018-12-19 | 2019-04-16 | 海南大学 | Mn-MoS2Monofilm photomagnetic material preparation method |
| CN111575787A (en) * | 2020-04-20 | 2020-08-25 | 天津理工大学 | Method for growing single-layer silicon phosphide crystal |
| CN111893565A (en) * | 2020-08-04 | 2020-11-06 | 中国人民解放军国防科技大学 | Method for growing single-layer molybdenum disulfide or molybdenum diselenide by using promoter |
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