CN116169012A - Preparation method of two-dimensional layered semiconductor material with room-temperature ferromagnetism and ferroelectricity - Google Patents
Preparation method of two-dimensional layered semiconductor material with room-temperature ferromagnetism and ferroelectricity Download PDFInfo
- Publication number
- CN116169012A CN116169012A CN202310461728.3A CN202310461728A CN116169012A CN 116169012 A CN116169012 A CN 116169012A CN 202310461728 A CN202310461728 A CN 202310461728A CN 116169012 A CN116169012 A CN 116169012A
- Authority
- CN
- China
- Prior art keywords
- temperature
- powder
- ferroelectricity
- ferromagnetism
- dimensional layered
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02568—Chalcogenide semiconducting materials not being oxides, e.g. ternary compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/20—Methods for preparing sulfides or polysulfides, in general
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G47/00—Compounds of rhenium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/0257—Doping during depositing
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method of a two-dimensional layered semiconductor material with room-temperature ferromagnetism and ferroelectricity. The method comprises the following steps: (1) Mixing manganese acetate powder and sodium cholate powder, and dissolving the mixture in water to form a precursor solution; (2) spin-coating the precursor liquid on the clean silicon wafer surface; (3) Placing ammonium perrhenate powder and sodium chloride powder into a downstream quartz boat by adopting a double-temperature-zone tube furnace, placing a silicon wafer subjected to spin coating above the mixed powder, and placing sublimed sulfur powder into an upstream quartz boat; (4) reactant preheating: heating the upstream and downstream temperature areas to a specified temperature and introducing argon; (5) heat preservation reaction; (6) Naturally cooling to room temperature to obtain the two-dimensional layered manganese doped rhenium disulfide material. The two-dimensional layered manganese doped rhenium disulfide material has ferroelectricity and ferromagnetism at the same time, and the transition temperature of the ferromagnetism and the ferroelectricity exceeds the room temperature.
Description
Technical Field
The invention belongs to the technical field of semiconductor materials, and relates to a preparation method of a two-dimensional layered semiconductor material with room-temperature ferromagnetism and ferroelectricity.
Background
The two-dimensional layered material has the advantages of high mobility, adjustable band gap, large specific surface area, atomic-level thickness and the like, has wide application prospect in the fields of electronics, optoelectronics, sensors, flexible devices and the like, and is a preferable material for the research and development of the next-generation electronic information technology. The two-dimensional ferrimagnetic and multiferroic semiconductor material has spontaneous polarization with degrees of freedom such as charge, spin and energy valley, can realize response to multiple physical fields such as magnetic field, electric field and optical field, has great application potential in the aspects of high-density storage and low-power consumption devices of data, and has important significance in breaking through the technical bottleneck of semiconductor chips facing the post-molar era and developing next-generation high-density, fast-response, low-energy-consumption and nonvolatile electronic information storage devices.
Multiferroic materials refer to materials having more than two primary ferri-character, such properties including (anti) ferroelectricity, (anti) ferromagnetism, ferroelasticity, etc. The existence of multiferroics creates conditions for the birth of more novel logic memory devices. Along with the continuous optimization of the preparation process and the rapid development of micro-nano technology, miniaturization, integration and multifunctionality of electronic elements have become development trends, and iron research under the nano scale has become a focus of attention in the field of research of novel functional materials. How to integrate ferroelectricity, ferromagnetism and multiferroics in two-dimensional or lower-dimensional materials, and then develop a multi-stable and multifunctional spintronics device and a nonvolatile memory device has become an important target pursued by researchers. Taking ferroelectric properties as an example, in recent years, researchers have conducted a great deal of research both theoretically and experimentally, and have made remarkable progress. In these two-dimensional ferroelectric materials (e.g. SnTe, snS, snSe, bi 2 O 2 Se、CuInP 2 S 6 、α-In 2 Se 3 、dT-MoTe 2 Etc.), spontaneous polarization is derived from the arrangement of atoms in the unit cell, so that the positive and negative charge centers of the atoms are relatively displaced along a certain direction, and are strictly constrained by lattice symmetry and structural stability. Thus, only a small amount of two-dimensional layered material has been experimentally confirmed to have intrinsic ferroelectricity so far. In addition, according to Mermin-Wagner's law, in an ultrathin isotropic film, long-range magnetic order heat fluctuation is strongly suppressed, and intrinsic two-dimensional magnetism is considered to be absent; while anisotropy in certain two-dimensional layered materials can counteract the negative effects of thermal fluctuations, exhibiting magnetic ordering at a certain temperature. Layered magnetic materials in two-dimensional limits since 2017 (e.g. CrI 3 、Cr 2 Ge 2 Te 6 And Fe (Fe) 3 GeTe 2 Etc.), successively reported. These efforts have created a new era of two-dimensional magnetic research.
