CN111304747A - Non-layered two-dimensional PbSe crystal material and preparation method thereof - Google Patents
Non-layered two-dimensional PbSe crystal material and preparation method thereof Download PDFInfo
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- CN111304747A CN111304747A CN202010247872.3A CN202010247872A CN111304747A CN 111304747 A CN111304747 A CN 111304747A CN 202010247872 A CN202010247872 A CN 202010247872A CN 111304747 A CN111304747 A CN 111304747A
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Abstract
The invention belongs to the field of nano semiconductor materials, and discloses a non-layered two-dimensional PbSe crystal material and a preparation method thereof. The preparation method comprises the following steps: (a) selecting a reaction container marked as an upstream area, a central area and a downstream area, and selecting Se powder as a selenium source to be arranged in the upstream area; (b) selecting Pb3O4Taking the lead as a lead source, mixing the lead source with potassium chloride to obtain a precursor, then placing the precursor in a central area, and selecting mica as a growth substrate to be placed in a downstream area; (c) introducing argon as a carrier gas into the reaction vessel, introducing hydrogen as a reaction gas, and heating for reaction to obtain the non-layered two-dimensional PbSe crystal material on the mica substrate. The invention also discloses a product prepared by the method. The invention meets the preparation requirement of large-batch two-dimensional nano PbSe crystal materials, and the product crystal has the advantages of smooth and clean surface, uniform appearance, uniform element distribution, abundant raw materials, low price, simple preparation, convenient popularization and large scaleAnd (4) production.
Description
Technical Field
The invention belongs to the related technical field of nano semiconductor materials, and particularly relates to a non-layered two-dimensional PbSe crystal material and a preparation method thereof.
Background
Since the first mechanical stripping of graphene in 2004, two-dimensional materials represented by graphene have attracted extensive attention from researchers. To date, in addition to graphene, a large number of two-dimensional nanomaterials have been prepared by researchers, such as transition metal sulfur compounds, layered metal oxides, transition metal carbides, and the like. Due to the ultra-high specific surface area and strong quantum confinement of electrons in two dimensions, the two-dimensional nano materials show a plurality of unconventional physical, optical, chemical and electronic properties, and show huge application potential in the fields of catalysis, energy storage and conversion, sensing, biomedicine and the like of electronic devices. At present, research on two-dimensional materials is mainly focused on layered structure materials, however, in nature, more non-layered materials forming chemical bonds in three-dimensional space are reported, and the non-layered materials are few because the non-layered materials form bonds in three-dimensional directions. Inspired by two-dimensional material crystals, one can expect that controlled synthesis of non-layered structured two-dimensional materials may bring some unique properties and advanced functions that are not achievable with materials of other dimensions.
As a traditional IV-VI semiconductor material, PbSe has a narrow direct band gap (0.28eV), a large exciton Bohr radius (46nm), an extremely strong quantum confinement effect, high carrier mobility and a low thermal conductivity coefficient, so that the PbSe has important potential application value in a plurality of fields including field effect transistors, photoelectric detectors, solar cells and the like. However, the current research on PbSe is based on zero-dimensional quantum dots and one-dimensional nanomaterials. Due to the three-dimensional bonding of the self structure, the acquisition of the non-layered two-dimensional PbSe material must break the thermodynamic equilibrium state, and the kinetic controllability is artificially introduced to limit the three-dimensional anisotropic growth of the material.
Mechanical stripping is an effective method for rapidly obtaining a two-dimensional material, but the method is only suitable for materials with weak interlayer bonding force, and has low yield and high randomness. In addition, in wet chemical synthesis methods, the product size is small, the surface quality is poor and integration on silicon-based substrates is difficult due to the liquid environment.
Therefore, how to prepare the non-layered two-dimensional PbSe material with large size, uniform appearance and clean surface is an important problem which needs to be solved urgently at present.
