CN114232102B - Two-dimensional ZnTe crystal material and preparation method and application thereof - Google Patents

Two-dimensional ZnTe crystal material and preparation method and application thereof Download PDF

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CN114232102B
CN114232102B CN202111535611.2A CN202111535611A CN114232102B CN 114232102 B CN114232102 B CN 114232102B CN 202111535611 A CN202111535611 A CN 202111535611A CN 114232102 B CN114232102 B CN 114232102B
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CN114232102A (en
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周兴
李东燕
翟天佑
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Huazhong University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
    • C30B29/48—AIIBVI compounds wherein A is Zn, Cd or Hg, and B is S, Se or Te
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
    • C30B23/02—Epitaxial-layer growth
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
    • C30B29/64—Flat crystals, e.g. plates, strips or discs

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Abstract

The invention belongs to the field of optical encryption materials, and particularly discloses a two-dimensional ZnTe crystal material as well as a preparation method and application thereof, wherein the preparation method comprises the following steps: respectively taking zinc chloride and tellurium powder as a Zn source and a Te source, respectively placing the Zn source and the Te source at the upstream of a central temperature zone, respectively placing molecular sieves above the Zn source and the Te source, and placing a substrate at the downstream of the central temperature zone; controlling the temperature of the central temperature zone to 850-980 ℃, carrying the evaporated Zn source and Te source to the substrate by using carrier gas containing hydrogen, and reacting the Zn source and the Te source under the action of the hydrogen to generate a flaky two-dimensional ZnTe crystal material on the substrate. The method can prepare the two-dimensional ZnTe crystal material with regular appearance and uniform element distribution, and realizes the synthesis of the ultrathin ZnTe nanosheet.