The magnetoelectric multiferroic material can provide a new way for digital information processing by utilizing the coupling between the ferroelectric sequence and the ferromagnetic sequence and regulating the stable state of the medium through effective means, and is honored as a pilot for future information storage. In a two-dimensional multiferroic semiconductor material system, coexistence, coupling and regulation of a ferroelectric sequence and a ferromagnetic sequence are realized, and properties such as charge, spin and polarization of electrons can be controlled simultaneously, so that information processing and storage functions are integrated on a single chip, which becomes one of important directions of development of next-generation information technology. However, it is extremely difficult to obtain the above two physical properties in the same material system due to the difference in physical origin of the ferroelectric sequence and the ferromagnetic sequence. Therefore, the experimentally prepared two-dimensional multiferroic material is rare, and represented by CuCrP 2 S 6 、NiI 2 p-SnSe. Wherein CuCrP 2 S 6 、NiI 2 Both the (anti) ferroelectric and (anti) ferromagnetic transition temperatures are below room temperature (Wang X, shang Z, zhang C, et al Electrical and magnetic anisotropies in van der Waals multiferroic CuCrP) 2 S 6 [J]. Nature Communications, 2023, 14 (1): 840; Song Q, Occhialini CA, Ergecen E, et al., Evidence for a single-layer van der Waals multiferroic[J]. Nature, 2022, 602 (7898): 601-605.），p-The ferroelectric and ferromagnetic transition temperatures of SnSe are above room temperature (Du R, wang Y, cheng M, et al, two-dimensional multiferroic material of metallic p-doped SnSe [ J ]]. Nature Communications, 2022, 13 (1): 6130; Chang K, Küster F, Miller BJ, et al., Microscopic Manipulation of Ferroelectric Domains in SnSe Monolayers at Room Temperature[J]Nano Letters 2020, 20 (9): 6590-6597.) but, because of its metallic nature, can have a performance impact in the application of the device.
Rhenium disulfide is a recently reported slipping ferroelectric material whose ferroelectricity is derived from ferroelectric polarization resulting from charge transfer caused by interlayer slipping in a multilayer state. And in the double-layer state, the ferroelectric transition temperature can reach 405K (Wan Y, hu T, mao X, et al, room-Temperature Ferroelectricity in T' -ReS) 2 Multilayers[J]Physical Review Letters, 2022, 128 (6): 067601.) are significantly above room temperature. For the two-dimensional ferromagnetic materials reported at present, the two-dimensional ferromagnetic materials have the characteristic of low magnetic transition temperature, which also causes the problem that the two-dimensional ferromagnetic materials are difficult to normally apply at room temperature. However, in theory, there are also materials with higher ferromagnetic transition temperatures, mnS 2 Is of interest to researchers because of its relatively high magnetic transition temperature of 225K (Kan M, adhikari S, sun Q, ferromagnetism in MnX) 2 (X=S, Se) monolayers[J]Physical Chemistry Chemical Physics, 2014, 16 (10): 4990-4994. However, two-dimensional MnS has not been produced by experimental means so far 2 。
Therefore, a series of problems of how to raise the working temperature and strengthen the multi-degree-of-freedom coupling of the two-dimensional multiferroic material need to be solved. Obtaining room temperature stable two-dimensional multiferroic semiconductor materials remains an important challenge.
Disclosure of Invention
Aiming at the problem that the existing two-dimensional material magnetic doping is limited to the doping mainly aiming at local magnetic atoms, and the substitution type doping with large area uniformity and high concentration is difficult to realize in a two-dimensional material system, the invention provides a preparation method of a two-dimensional layered semiconductor material with room-temperature ferromagnetism and ferroelectricity. The invention takes the difficulty of introducing a magnetic ordered structure into a two-dimensional system into consideration, adopts a universal mixed salt-mediated chemical vapor deposition method to prepare the room-temperature two-dimensional magnetoelectric multiferroic material-manganese doped rhenium disulfide, and has high controllability and reproducibility.
