CN115341272B - Preparation method of millimeter-level two-dimensional topological material bismuth selenide monocrystal - Google Patents
Preparation method of millimeter-level two-dimensional topological material bismuth selenide monocrystal Download PDFInfo
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- 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
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Abstract
The invention belongs to the technical field of topological insulator preparation, and particularly relates to a preparation method of a millimeter-level two-dimensional topological material bismuth selenide monocrystal. To solve the current Bi 2 Se 3 The preparation method still cannot meet the problems of low cost, batch preparation, large size and high uniformity, and the method effectively solves the problem of uneven nucleation and realizes Bi by adopting methods of time-limited ventilation (a method of maintaining vacuum in a temperature rising process and ventilating after reaching a set temperature), taking Bi powder and Se powder with low melting point as precursor sources, precisely controlling the substrate temperature (growth temperature) and the like 2 Se 3 Uniform and controllable growth of single crystal wafer, finally obtaining millimeter Bi 2 Se 3 A single chip.
Description
Technical Field
The invention belongs to the technical field of topological insulator preparation, and particularly relates to a preparation method of a millimeter-level two-dimensional topological material bismuth selenide monocrystal.
Background
Two-dimensional Bi 2 Se 3 The topological insulator has the advantages of high mobility, narrow band gap, high stability and the like, and has great application potential in the infrared detection field. However, the prior preparation method has the problems of small product size, uncontrollable thickness, uneven size and the like, thereby greatly limiting Bi 2 Se 3 Is used in the application of (a).
Currently, common Bi 2 Se 3 The preparation method mainly comprises the following steps: (1) mechanical stripping method: the method generally comprises repeatedly peeling bulk single crystal with adhesive tape, wherein the adhesive force of the adhesive tape to single crystal is greater than interlayer Van der Waals force, single crystal is easily peeled by at least one layer or even a single layer, and the peeled single crystal is nanometerThe rice flakes can be transferred to any target substrate for investigation. However, the method can only obtain a single crystal wafer with a diameter of tens of micrometers, the shape and thickness of the sample are uncontrollable, the preparation cost is high, the time consumption is long, the yield is low, and the method is not beneficial to industrial application. (2) liquid phase Synthesis method: the process typically involves dissolving one or more precursors in an organic solution to react to form the desired compound. In the case of using bismuth nitrate pentahydrate (Bi (NO) 3 ) 3 ·5H 2 O) and sodium selenate (Na 2 SeO 3 ) As a reaction source, preparing two-dimensional Bi with regular morphology in polyvinylpyrrolidone and ethylene glycol organic solution 2 Se 3 A nano-sheet. Despite the high yields of this process, the lateral dimensions of the product are only tens of microns, and it is difficult to obtain products with few layers or even a monolayer, and the solvent remaining on the sample surface during the reaction also reduces its performance. (3) molecular beam epitaxy: the method is carried out under ultra-high vacuum (10 -8 Pa), heating the ultrapure source material to slowly sublimate the ultrapure source material, so that the generated gaseous elements are condensed on the target substrate and react with each other to form a target product. Although the method can obtain a high-quality monocrystalline film, the preparation conditions are very strict, strict lattice matching is required between a substrate and a material, the preparation cost is high, and industrial application is difficult to realize. (4) chemical vapor deposition method (CVD): the method is to heat and evaporate the high-purity Bi in the center of a tube furnace 2 Se 3 And (3) a powder source, and transporting the evaporated gaseous source to a substrate downstream of the tube furnace to grow by taking inert gas as carrier gas. For example, there have been studies on SiO in an amorphous state by this method 2 Obtaining two-dimensional Bi with the thinnest thickness of 3nm and the maximum size of about 20 mu m on the substrate 2 Se 3 A nano-sheet. Bi having a lateral dimension of 400 μm was also studied to be produced on a mica substrate by the same method 2 Se 3 A single chip. Although Bi is used as the method 2 Se 3 Provides a basis for large-scale mass production of (C), but at present, bi is prepared by CVD 2 Se 3 The following problems remain with the process of (a): (1) bi is used as 2 Se 3 The powder is the source, and due to its high melting point (710 ℃) nature, it is necessary to place it in a single temperature zoneThe center of the tube furnace to promote evaporation, and the substrate is arranged at the downstream of the tube furnace, so that the substrate needs to be heated in a heat conduction mode, and the temperature of the surface of the substrate is difficult to control accurately; (2) in the whole process, the carrier gas is required to be kept flowing, and a small amount of Bi is necessary in the heating process 2 Se 3 Evaporation to the substrate, resulting in the formation of undesirable Bi 2 Se 3 The temperature zone of growth may exhibit unwanted nucleation sites, thereby resulting in high nucleation densities. The problems with the above two process drawbacks are: the growth temperature is uncontrollable, so that the growth speed is uncontrollable, and large-size single crystals cannot be obtained; the unnecessary nucleation sites in turn lead to different times at which growth begins, resulting in different thickness and size of the product and poor uniformity.