Description

Two-dimensional ZnTe crystal material and preparation method and application thereof
Technical Field
The invention belongs to the field of optical encryption materials, and particularly relates to a two-dimensional ZnTe crystal material and a preparation method and application thereof.
Background
With the rapid development of information technology, information security has attracted close attention of people. Encryption is of great importance in the storage and transmission of data as a means of securing information (ACS Nano 2021,15, 6257-6265). However, most of the current encryption methods focus on terminal encryption, and internal logic operation encryption is rarely involved (Angew. Chem. Int. Ed.2019,58, 15128-15135). The logical operation as a basic operation unit generates a large amount of data and is easily hacked and tampered. Therefore, encryption of logical operations is important to further improve information security.
Generally, photoluminescence (PL) is one of the most commonly used encryption methods because of its fast readability and simple design. In recent years, many photoluminescent materials such as quantum dots, upconversion nanoparticles, perovskites, and organic dyes have been used for information encryption (Nano lett.2021,21, 5186-5194). However, these materials are often not tunable in their PL properties after preparation. To implement encryption, a more complex design is required to adjust the PL properties, which is detrimental to applying logical operations encryption. Furthermore, since the invisibility of PL in natural light is widely known, the encryption technique of optical information is easily broken. In summary, an advanced encryption method with multi-mode, high adjustability and high security is urgently needed.
ZnTe is a direct bandgap semiconductor with a bandgap of 2.26eV. Many stoichiometric defects are easily generated during the synthesis of ZnTe, and induce the formation of defect emission peaks, which allows ZnTe to exhibit a rich luminescence mode (adv. Mater.2016,28, 276-283). Furthermore, the external field easily adjusts the optical properties of ZnTe, which makes it promising to achieve a high security of the logically operated encryption process in ZnTe (j.electron.mater.2004, 33, 579-582). Thus, znTe has significant advantages in logically operating encryption. However, the synthesis of ZnTe is limited in nanowire aspect, and the synthesis of ultrathin ZnTe nanosheets is limited by many limitations.
Disclosure of Invention
Aiming at the defects or improvement requirements of the prior art, the invention provides a two-dimensional ZnTe crystal material and a preparation method and application thereof, and aims to prepare the two-dimensional ZnTe crystal material with regular appearance and uniform element distribution.
To achieve the above object, according to a first aspect of the present invention, there is provided a method for preparing a two-dimensional ZnTe crystal material, comprising the steps of:
respectively taking zinc chloride and tellurium powder as a Zn source and a Te source, respectively placing the Zn source and the Te source at the upstream of a central temperature zone, respectively placing molecular sieves above the Zn source and the Te source, and placing a substrate at the downstream of the central temperature zone; controlling the temperature of the central temperature zone to 850-980 ℃, carrying the evaporated Zn source and Te source to the substrate by the carrier gas containing hydrogen, and reacting the Zn source and Te source under the action of the hydrogen to generate the flaky two-dimensional ZnTe crystal material on the substrate.
More preferably, the flow rate of the hydrogen gas is 5sccm to 10sccm.
More preferably, the reaction time is 10 to 20min.
As a further preference, the Zn source is further away from the central temperature zone than the Te source.
As a further preference, the Zn source and Te source are placed respectively at 16cm, 14cm upstream from the central temperature zone, and the substrate is placed at 10cm downstream from the central temperature zone.
More preferably, the temperature rise rate of the central temperature region is 30 to 40 ℃/min.
Further preferably, the carrier gas is a mixed gas of argon gas and hydrogen gas, and the flow rate of argon gas is 50sccm.
Further preferably, the reaction is carried out in a single-temperature-zone horizontal tube furnace, the outer diameter of a tube opening is 25mm, and the length of a central temperature zone is 10cm; the substrate is a fluorophlogopite sheet.
According to a second aspect of the present invention, there is provided a two-dimensional ZnTe crystalline material prepared by the above method.
According to a third aspect of the invention there is provided the use of a two-dimensional ZnTe crystal material as described above for optical encryption.
Generally, compared with the prior art, the above technical solution conceived by the present invention mainly has the following technical advantages:
1. the invention selects zinc chloride and tellurium powder as sources, adopts molecular sieves, can slow down the evaporation rate of the zinc chloride and tellurium powder, and the zinc chloride and tellurium powder are in H 2 ZnTe and HCl gas are generated by reaction under the action of gas, the melting point of zinc chloride is lower, the reaction temperature is reduced, the energy consumption is reduced, and the controllability of the preparation process is realized; and meanwhile, the temperature of the central temperature zone is controlled, so that a two-dimensional ZnTe crystal material with regular appearance and uniform element distribution is obtained, and the synthesis of ultrathin ZnTe nanosheets with the thickness of about 7nm is realized.
2. According to the invention, the temperature of the control center temperature zone and the flow rate of the carrier gas are comprehensively controlled, on one hand, too low reaction temperature can cause too little ZnTe nanosheet product, because the temperature is too low, the evaporation temperature of the source is correspondingly reduced, so that the evaporation content of the source is less, and further the yield is reduced; on the other hand, too high a reaction temperature leads to too fast a source evaporation rate, resulting in many granular samples being produced, making the substrate very dirty. Meanwhile, argon is used as transport gas, hydrogen is used as reaction gas, a proper amount of Zn source and Te source are ensured to reach the substrate, sufficient reaction gas is fully reacted, and the hydrogen has the effect of etching and thinning, so that the ultrathin flaky ZnTe is obtained.
3. The invention keeps a certain distance between the substrate and the central temperature zone, and can avoid the damage of the substrate due to overhigh temperature; meanwhile, according to the melting point of the Zn source and the melting point of the Te source, the Zn source and the Te source are respectively arranged at different positions at the upstream of the central temperature region, so that the Zn source and the Te source can uniformly reach the substrate, and the element distribution in the ZnTe crystal material is more uniform.