According to the invention, manganese atoms are introduced into multi-layer rhenium disulfide through doping means for the first time, so that the two-dimensional multiferroic semiconductor material with ferroelectricity and ferromagnetism is successfully prepared, and the ferroelectricity and ferromagnetism of the two-dimensional multiferroic semiconductor material are characterized to exceed the room temperature. For doping of manganese element, the traditional chemical vapor deposition method based on the solid phase doping source is difficult to synthesize a clean sample, and the manganese content in the generated sample is also difficult to control, so that the solid phase doping source is used for doping manganese element, and the implementation difficulty is high.
The technical scheme of the invention is as follows:
the preparation method of the two-dimensional layered semiconductor material with room temperature ferromagnetism and ferroelectricity comprises the following steps:
step 3, sample loading: a double-temperature zone tube furnace is adopted, and the mass ratio of ammonium perrhenate powder to sodium chloride powder is 10: fully mixing ammonium perrhenate powder and sodium chloride powder, then placing the mixture into a downstream quartz boat, placing the silicon wafer subjected to spin coating above the mixed powder, enabling the spin coating surface to face the powder, and placing sublimed sulfur powder into an upstream quartz boat;
Preferably, in the step 1, the mass ratio of the manganese acetate to the sodium cholate to the deionized water is 1:2:150-250, and more preferably 1:2:200.
Preferably, in the step 2, the pretreatment method of the clean silicon wafer comprises the following steps: and sequentially carrying out ultrasonic cleaning on the silicon wafer by using acetone, ethanol and deionized water, and then airing.
Preferably, in the step 2, the spin coating speed is 2500-3000 rpm, and the time is 1-1.5 min.
Preferably, in step 4, the temperature rising speed of the upstream temperature zone is 18.75 ℃/min, and the temperature rising speed of the downstream temperature zone is 5 ℃/min.
Preferably, in the step 4, the flow rate of argon is 80+ -5 sccm.
Compared with the prior art, the invention has the following advantages:
(1) The two-dimensional layered manganese doped rhenium disulfide material prepared by the invention has ferroelectricity and ferromagnetism at the same time, and the transition temperature of the ferromagnetism and the ferroelectricity exceeds the room temperature;
(2) The prepared two-dimensional layered manganese doped rhenium disulfide material is uniform in appearance and large in size, and is beneficial to subsequent characterization and use;
(3) Due to the addition of the precursor solution, the manganese element doping concentration of the two-dimensional layered manganese doped rhenium disulfide material prepared by the invention is relatively stable.
Drawings
FIG. 1 is a schematic diagram of a two-dimensional layered semiconductor material with room temperature ferromagnetism and ferroelectricity, wherein 1 is SiO 2 The Si substrate, 2 is the quartz boat I, 3 is the quartz boat II, 4 is the temperature zone I, and 5 is the temperature zone II.
Fig. 2 is a transmission electron micrograph of manganese doped rhenium disulfide (a): a thicker region morphology map of manganese doped rhenium disulfide; (b): a morphology diagram of a thinner area of manganese doped rhenium disulfide; (c): an enlarged area topography of fig. 2 (b).
Fig. 3 is a graph of the structure and composition analysis results of manganese doped rhenium disulfide, (a): high angle annular dark field scanning transmission electron microscope (HAADF-STEM) atomic images of pure phase rhenium disulfide; (b): manganese doped rhenium disulfide HAADF-STEM atomic images; (c): an atomic model of manganese doped rhenium disulfide; (d): element profile of manganese doped rhenium disulfide; (e): an elemental composition map of manganese doped rhenium disulfide; (f): x-ray photoelectron spectroscopy (XPS) of rhenium, sulfur and manganese in manganese doped rhenium disulfide.
Fig. 4 is a graph of the temperature swing ferromagnetism characterization of manganese doped rhenium disulfide (a): along the in-plane direction, the manganese doped rhenium disulfide sample has a complete hysteresis loop; (b): along the in-plane direction, a graph of coercive force versus temperature of the manganese doped rhenium disulfide sample; (c): along the out-of-plane direction, the manganese doped rhenium disulfide sample has a complete hysteresis loop; (d): and (3) in the out-of-plane direction, a graph of coercive force of the manganese doped rhenium disulfide sample versus temperature.