Disclosure of Invention
In view of the above-mentioned disadvantages and/or needs for improvement of the prior art, the present invention provides a method for preparing a non-layered two-dimensional PbSe crystal material and a product thereof, in which Se powder is used as a selenium source by adding Pb to the crystal material3O4Mixing with KCl to obtain precursor, lowering evaporation temperature, and forming intermediate transition state to promote reaction. And the molecular sieve is added to be used as a slow release agent to control the source quantity supply, so that the preparation of the two-dimensional PbSe crystal material is realized.
In order to achieve the above objects, according to one aspect of the present invention, there is provided a method for preparing a non-layered two-dimensional PbSe crystalline material, comprising the steps of:
(a) dividing the reaction vessel into an upstream region, a central region and a downstream region;
(b) selecting Se powder as a selenium source and placing the Se powder in an upstream area; selecting Pb3O4As a lead source, mixing the lead source with potassium chloride to obtain a precursor, and then placing the precursor in a central area; selecting mica as a growth substrate, and sequentially and tightly arranging a plurality of pieces of mica in a downstream area;
(c) introducing argon as a carrier gas into the reaction container, introducing hydrogen as a reaction gas, heating and reacting to obtain the non-layered two-dimensional PbSe crystal material on the mica substrate, wherein the carrier gas and the reaction gas flow from the upstream area to the downstream area.
Further, in step (a), the upstream region is 17cm to 19cm from the central region.
Further, in the step (b), a molecular sieve is arranged above the precursor for slowing down the evaporation rate of the precursor, and the downstream area is 9-13 cm away from the central area.
Further, in the step (c), the carrier gas and the reaction gas are both high-purity gases, the flow rate of the argon gas is 20sccm to 50sccm, and the flow rate of the hydrogen gas is 5 sccm.
Further, in the step (c), heating is carried out by adopting a rapid heating mode, and the temperature of the central temperature zone is 600-700 ℃.
Further, the pressure of the central temperature area and the pressure of the downstream deposition area are less than or equal to one atmosphere.
Further, the substrate is mica.
To achieve the above object, according to one aspect of the present invention, there is provided a non-layered two-dimensional PbSe crystalline material prepared by the preparation method as described in any one of the above.
Generally, compared with the prior art, the above technical solution conceived by the present invention mainly has the following technical advantages:
1. according to the invention, potassium chloride molten salt is used for assisting vapor deposition, wherein the mixture of potassium chloride and a metal precursor can effectively reduce the reaction temperature of a central temperature zone, and a volatile intermediate is generated to promote the reaction, so that the energy consumption in the preparation process is reduced; the reactor is divided into three areas, different reaction sources are separately placed in different areas to realize independent control of evaporation of different source materials, and the molecular sieve is added on the precursor to serve as a slow release agent, so that the evaporation rate of the source materials is effectively controlled, and uniform reaction is facilitated.
2. The invention is in Pb3O4The potassium chloride is added as a precursor, the temperature required by the reaction can be reduced by utilizing the characteristic that the salt and the metal oxide are mixed, so that the energy consumption is reduced, and meanwhile, a volatile intermediate transition state is formed in the reaction process to promote the reaction.
3. The molecular sieve is added on the precursor to play a role of a slow release agent, so that the evaporation rate of the precursor can be effectively slowed down, the supply of raw materials is controlled, and the source materials are fully reacted.
4. The invention adopts a rapid heating method to carry out reaction, effectively controls the evaporation time of the source materials, realizes the synchronous reaction and avoids the situation of insufficient reaction caused by advanced evaporation due to different evaporation temperatures of the source materials.
5. The invention protects the product from being oxidized by introducing inert gas as carrier gas into the reactor, simultaneously carries product molecules to downstream deposition, and additionally introduces hydrogen as reaction gas to participate in the reaction of chemical vapor deposition.
6. The mica substrate is selected as the substrate for preparing the non-layered two-dimensional PbSe crystal material, the surface is flat at the atomic level, a dangling bond is not formed, the three-dimensional growth of the non-layered material can be limited, and the material is easy to transfer to other substrates for continuous processing.