In conclusion, the present Bi 2 Se 3 The preparation method still cannot meet the requirements of low cost, batch preparation, large size and high uniformity. Therefore, it is necessary to develop a device capable of achieving millimeter Bi 2 Se 3 The method for preparing the single crystal ensures the uniformity and growth controllability of the single crystal preparation.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a preparation method of a millimeter-level two-dimensional topological material bismuth selenide monocrystal, which effectively solves the problem of uneven nucleation and realizes millimeter-level Bi 2 Se 3 Uniform and controllable growth of single crystal wafers.
In order to achieve the above purpose, the present invention is realized by the following technical scheme:
the invention provides a preparation method of a millimeter-level two-dimensional topological material bismuth selenide monocrystal, which specifically comprises the following steps: bismuth (Bi) powder and selenium (Se) powder are respectively used as Bi sources and Se sources, the Bi powder and the Se powder are respectively placed in different areas at the upstream of a single-temperature-zone tube furnace, and a mica substrate is placed in a central temperature zone; and then the temperature of the central temperature zone is raised to a preset temperature of 500-800 ℃ in a vacuum state, the vaporized Bi source and Se source are transmitted to the substrate by taking argon-hydrogen mixed gas as carrier gas, bismuth and selenium react under the action of hydrogen, and finally bismuth selenide (Bi 2Se 3) single crystals are generated on the mica substrate.
Preferably, the Se source is further from the central temperature zone than the Bi source. The bismuth and selenium sources were placed 10cm and 15cm upstream, respectively, from the central temperature zone.
Preferably, the reaction time of bismuth and selenium is 5-20 min, and the bismuth and selenium are naturally cooled to room temperature after the reaction is finished.
Preferably, the temperature rising rate of the central temperature zone is 30-40 ℃/min.
Preferably, in the argon-hydrogen mixed gas, the flow rate of argon is 50-100 sccm, and the flow rate of hydrogen is 2.5-5 sccm.
Preferably, the mica substrate is freshly exfoliated fluorophlogopite.
Preferably, before the central temperature zone begins to rise, the pressure in the furnace tube is pumped to a vacuum state of 10-100 Pa, then the furnace tube is closed, and the heating program is started. More preferably, before the furnace tube is sealed under the pressure, the furnace tube is pre-vacuumized to 9-15Pa, ar is filled to the atmospheric pressure, and the furnace tube is repeatedly scrubbed to remove residual oxygen. The process can effectively avoid unnecessary nucleation points in the heating process, effectively reduce nucleation density, improve growth speed and is beneficial to synthesizing large-size single crystal wafers.
Preferably, when the argon-hydrogen mixture is used as carrier gas to pass through the furnace chamber, the pressure in the furnace chamber is increased to the atmospheric pressure, and the air outlet valve is opened to enable bismuth and selenium to react under the action of hydrogen.
Preferably, the temperature of the central temperature zone is 500-700 ℃. More preferably, the temperature of the central temperature zone is 600 ℃.