Fig. 5 is a graph of room temperature ferroelectricity characterization of manganese doped rhenium disulfide, (a): a microscopic image of a manganese doped rhenium disulfide sample disposed on a conductive gold substrate; (b): an Atomic Force Microscope (AFM) morphology characterization map of manganese doped rhenium disulfide; (c): a piezoelectric microscope (PFM) amplitude plot of manganese doped rhenium disulfide; (d): PFM phase diagram of manganese doped rhenium disulfide; (e): a manganese doped rhenium disulfide thickness analysis corresponding to fig. 5 (b); (f): PFM butterfly graph of manganese doped rhenium disulfide; (g): PFM hysteresis loop plot of manganese doped rhenium disulfide.
Fig. 6 is a graph of the morphology of manganese doped rhenium disulfide samples prepared at two growth temperatures.
Detailed Description
The invention will be described in further detail with reference to specific embodiments and drawings.
Example 1
(1) Preparing a precursor liquid: manganese acetate powder (99.999%, alfa Aesar) and sodium cholate powder (99%, alfa Aesar) were weighed in order and put into a 40 ml glass sample bottle, followed by adding deionized water, and shaking for 5min to mix thoroughly, to prepare a precursor liquid. The mass ratio of the manganese acetate powder to the sodium cholate powder to the deionized water is 1:2:200.
(2) Spin coating: cut out 2×2 cm 2 The silicon wafer is washed by acetone, ethanol and deionized water for 5min, the washed and dried silicon wafer is placed on a spin coater and rotated for 1 min at 3000rpm, the prepared precursor liquid is rapidly sucked by a rubber head dropper after the rotation starts, the precursor liquid is dripped onto the silicon wafer in a rotating state, 3 drops are dripped, and the spin coating is waited to finish.
(3) Sample loading: weighing ammonium perrhenate powder (more than or equal to 99 percent), SIGMA-ALDRICH and sodium chloride powder (99.8 percent) and putting the mixture into a No. I quartz boat after fully mixing, and obliquely lapping a spin-coated silicon wafer right above the mixed powder of ammonium perrhenate and sodium chloride, wherein the spin-coating surface faces the mixed powder. The sublimated sulfur powder (more than or equal to 99.5 percent) is weighed and put into a quartz boat II. The mass ratio of ammonium perrhenate powder, sodium chloride powder and sublimed sulfur powder is 10:3:90. as shown in FIG. 1, the quartz boat I and the quartz boat II are respectively placed in a temperature zone I and a temperature zone II in a double-temperature zone tube furnace.
(4) Reactant preheating: the temperatures of the temperature zone I and the temperature zone II are respectively increased to 750 ℃ and 200 ℃ at the rates of 18.75 ℃/min and 5 ℃/min, argon is kept to be introduced into the tubular furnace at the flow rate of 80sccm, and the air flow direction is from the temperature zone II to the temperature zone I.
(5) Formal reaction: after the temperature of the temperature zone I and the temperature zone II reach the designated temperature, the temperature of the two zones is kept unchanged for 10 min, and argon is still kept to be introduced into the tubular furnace at the flow rate of 80sccm during the period, and the air flow direction is kept unchanged.
(6) And (3) naturally cooling: and after the reaction is finished, naturally cooling the quartz tube to room temperature.
As shown in fig. 2, with the aid of a transmission electron microscope, it can be observed that: the synthesized sample has the shape of a lamellar sheet, uniform thickness and clean surface (figures 2 (a) - (c)). In pure phase ReS 2 In the HAADF-STEM image (FIG. 3 (a)), the rhenium chain structure is clearly visible, the rhenium chain direction corresponding to ReS 2 [010 of]The crystal orientation, i.e., the b-axis direction, had a interplanar spacing of 0.34 nm. 100 at an angle of about 60 DEG to the b-axis]The crystal orientation, i.e., the A-Axis direction, had a interplanar spacing of 0.31 nm. The above resultsIs in agreement with the values reported in the prior literature (LinYC, komsa HP, yeh CH, et al, single-Layer ReS) 2 : Two-Dimensional Semiconductor with Tunable In-Plane Anisotropy[J]. ACS Nano, 2015, 9(11): 11249-11257; Cui F, Wang C, Li X, et al., Tellurium-Assisted Epitaxial Growth of Large-Area, Highly Crystalline ReS 2 Atomic Layers on Mica Substrate[J]Advanced Materials, 2016, 28 (25): 5019-5024.). Further, by contrast of HAADF-STEM atomic images of pure phase rhenium disulfide (fig. 3 (a)) and manganese doped rhenium disulfide (fig. 3 (b)), the doped manganese atomic distribution was successfully observed (fig. 3 (c) is the corresponding atomic model of fig. 3 (b)). HAADF-STEM analysis confirmed that Mn site was incorporated in a substitutional form with ReS 2 In ReS 2 In which MnS is realized 2 Local phase segregation of microdomains (radial dimensions of about 3-5 nm).