7. The non-layered two-dimensional PbSe crystal material prepared by the method has the advantages of smooth surface, uniform appearance and uniform element distribution.
Drawings
FIG. 1 is a schematic diagram of an apparatus for preparing a non-layered two-dimensional PbSe crystal material provided by the present invention;
FIGS. 2a to 2d are top views of the morphologies of the non-layered two-dimensional PbSe crystal materials prepared in examples 1 to 4 of the present invention, respectively;
FIG. 3 is a thickness measurement chart of a non-layered two-dimensional PbSe crystal material prepared in example 1 of the present invention;
FIG. 4 is a Raman spectrum of a non-layered two-dimensional PbSe crystal material prepared in example 1 of the present invention;
fig. 5a and 5b are elemental composition analysis diagrams of a non-layered two-dimensional PbSe crystal material prepared in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
As shown in fig. 1, the embodiment of the present invention provides a method for preparing a non-layered two-dimensional PbSe crystal material, and the preparation method specifically includes:
(a) selecting a reaction container which is divided into an upstream area, a central area and a downstream area, selecting Se powder as a selenium source, and placing the Se powder in the upstream area;
(b) selecting Pb3O4Taking the lead as a lead source, mixing the lead source with potassium chloride to obtain a precursor, then placing the precursor in a central region, selecting mica as a growth substrate, and sequentially and tightly arranging a plurality of pieces of mica in a downstream region;
(c) introducing argon gas as a carrier gas into the reaction container, introducing hydrogen gas as a reaction gas, and heating for reaction to obtain the non-layered two-dimensional PbSe crystal material on the mica substrate, wherein the gas flows from the upstream area to the downstream area.
More specifically, at Pb3O4The potassium chloride is added as a precursor, because the temperature required by the reaction can be reduced by mixing the salt and the metal oxide, the energy consumption is further reduced, and meanwhile, a volatile intermediate transition state is formed in the reaction process to promote the reaction. The molecular sieve is added on the precursor to play a role of a slow release agent, so that the evaporation rate of the precursor can be effectively slowed down, the supply of raw materials is controlled, and the source materials are fully reacted.
Further, the precursor is placed in the central region, Se powder is placed in an upstream region 17cm to 19cm from the central region, and the mica substrate is placed in a downstream region 9cm to 13cm from the central region. The reactor is filled with high-purity gas, the argon flow is 20 sccm-50 sccm, and the hydrogen flow is 5 sccm. The reaction is carried out by adopting a rapid heating mode, and the temperature of the central temperature zone is preferably 600-700 ℃.
In summary, the invention provides a method for preparing a non-layered two-dimensional PbSe crystal material, which can meet the requirements of mass preparation, smooth surface of the product, uniform appearance and uniform element distribution.
The preparation method of the non-layered two-dimensional PbSe crystal material provided by the invention is further illustrated by the following specific examples.
Example 1
A single-temperature-zone horizontal tube furnace is adopted as a reactor, the tube length of the horizontal tube furnace is 90cm, the outer diameter of the horizontal tube furnace is 25mm, the tube wall thickness is 2mm, the range of a constant-temperature zone is 10cm, the temperature of a central temperature zone is set to be 650 ℃, and the heating rate is 30 ℃/min. Using Se powder (purity)>99.99%) as a selenium source placed in the upstream zone; pb3O4Powder of(purity of>99.99%) as lead source, adding KCl to obtain precursor, covering molecular sieve on the precursor, and placing in central temperature zone; the mica substrate was placed in the downstream area to collect the product. Before the reaction, pre-vacuumizing to about 10Pa, then filling Ar of 600sccm to atmospheric pressure, and repeatedly washing for 3 times to remove residual oxygen; ar of 20sccm is introduced as a carrier gas and H of 5sccm is introduced in the reaction process2And (3) as reaction gas, keeping the pressure at one atmospheric pressure, reacting for 25 minutes, keeping the carrier gas unchanged after the reaction is finished, cooling the product to room temperature along with the furnace, and obtaining the non-layered two-dimensional PbSe crystal material on the mica substrate.