Drawings
FIG. 1 is a schematic view of an apparatus for preparing a two-dimensional ZnTe crystal material according to an embodiment of the present invention;
FIGS. 2a to 2c are top views of the shapes of two-dimensional ZnTe crystal materials prepared in examples 1 to 3 of the present invention, respectively;
FIG. 3 is a measurement characterization diagram of the thickness of the two-dimensional ZnTe crystal material prepared in example 1 of the present invention;
fig. 4a and 4b are analysis diagrams of the zinc and tellurium element components of the two-dimensional ZnTe crystal material prepared in example 1 of the present invention, respectively.
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 do not 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.
The embodiment of the invention provides a preparation method of a two-dimensional ZnTe crystal material, which comprises the following steps:
adopting a single-temperature-zone horizontal tube furnace, as shown in figure 1, wherein the outer diameter of a tube opening is 25mm, vacuumizing to about 10Pa before reaction, then filling 600sccm Ar to atmospheric pressure, and repeatedly washing gas to remove residual oxygen;
respectively taking zinc chloride and tellurium powder (with the purity of more than 99.99%) as a Zn source and a Te source, respectively placing the Zn source and the Te source at the upstream of a central temperature zone, respectively placing molecular sieves above the Zn source and the Te source, taking fluorophlogopite sheets as a deposition substrate, and placing the deposition substrate at the downstream of the central temperature zone;
the length of the central temperature area, namely the constant temperature area is 10cm, and the temperature of the central temperature area is increased to 850-980 ℃ at the temperature increasing speed of 30-40 ℃/min; and then carrying the Zn source and the Te source to the substrate for reaction by using hydrogen-containing carrier gas, keeping the pressure at one atmospheric pressure, reacting the Zn source and the Te source under the action of hydrogen to generate ZnTe and HCl gas, reacting for 10-20 min, 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 ZnTe crystal material from the fluorophlogopite.
Furthermore, because the melting point of the Zn source is lower than that of the Te source, the Zn source is farther away from the central temperature region, specifically, the Zn source and the Te source are respectively arranged at the upstream positions 16cm and 14cm away from the central temperature region, and the substrate is arranged at the downstream position 10cm away from the central temperature region, so that the substrate is prevented from being damaged.
Further, the carrier gas is Ar and H 2 Wherein Ar is used as a transport gas, H 2 As a reaction gas, and Ar flow rate is 50sccm 2 The flow rate is 5sccm to 10sccm.
The following are specific examples:
example 1
A single-temperature-zone horizontal tube furnace is adopted, the tube length is 90cm, the outer diameter is 25mm, the tube wall thickness is 2mm, the constant-temperature zone range is 10cm, the central temperature is set to be 950 ℃, and the heating rate is 30 ℃/min. Using zinc chloride and tellurium powder (purity)>99.99%) as Zn and Te sources, and molecular sieves are respectively arranged above the sources and at positions 14cm and 16cm upstream from the central temperature region; adopting fluorophlogopite sheet as a deposition substrate and placing the deposition substrate at a position which is 10cm away from a central temperature area at the downstream; before the reaction, the reaction is carried out, the vacuum is firstly pumped to about 10Pa, and then 600sccm Ar is filled into the atmospherePressurizing and repeatedly washing gas to remove residual oxygen; ar of 50sccm and H of 5sccm are introduced in the reaction process 2 And (3) serving as a carrier gas, keeping the pressure at one atmospheric pressure, reacting for 15 minutes, keeping the carrier gas unchanged after the reaction is finished, cooling the product to room temperature along with a furnace, and obtaining the two-dimensional ZnTe crystal material from the fluorophlogopite sheet.
As shown in fig. 2a, is a morphology characterization of the obtained two-dimensional ZnTe crystal material; as shown in fig. 3, which is a measurement of the thickness of the two-dimensional ZnTe crystal material, the thickness was about 6.4nm, confirming that the obtained product was a two-dimensional material. As shown in fig. 4a and 4b, the elemental composition analysis of the two-dimensional ZnTe crystal material shows that the two elements of zinc and tellurium are uniformly distributed from the elemental mapping chart of the product, and the product is the ZnTe crystal material.
Example 2
A single-temperature-zone horizontal tube furnace is adopted, the tube length is 90cm, the outer diameter is 25mm, the tube wall thickness is 2mm, the constant-temperature zone range is 10cm, the central temperature is set to be 850 ℃, and the heating rate is 30 ℃/min. Using zinc chloride and tellurium powder (purity)>99.99%) as Zn and Te sources, and molecular sieves are respectively arranged above the sources and at positions 14cm and 16cm upstream from the central temperature region; adopting fluorophlogopite sheet as a deposition substrate and placing the deposition substrate at a position which is 10cm away from a central temperature area at the downstream; before the reaction, pre-vacuumizing to about 10Pa, then filling 600sccm Ar to atmospheric pressure, and repeatedly washing gas to remove residual oxygen; introducing 50sccm Ar and 6sccm H in the reaction process 2 And (3) the product is cooled to room temperature along with the furnace, and a two-dimensional ZnTe crystal material is obtained from a fluorophlogopite sheet, wherein the shape representation of the two-dimensional ZnTe crystal material is shown in figure 2 b.
Example 3
A single-temperature-zone horizontal tube furnace is adopted, the tube length is 90cm, the outer diameter is 25mm, the tube wall thickness is 2mm, the constant-temperature zone range is 10cm, the central temperature is set to be 980 ℃, and the heating rate is 40 ℃/min. Using zinc chloride and tellurium powder (purity)>99.99%) as Zn and Te sources, and molecular sieves are respectively arranged above the sources and at positions 14cm and 16cm upstream from the central temperature region; using fluorophlogopite sheet as deposition substrate and placing it in downstream distance centerThe temperature zone is 10cm; before the reaction, pre-vacuumizing to about 10Pa, then filling 600sccm Ar to atmospheric pressure, and repeatedly washing gas to remove residual oxygen; ar of 50sccm and H of 8sccm are introduced in the reaction process 2 And (3) serving as a carrier gas, keeping the pressure at one atmospheric pressure for 15 minutes, keeping the carrier gas unchanged after the reaction is finished, cooling the product to room temperature along with a furnace, and obtaining a two-dimensional ZnTe crystal material from the fluorophlogopite sheet, wherein the morphological characterization of the material is shown in figure 2 c.
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 (9)