The constituent elements and their distribution were determined by an X-ray spectrometer (EDS) (fig. 3 (d), 3 (e)). EDS characterization results show that Re/Mn: the S ratio is about 1:2.09, according to 1:2, the doping concentration of Mn is about 2.7%, and the content is extremely low. With XPS, fine spectrum scanning of characteristic elements was performed, and characteristic peaks of Re, S and Mn elements were clearly seen (FIG. 3 (f)). Proof that manganese element was successfully doped in ReS 2 Among them.
The magnetic properties of the sample in both in-plane and out-of-plane directions were confirmed by a comprehensive physical property measurement system, and the test results are shown in FIG. 4. In the temperature range of 4K (kelvin, thermodynamic temperature scale) to 300K (room temperature), complete hysteresis loops of the manganese doped rhenium disulfide samples were tested both in the in-plane and out-of-plane directions (fig. 4 (a), 4 (c)), and the coercivity sizes exhibited a decreasing trend with increasing temperature (fig. 4 (b), 4 (d)). The test sample was confirmed to have ferromagnetism at room temperature.
The room temperature ferroelectric properties of the manganese doped rhenium disulfide samples were verified by PFM testing (fig. 5). Due to the test requirements, the sample was transferred onto the conductive gold substrate in advance (fig. 5 (a)). Ferroelectric domains were drawn on a test piece of thickness 2.09 nm (approximately two layers, fig. 5 (b), 5 (e)) using PFM techniques (fig. 5 (c), 5 (d)). And the butterfly curve and the hysteresis loop (fig. 5 (f), 5 (g)) were measured, demonstrating that the manganese doped rhenium disulfide sample has ferroelectricity. Therefore, the manganese doped rhenium disulfide prepared by the invention is proved to be a two-dimensional multiferroic material with room-temperature ferromagnetism and ferroelectricity.
TABLE 1 comparison of the two-dimensional multiferroic materials and manganese doped rhenium disulfide properties
| Multiferroic material Material | (anti-) ferroelectric Transition temperature | (anti) ferromagnetic Transition temperature | Reference to the literature |
| CuCrP 2 S 6 | 145K | 32K | Wang X, Shang Z, Zhang C, et al., Electrical and magnetic anisotropies in van der Waals multiferroic CuCrP 2 S 6 [J]. Nature Communications, 2023, 14 (1): 840. |
| NiI 2 | 59.5K | 59.5K | Song Q, Occhialini CA, Ergecen E, et al., Evidence for a single-layer van der Waals multiferroic[J]. Nature, 2022, 602 (7898): 601-605. |
| p-SnSe (Metal) Sex toy | 400K | 337K | Du R, Wang Y, Cheng M, et al., Two-dimensional multiferroic material of metallic p-doped SnSe[J]. Nature Communications, 2022, 13 (1): 6130.Chang K, Küster F, Miller BJ, et al., Microscopic Manipulation of Ferroelectric Domains in SnSe Monolayers at Room Temperature[J]. Nano Letters, 2020, 20 (9): 6590-6597. |
| Re 1- x Mn x S 2 | 405K | ＞300K | The invention is that |
In conclusion, the manganese-doped rhenium disulfide prepared by the method realizes coexistence of ferroelectricity and ferromagnetism at room temperature, and expands the two-dimensional multiferroic semiconductor material family. Meanwhile, the manganese doped rhenium disulfide is a semiconductor material, so that the manganese doped rhenium disulfide has application advantages compared with p-SnSe with metal. In addition, from the ferromagnetic point of view, manganese doped rhenium disulfide is more than the intrinsic two-dimensional MnS predicted by theoretical calculation 2 The magnetic transition temperature (225K) is higher (300+K, above room temperature), described in intrinsic ReS 2 The intermediate doping of Mn element produces unexpected technical effects.