Example 2
A single-temperature-zone horizontal tube furnace is adopted as a reactor, the tube length of the horizontal tube furnace is 90cm, the outer diameter of the horizontal tube furnace is 25mm, the tube wall thickness is 2mm, the range of a constant-temperature zone is 10cm, the temperature of a central temperature zone is set to be 700 ℃, and the heating rate is 30 ℃/min. Using Se powder (purity)>99.99%) as a selenium source placed in the upstream zone; pb3O4Powder (purity)>99.99%) as lead source, adding KCl to obtain precursor, covering molecular sieve on the precursor, and placing in central temperature zone; the mica substrate was placed in the downstream area to collect the product. Before the reaction, pre-vacuumizing to about 10Pa, then filling Ar of 600sccm to atmospheric pressure, and repeatedly washing for 3 times to remove residual oxygen; ar of 30sccm is introduced as a carrier gas and H of 5sccm is introduced in the reaction process2And (3) as reaction gas, keeping the pressure at one atmospheric pressure, reacting for 25 minutes, keeping the carrier gas unchanged after the reaction is finished, cooling the product to room temperature along with the furnace, and obtaining the non-layered two-dimensional PbSe crystal material on the mica substrate.
Example 3
A single-temperature-zone horizontal tube furnace is adopted as a reactor, the tube length of the horizontal tube furnace is 90cm, the outer diameter of the horizontal tube furnace is 25mm, the tube wall thickness is 2mm, the range of a constant-temperature zone is 10cm, the temperature of a central temperature zone is set to be 650 ℃, and the heating rate is 30 ℃/min. Using Se powder (purity)>99.99%) as a selenium source placed in the upstream zone; pb3O4Powder (purity)>99.99%) as lead source, adding KCl to obtain precursor, covering molecular sieve on the precursor, and placing in central temperature zone; mica liningThe bottom was placed in the downstream region to collect the product. Before the reaction, pre-vacuumizing to about 10Pa, then filling Ar of 600sccm to atmospheric pressure, and repeatedly washing for 3 times to remove residual oxygen; ar of 20sccm is introduced as a carrier gas and H of 5sccm is introduced in the reaction process2And (3) as reaction gas, keeping the pressure at one atmospheric pressure, reacting for 30 minutes, keeping the carrier gas unchanged after the reaction is finished, cooling the product to room temperature along with the furnace, and obtaining the non-layered two-dimensional PbSe crystal material on the mica substrate.
Example 4
A single-temperature-zone horizontal tube furnace is adopted as a reactor, the tube length of the horizontal tube furnace is 90cm, the outer diameter of the horizontal tube furnace is 25mm, the tube wall thickness is 2mm, the range of a constant-temperature zone is 10cm, the temperature of a central temperature zone is set to be 600 ℃, and the heating rate is 30 ℃/min. Using Se powder (purity)>99.99%) as a selenium source placed in the upstream zone; pb3O4Powder (purity)>99.99%) as lead source, adding KCl to obtain precursor, covering molecular sieve on the precursor, and placing in central temperature zone; the mica substrate was placed in the downstream area to collect the product. Before the reaction, pre-vacuumizing to about 10Pa, then filling Ar of 600sccm to atmospheric pressure, and repeatedly washing for 3 times to remove residual oxygen; ar of 20sccm is introduced as a carrier gas and H of 5sccm is introduced in the reaction process2And (3) as reaction gas, keeping the pressure at one atmospheric pressure, reacting for 20 minutes, keeping the carrier gas unchanged after the reaction is finished, cooling the product to room temperature along with the furnace, and obtaining the non-layered two-dimensional PbSe crystal material on the mica substrate.
The surface morphology of the non-layered two-dimensional PbSe crystal materials prepared in examples 1 to 4 was characterized by an optical microscope, and the results are shown in FIGS. 2a to 2 d. The consistent morphology of the material can be seen in figures 2a, 2b, 2c and 2 d.