1. A preparation method of a two-dimensional ZnTe crystal material is characterized by comprising the following steps:
respectively taking zinc chloride and tellurium powder as a Zn source and a Te source, respectively placing the Zn source and the Te source at the upstream of a central temperature zone, respectively placing molecular sieves above the Zn source and the Te source, and placing a substrate at the downstream of the central temperature zone; controlling the temperature of the central temperature zone to be 850-980 ℃, carrying the evaporated Zn source and Te source to the substrate by carrier gas containing hydrogen, wherein the flow rate of the hydrogen is 5-10 sccm, and the Zn source and the Te source react under the action of the hydrogen to generate a flaky two-dimensional ZnTe crystal material on the substrate.
2. A method for preparing a two-dimensional ZnTe crystal material according to claim 1, wherein the reaction time is 10min to 20min.
3. A method of preparing a two-dimensional ZnTe crystalline material as claimed in claim 1, wherein the Zn source is located at a greater distance from the central temperature zone than the Te source.
4. A method for preparing a two-dimensional ZnTe crystalline material as claimed in claim 3, wherein the Zn source and the Te source are respectively placed at 16cm and 14cm upstream from the central temperature zone, and the substrate is placed at 10cm downstream from the central temperature zone.
5. A method for preparing a two-dimensional ZnTe crystal material as defined in claim 1, wherein the temperature rising rate of the central temperature zone is 30 to 40 ℃/min.
6. A method for preparing a two-dimensional ZnTe crystalline material according to claim 1, wherein the carrier gas is a mixed gas of argon and hydrogen, and the flow rate of argon is 50 seem.
7. A method for the preparation of a two-dimensional ZnTe crystal material according to any one of claims 1 to 6, wherein the reaction is carried out in a single-temperature zone horizontal tube furnace with a 25mm external diameter of the tube orifice, wherein the length of the central temperature zone is 10cm; the substrate is a fluorophlogopite sheet.
8. A two-dimensional ZnTe crystalline material, prepared by the method of any one of claims 1 to 7.
9. Use of a two-dimensional ZnTe crystal material as claimed in claim 8, characterized in that the two-dimensional ZnTe crystal material is used for optical encryption.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104962990A (en) * 2015-07-23 2015-10-07 华中科技大学 Preparation method of two-dimensional nano SnSe2 crystal material
CN105463580A (en) * 2016-01-07 2016-04-06 中国科学院理化技术研究所 Preparation method of cadmium selenide or cadmium sulfide two-dimensional single crystal nanosheet
CN111304747A (en) * 2020-04-01 2020-06-19 华中科技大学 Non-layered two-dimensional PbSe crystal material and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104962990A (en) * 2015-07-23 2015-10-07 华中科技大学 Preparation method of two-dimensional nano SnSe2 crystal material
CN105463580A (en) * 2016-01-07 2016-04-06 中国科学院理化技术研究所 Preparation method of cadmium selenide or cadmium sulfide two-dimensional single crystal nanosheet
CN111304747A (en) * 2020-04-01 2020-06-19 华中科技大学 Non-layered two-dimensional PbSe crystal material and preparation method thereof

Non-Patent Citations (2)

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Optical identification using imperfections in 2D materials;Yameng Cao et al.;《2D Materials》;20170928;参见摘要部分、第2页左栏第1段 *

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