Comparative example 1
This comparative example is essentially the same as example 1, except that the growth temperature is changed from 750 ℃ to 700 ℃. Fig. 6 is a graph of the morphology of the manganese doped rhenium disulfide samples prepared at two growth temperatures, and shows that the morphology of the samples is uneven and the thickness is extremely thick at 700 ℃, and the morphology of the samples at 750 ℃ is uniform and the thin layer area is large, so that the subsequent experimental characterization is facilitated.
Claims (8)
1. The preparation method of the two-dimensional layered semiconductor material with room temperature ferromagnetism and ferroelectricity is characterized by comprising the following steps:
step 1, preparing a precursor liquid: mixing manganese acetate powder and sodium cholate powder according to the mass ratio of 1:2, and dissolving the mixture into deionized water to obtain a precursor solution;
step 2, spin coating: spin-coating the precursor liquid on the surface of a clean silicon wafer;
step 3, sample loading: a double-temperature zone tube furnace is adopted, and the mass ratio of ammonium perrhenate powder to sodium chloride powder is 10: fully mixing ammonium perrhenate powder and sodium chloride powder, then placing the mixture into a downstream quartz boat, placing the silicon wafer subjected to spin coating above the mixed powder, enabling the spin coating surface to face the powder, and placing sublimed sulfur powder into an upstream quartz boat;
step 4, reactant preheating: heating the upstream temperature zone to 750-770 ℃, heating the downstream temperature zone to 200-220 ℃, and simultaneously introducing argon into the upstream temperature zone, wherein the air flow direction is from upstream to downstream;
step 5, formal reaction: after the two temperature areas reach the designated temperature, keeping the temperature of the two temperature areas unchanged, maintaining for 10-15 min, and continuously introducing argon;
step 6, naturally cooling: stopping heating after the reaction is completed, and naturally cooling to room temperature to obtain the two-dimensional layered manganese doped rhenium disulfide material.
2. The preparation method of claim 1, wherein in the step 1, the mass ratio of manganese acetate, sodium cholate and deionized water is 1:2:150-250.
3. The preparation method according to claim 1, wherein in the step 1, the mass ratio of manganese acetate, sodium cholate and deionized water is 1:2:200.
4. The method according to claim 1, wherein in step 2, the pretreatment method of the clean silicon wafer comprises: and sequentially carrying out ultrasonic cleaning on the silicon wafer by using acetone, ethanol and deionized water, and then airing.
5. The method according to claim 1, wherein in the step 2, the spin coating speed is 2500 to 3000rpm for 1 to 1.5 minutes.
6. The method according to claim 1, wherein in step 4, the temperature rising rate in the upstream temperature zone is 18.75 ℃/min, and the temperature rising rate in the downstream temperature zone is 5 ℃/min.
7. The method according to claim 1, wherein in the step 4, the flow rate of argon gas is 80.+ -.5 sccm.
8. The two-dimensional layered semiconductor material having room temperature ferromagnetism and ferroelectricity manufactured by the manufacturing method according to any one of claims 1 to 7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310461728.3A CN116169012B (en) | 2023-04-26 | 2023-04-26 | Preparation method of two-dimensional layered semiconductor material with room-temperature ferromagnetism and ferroelectricity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310461728.3A CN116169012B (en) | 2023-04-26 | 2023-04-26 | Preparation method of two-dimensional layered semiconductor material with room-temperature ferromagnetism and ferroelectricity |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116169012A true CN116169012A (en) | 2023-05-26 |
| CN116169012B CN116169012B (en) | 2023-08-08 |
Family
ID=86414942
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310461728.3A Active CN116169012B (en) | 2023-04-26 | 2023-04-26 | Preparation method of two-dimensional layered semiconductor material with room-temperature ferromagnetism and ferroelectricity |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116169012B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117737859A (en) * | 2023-12-20 | 2024-03-22 | 武汉理工大学 | Two-dimensional Bi with biaxial tensile strain 2 O 2 Se single crystal and process for producing the same |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105668530A (en) * | 2016-01-14 | 2016-06-15 | 苏州微格纳米科技有限公司 | Preparation method of two-dimensional nanomaterial |