The non-layered two-dimensional PbSe crystal material prepared in example 1 was subjected to thickness measurement by scanning the surface of the sample with an atomic force microscope probe, and the monolithic thickness of the material prepared in example 1 was measured to be 34nm, and the measurement results are shown in fig. 3.
The non-layered two-dimensional PbSe crystal material prepared in example 1 was subjected to composition analysis by raman spectroscopy, and the results are shown in fig. 4, and it was confirmed that the product was a non-layered two-dimensional PbSe crystal material by measuring a raman peak corresponding to a PbSe standard raman peak.
The non-layered two-dimensional PbSe crystal material prepared in example 1 was subjected to composition analysis using energy-dispersive X-ray spectroscopy, and the results are shown in FIGS. 5a to 5b, demonstrating that two elements of Pb and Se in the product were uniformly distributed.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (8)
1. A preparation method of a non-layered two-dimensional PbSe crystal material is characterized by comprising the following steps:
(a) dividing the reaction vessel into an upstream region, a central region and a downstream region;
(b) selecting Se powder as a selenium source and placing the Se powder in an upstream area; selecting Pb3O4As a lead source, mixing the lead source with potassium chloride to obtain a precursor, and then placing the precursor in a central area; selecting mica as a growth substrate, and sequentially and tightly arranging a plurality of pieces of mica in a downstream area;
(c) introducing argon as a carrier gas into the reaction container, introducing hydrogen as a reaction gas, heating and reacting to obtain the non-layered two-dimensional PbSe crystal material on the mica substrate, wherein the carrier gas and the reaction gas flow from the upstream area to the downstream area.
2. The method for preparing a non-layered two-dimensional PbSe crystalline material according to claim 1, wherein in step (a), the upstream region is 17cm to 19cm from the central region.
3. The method according to claim 1 or 2, wherein in step (b), a molecular sieve is disposed above the precursor for slowing down the evaporation rate of the precursor, and the downstream region is 9-13 cm away from the central region.
4. The method for preparing a non-layered two-dimensional PbSe crystal material according to any one of claims 1 to 3, wherein in the step (c), the carrier gas and the reaction gas are high-purity gases, the flow rate of argon is 20sccm to 50sccm, and the flow rate of hydrogen is 5 sccm.
5. The method for preparing a non-layered two-dimensional PbSe crystal material as claimed in any of claims 1 to 3, wherein in step (c), heating is performed by rapid temperature rise, and the temperature of the central temperature region is 600-700 ℃.
6. The method for preparing a non-layered two-dimensional PbSe crystal material as set forth in any of claims 1 to 3, wherein the pressure of the central temperature zone and the downstream deposition zone is one atmosphere or less.
7. The method for preparing a non-layered two-dimensional PbSe crystal material according to any one of claims 1 to 3, wherein the substrate is mica.
8. A non-layered two-dimensional PbSe crystal material, which is prepared by the preparation method according to any one of claims 1 to 7.
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| CN114232102A (en) * | 2021-12-15 | 2022-03-25 | 华中科技大学 | Two-dimensional ZnTe crystal material and preparation method and application thereof |
| CN115287625A (en) * | 2022-07-08 | 2022-11-04 | 武汉大学 | Method for preparing two-dimensional non-layered narrow-band-gap semiconductor material based on Van der Waals epitaxy |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113089100A (en) * | 2021-03-22 | 2021-07-09 | 华中科技大学 | Two-dimensional ferromagnetic Cr sensitive to strain2Te3Nanosheet and preparation method thereof |
| CN113526472A (en) * | 2021-06-28 | 2021-10-22 | 清华-伯克利深圳学院筹备办公室 | Non-layered manganese selenide nanosheet and preparation method thereof |
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| CN115287625A (en) * | 2022-07-08 | 2022-11-04 | 武汉大学 | Method for preparing two-dimensional non-layered narrow-band-gap semiconductor material based on Van der Waals epitaxy |
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