Compared with the prior art, the invention has the beneficial effects that:
the invention discloses a preparation method of a millimeter-level two-dimensional topological material bismuth selenide monocrystal, which effectively solves the problem of uneven nucleation and realizes millimeter-level Bi by adopting methods of time-limited ventilation (a method of maintaining vacuum in a temperature rising process and ventilating after reaching a set temperature), taking Bi powder and Se powder with low melting points as precursor sources, precisely controlling the substrate temperature (growth temperature) and the like 2 Se 3 Uniform and controllable growth of single crystal wafers. Specifically, the invention has the following advantages:
(1) The invention adopts a time-limited ventilation method, thereby effectively avoiding Bi 2 Se 3 The single crystal wafer has uneven size and thickness and undersize. In the conventional method, the carrier gas runs through the whole process, and source evaporation occurs before the substrate does not reach the set temperature in the heating process, and then the carrier gas is transported to the substrate, so that unnecessary nucleation and growth are caused. When the temperature reaches the set temperature, the source evaporation increases, more sources are transported to the substrate, secondary nucleation and growth occur, resulting in poor uniformity, small size, and high nucleation density of the final product. In the heating process, the furnace tube is sealed, so that unnecessary nucleation is effectively avoided, and carrier gas is introduced after the temperature reaches the set temperature, thereby ensuring that all single crystal wafers nucleate and grow simultaneously, and further obtaining large-size Bi with uniform size and thickness 2 Se 3 A single chip;
(2) The invention selects Bi powder (melting point 271 ℃) and Se powder (melting point 221 ℃) with low melting point as reaction sources, and places the substrate in a heating center, thereby effectively avoiding the problem of small size of single crystal wafer caused by uncontrollable substrate temperature. The growth of two-dimensional materials is mainly affected by the growth temperature, and for the traditional growth mode, bi 2 Se 3 The melting point is higher (710 ℃) and the material growth temperature is lower, the substrate is placed in a low-temperature area at the downstream, the substrate temperature cannot be precisely controlled by heat conduction heating through the heating center, and the surface of the substrate has a temperature gradient difference, so that the optimal growth temperature cannot be precisely obtained, and the size of a product is usually small. The substrate is placed in the heating center, the growth temperature can be accurately controlled, and meanwhile, the thickness and the size controllability can be realized by comprehensively controlling the carrier gas flow, so that the obtained Bi 2 Se 3 The size of the single crystal wafer can reach 0.9mm;
(3) The invention realizes large-size growth by controlling the temperature of the heating center and the flow of the carrier gas. When the temperature is too low, the nucleation density is larger, the growth rate is slower, the source evaporation amount is smaller, the precursor supply is insufficient, and only a small and thin product can be obtained at the moment; when the temperature is too high, atomic desorption on the surface of the substrate is enhanced, and a large number of precursor particles cannot be generatedThe Bi is adsorbed on the surface of the substrate, and the adsorption energy of the surface of the single crystal wafer is increased at the same time 2 Se 3 The single crystal wafer tends to grow vertically, and the obtained product is small and thick, and the yield is low. Meanwhile, a proper amount of argon-hydrogen mixed gas flow rate can ensure sufficient supply of Bi source and Se source and satisfy Bi 2 Se 3 The growth requirement, hydrogen can enhance the reducibility of Se and accelerate Bi 2 Se 3 Is a growth of (a). Finally obtain millimeter Bi 2 Se 3 A single chip;
(4) According to the melting points of the Bi source and the Se source, the invention is arranged at a place which keeps a certain distance from a heating center, ensures that the Bi source and the Se source are uniformly transmitted to the substrate, and ensures that the Bi 2 Se 3 The single crystal element is uniformly distributed and has good crystallinity.
Drawings
FIG. 1 shows the preparation of two-dimensional Bi 2 Se 3 Schematic of an apparatus for single crystal material;
FIG. 2 shows the large-size Bi prepared in example 1 2 Se 3 Optical microscopy of single-wafer (2 a high power optical view, 2b low power optical view);
FIG. 3 shows Bi prepared in example 1 2 Se 3 A high resolution transmission electron microscope image of a single wafer;
FIG. 4 shows Bi prepared in example 1 2 Se 3 Element distribution diagram of single chip;
FIG. 5 shows Bi prepared in example 1 2 Se 3 Raman spectra of single-crystal wafers;
FIG. 6 shows Bi prepared in example 2 2 Se 3 Optical microscopy of single-wafer;
FIG. 7 shows Bi prepared in example 3 2 Se 3 Optical microscopy of single-wafer;
FIG. 8 is Bi prepared in comparative example 1 2 Se 3 Optical microscopy of single-wafer;
FIG. 9 shows Bi prepared in example 1 and comparative example 1 2 Se 3 A product size comparison plot of a single wafer;
FIG. 10 shows Bi prepared in example 1 and comparative example 1 2 Se 3 Single wafer productThickness comparison graph.
Detailed Description
The following describes the invention in more detail. The description of these embodiments is provided to assist understanding of the present invention, but is not intended to limit the present invention. In addition, the technical features of the embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
The experimental methods in the following examples, unless otherwise specified, are conventional, and the experimental materials used in the following examples, unless otherwise specified, are commercially available.
Example 1 preparation method of millimeter-level two-dimensional topological Material bismuth selenide Single Crystal
A single temperature zone horizontal tube furnace (ThermoFisher, TF 55035C-1) is adopted, the tube length is 100cm, the outer diameter is 25mm, the tube wall thickness is 2.5mm, and the constant temperature zone range (namely the central temperature zone) is 10cm.
(1) The center temperature was set to 600℃and the heating rate was 30℃per minute. Bismuth powder and selenium powder (purity > 99.99%) are used as Bi and Se sources and are respectively placed at a position 10cm and a position 15cm away from the upstream of a central temperature zone; adopting a fluorogold mica sheet as a deposition substrate and placing the fluorogold mica sheet in a central temperature zone;
(2) Pre-vacuumizing to about 10Pa before reaction, then filling 600sccm Ar to atmospheric pressure, and repeatedly washing gas to remove residual oxygen;
(3) Before heating, pumping the pressure in the furnace tube to 10Pa, sealing the furnace tube (keeping vacuum in the heating process), heating, opening an air inlet valve at the upstream of the furnace tube when the temperature is heated to 600 ℃, and introducing 50sccm Ar and 2.5sccm H 2 Opening a downstream air outlet valve after the pressure in the furnace tube reaches atmospheric pressure, reacting for 10 minutes, keeping the carrier gas unchanged after the reaction is finished, cooling the product to room temperature along with the furnace, and obtaining the two-dimensional Bi from the fluorophlogopite sheet 2 Se 3 A single chip.
As shown in FIG. 2, bi is grown 2 Se 3 The single chip has uniform hexagon with large size of 0.9mm; FIG. 3 is Bi 2 Se 3 The high resolution transmission electron microscope photograph of the product shows that the monocrystal has a lattice structure which is arranged regularly, and the interplanar spacing is 0.22nm; FIG. 4 is Bi 2 Se 3 The element component analysis result of the single crystal wafer shows that the Bi element and the Se element are uniformly distributed; FIG. 4 is Bi 2 Se 3 The Raman spectrum of the single crystal plate shows three characteristic peaks of 70cm respectively -1 ，130m -1 ，171cm -1 . The above results indicate that the synthesized product is bismuth selenide single crystal with good crystallinity.
Example 2 preparation method of millimeter-level two-dimensional topological Material bismuth selenide Single Crystal
The specific preparation method is the same as in example 1, except that: the center temperature was set at 500 ℃.
The morphology is shown in FIG. 6, the thickness is thinner, and the size (180-210 μm) is obviously smaller than that of the embodiment 1.
Example 3 preparation method of millimeter-level two-dimensional topological Material bismuth selenide Single Crystal
The specific preparation method is the same as in example 1, except that: the center temperature was set at 700 ℃.
The morphology is shown in FIG. 7, the thickness is thicker, and the size (97-170 μm) is obviously smaller than that of the embodiment 1.
Comparative example 1 conventional bismuth selenide Single Crystal preparation method
The single temperature zone horizontal tube furnace is adopted, the tube length is 100cm, the outer diameter is 25mm, the tube wall thickness is 2.5mm, and the constant temperature zone range is 10cm.
' the center temperature was set at 700℃and the heating rate was 30℃per minute (1). Bismuth selenide powder (purity > 99.99%) is used as Bi and Se sources and is placed in a central temperature zone; adopting a fluorogold mica sheet as a deposition substrate, and placing the fluorogold mica sheet at a position 14cm away from the downstream of the central temperature zone;
(2) Pre-vacuumizing to about 10Pa before reaction, then filling 600sccm Ar to atmospheric pressure, and repeatedly washing gas to remove residual oxygen;
(3) Heating is started, and 50sccm Ar and 2.5sccm H are introduced in the whole process 2 The reaction time is 10 minutes, the product is cooled to room temperature along with the furnace, and the fluorophlogopite is used for preparing the productObtaining two-dimensional Bi on a chip 2 Se 3 A single chip. The morphology is shown in fig. 8, the size is significantly reduced and the thickness and size uniformity are deteriorated compared to example 1.
By counting the product sizes and thicknesses of example 1 and comparative example 1 (fig. 9, 10), it is evident that there are significant advantages of the present invention: first, the product of example 1 was significantly larger in size than comparative example 1 and high in uniformity of size, with 97% of the product in the range of 0.7-0.9mm, while comparative example 1 was small in size and dispersed, with the product size being distributed between 30-200 μm. Second, the product of example 1 was uniform in thickness, with a product ratio of 95.5% between 9 and 11nm, while the product of comparative example 1 was distributed between 6 and 15nm in thickness. Thus, on the one hand, the invention realizes large-size Bi 2 Se 3 The preparation of single crystals, on the other hand, realizes the uniform growth of the thickness and the size height of the single crystal wafer.
The embodiments of the present invention have been described in detail above, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, and yet fall within the scope of the invention.
Claims (9)
1. A preparation method of a millimeter-level two-dimensional topological material bismuth selenide monocrystal is characterized in that bismuth powder and selenium powder are respectively used as a bismuth source and a selenium source, the bismuth powder and the selenium powder are respectively placed in different areas at the upstream of a single-temperature-zone tube furnace, and a mica substrate is placed in a central temperature zone; and then the temperature of the central temperature zone is raised to a preset temperature of 500-700 ℃ in a vacuum state, and then the vaporized bismuth source and selenium source are transmitted to the substrate by taking argon-hydrogen mixed gas as carrier gas, bismuth and selenium react under the action of hydrogen, and finally bismuth selenide monocrystal is generated on the mica substrate.
2. The method for preparing a bismuth selenide single crystal as claimed in claim 1, wherein the bismuth source and the selenium source are respectively placed at the upstream of 10cm and 15cm from the central temperature zone.
3. The method for preparing the bismuth selenide monocrystal as claimed in claim 1, wherein the reaction time of bismuth and selenium is 5-20 min, and the bismuth selenide monocrystal is naturally cooled to room temperature after the reaction.
4. The method for preparing the bismuth selenide monocrystal as claimed in claim 1, wherein the heating rate of the central temperature zone is 30-40 ℃/min.
5. The method for preparing the bismuth selenide single crystal as claimed in claim 1, wherein the argon-hydrogen mixed gas has a flow rate of 50-100 sccm and a flow rate of 2.5-5 sccm.
6. The method for preparing a millimeter-sized two-dimensional topological material bismuth selenide monocrystal according to claim 1, wherein the mica substrate is freshly peeled fluorophlogopite.
7. The method for preparing the bismuth selenide monocrystal made of the millimeter-scale two-dimensional topological material, according to claim 1, is characterized in that before the central temperature zone begins to rise in temperature, the pressure in the furnace tube is pumped to a vacuum state of 10-100 Pa, then the furnace tube is closed, and the heating program is started.
8. The method for preparing bismuth selenide single crystals as claimed in claim 7, wherein the vacuum is pre-pumped to 9-15Pa, inert gas is introduced to atmospheric pressure, and the gas is repeatedly washed to remove residual oxygen before the furnace tube is closed by the pumping pressure.
9. The method for preparing bismuth selenide monocrystal as claimed in claim 1, wherein the pressure in the furnace chamber is raised to atmospheric pressure when the argon-hydrogen mixture gas is used as carrier gas and passes through the furnace chamber, and the air outlet valve is opened to enable bismuth and selenium to react under the action of hydrogen.
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