| CN109023295A (en) * | 2018-07-16 | 2018-12-18 | 广东工业大学 | A kind of rhenium disulfide film of large-area two-dimensional and its preparation method and application |
| CN114892277A (en) * | 2022-04-20 | 2022-08-12 | 苏州科技大学 | Preparation method of ferromagnetic two-dimensional material with strong room temperature |
-
2023
- 2023-04-26 CN CN202310461728.3A patent/CN116169012B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105668530A (en) * | 2016-01-14 | 2016-06-15 | 苏州微格纳米科技有限公司 | Preparation method of two-dimensional nanomaterial |
| CN109023295A (en) * | 2018-07-16 | 2018-12-18 | 广东工业大学 | A kind of rhenium disulfide film of large-area two-dimensional and its preparation method and application |
| CN114892277A (en) * | 2022-04-20 | 2022-08-12 | 苏州科技大学 | Preparation method of ferromagnetic two-dimensional material with strong room temperature |
Non-Patent Citations (1)
| Title |
|---|
| MIN LUO，ET AL: "Structural and magnetic properties of transition-metal adsorbed ReS2 monolayer", 《JAPANESE JOURNAL OF APPLIED PHYSICS》, vol. 56, pages 055701 - 1 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117737859A (en) * | 2023-12-20 | 2024-03-22 | 武汉理工大学 | Two-dimensional Bi with biaxial tensile strain 2 O 2 Se single crystal and process for producing the same |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116169012B (en) | 2023-08-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Jundale et al. | Nanocrystalline CuO thin films: synthesis, microstructural and optoelectronic properties | |
| Goktas et al. | Influence of pH on the structural optical and magnetic properties of Zn1− xMnxO thin films grown by sol–gel method | |
| CN116169012B (en) | Preparation method of two-dimensional layered semiconductor material with room-temperature ferromagnetism and ferroelectricity | |
| CN109811307B (en) | Preparation method of two-dimensional material nano belt or micro belt | |
| CN111206283B (en) | Preparation and application of chromium diselenide two-dimensional material | |
| Guo et al. | Low temperature fabrication of thermochromic VO 2 thin films by low-pressure chemical vapor deposition | |
| CN113957412A (en) | Molybdenum disulfide film with consistent grain orientation height and preparation method thereof | |
| Jiang et al. | Tuning 2D Magnetism in Cobalt Monoxide Nanosheets Via In Situ Nickel‐Doping | |
| CN109987931A (en) | B doping bismuth ferrite solid solution membranes and its preparation method and application | |
| Radjehi et al. | Structural and magnetic properties of copper oxide films deposited by DC magnetron reactive sputtering | |
| Kayani et al. | Structural, optical, and magnetic properties of cobalt-doped dip coated ZnO films | |
| Tang et al. | High-coercivity CoFe2O4 thin films on Si substrates by sol-gel | |
| Gumiel et al. | Thin film processing of multiferroic BiFeO3: From sophistication to simplicity. A review | |
| Kayani et al. | Investigation of structural, optical and magnetic characteristics of Co3O4 thin films | |
| CN114775049A (en) | Cr (chromium)3Te4Non-laminated two-dimensional material and preparation and application thereof | |
| Zhang et al. | Influence of citric acid on the morphology and magnetic properties of barium ferrite thin films | |
| Kayani et al. | Structural, optical and magnetic properties of aluminum doped MnZnO films deposited by dip coating | |
| CN116623152A (en) | Two-dimensional CrS nano-sheet and preparation method and application thereof | |
| Dwivedi et al. | Enhanced magnetoresistance in pulsed laser deposited stable chromium oxide thin films | |
| WO2022032584A1 (en) | Solid solution multiferroic thin film and preparation method, and electronic device applied to 5g storage technology | |
| CN113789569A (en) | Two-dimensional magnetic Fe3O4Preparation method of single crystal nanosheet | |
| Cheng et al. | Manipulation of film quality and magnetic properties of CrO 2 (100) films on TiO 2 substrates with carrier gas and growth temperature | |
| Albino et al. | Effect of Ca and Ag doping on the functional properties of BiFeO 3 nanocrystalline powders and films | |
| Agusutrisno et al. | Control of inhomogeneity and magnetic properties of ZnO: Co films grown by magnetron sputtering using nitrogen | |
| Lee et al. | Growth of multiferroics BiFeO3 thin films by sol–gel method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |