CN114314659A - Two-dimensional inorganic molecular crystal Sb2O3Nano material, preparation method and application - Google Patents
Two-dimensional inorganic molecular crystal Sb2O3Nano material, preparation method and application Download PDFInfo
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- CN114314659A CN114314659A CN202111647168.8A CN202111647168A CN114314659A CN 114314659 A CN114314659 A CN 114314659A CN 202111647168 A CN202111647168 A CN 202111647168A CN 114314659 A CN114314659 A CN 114314659A
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Abstract
The invention discloses a two-dimensional inorganic molecular crystal Sb2O3Nanometer material, preparation method and application. The preparation method comprises the following steps: in Sb2O3Setting a substrate at a predetermined distance above the raw material, and aligning Sb2O3Heating the raw material to make Sb2O3The raw material sublimes upwards and deposits on the surface facing Sb2O3On a substrate of raw material to obtain a two-dimensional inorganic molecular crystal Sb formed on the substrate2O3And (3) nano materials. The invention improves the preparation process of the gas phase method to prepare the two-dimensional molecular crystal Sb with large size, regular shape and high crystallinity2O3And (3) nano materials. Therefore, the technical problems of high equipment cost, high energy consumption, small sample size, poor controllability of preparation conditions and the like in the conventional vapor deposition manufacturing method are solved.
Description
Technical Field
The invention belongs to the technical field of two-dimensional materials, and particularly relates to a two-dimensional inorganic molecular crystal Sb2O3Nanometer material, preparation method and application.
Background
The two-dimensional molecular crystal has molecular-level thickness, diversified molecular structure, effective charge transmission, easy realization of large-area preparation, and good effectPhysical flexibility and the like; has attracted people's attention in the fields of transistor, light detection, etc. Recently, Korea et al succeeded in preparing a two-dimensional inorganic molecular crystal Sb2O3The family of two-dimensional molecular crystals is expanded from organic molecules to inorganic molecules (see non-patent document nat. Commun.2019,10,4728.), and a new research field, namely two-dimensional inorganic molecular crystals, is opened up. As a typical representative of two-dimensional inorganic molecular crystals, Sb2O3Unlike conventional organic molecular crystals: (1) sb2O3The inorganic molecule does not contain a carbon skeleton side chain and a benzene ring, and the molecular structure is simpler; (2) sb2O3The inorganic molecule has extremely excellent thermal stability and air stability; (3) sb2O3Inorganic molecules have large band gaps and good dielectric properties, and have wide application potential in the field of dielectric layer materials (see non-patent literature Nat Commun 2020,11,2502.). Therefore, a simple, efficient, low-cost and environment-friendly preparation method is developed to realize the two-dimensional inorganic molecular crystal Sb2O3The controllable preparation of the material has important scientific research and application value.
The existing two-dimensional inorganic molecular crystal preparation technology mainly comprises a solution method and a gas phase method. Two-dimensional molecular crystals prepared by a solution method often have solvent residues, small size and poor crystallinity, and are harsh and long-consuming in preparation conditions (see non-patent literature chem.soc.rev.2019,48,1492.). The two-dimensional molecular crystal prepared by the gas phase method has high crystallinity and few defects, and is considered to be the Sb for preparing the two-dimensional inorganic molecular crystal2O3Good experimental scheme of nano material. However, two-dimensional inorganic molecular crystal Sb2O3The existing preparation scheme of the nano material faces many challenges such as low utilization rate of raw materials, small size of prepared samples, poor controllability of experimental conditions, high equipment cost, high energy consumption and the like (see non-patent documents nat. Commun.2019,10,4728; adv. Opt. Mater.2020,8,2000168.). Therefore, an environment-friendly, simple, efficient and low-cost vapor phase method preparation scheme is developed for preparing the two-dimensional inorganic crystal Sb2O3The nano material has important significance.
Disclosure of Invention
In response to the above-mentioned drawbacks or needs for improvement of the prior art, the present invention provides a two-dimensional inorganic molecular crystal Sb2O3The purpose of the nano material is to prepare a large-size, regular-shape and high-crystallinity two-dimensional molecular crystal Sb by improving a gas phase method preparation process2O3And (3) nano materials. Therefore, the technical problems of high equipment cost, high energy consumption, small sample size, poor controllability of preparation conditions and the like in the conventional vapor deposition manufacturing method are solved.
To achieve the above object, according to one aspect of the present invention, there is provided a two-dimensional inorganic molecular crystal Sb2O3A method of preparing a nanomaterial comprising: in Sb2O3Setting a substrate at a predetermined distance above the raw material, and aligning Sb2O3Heating the raw material to make Sb2O3The raw material sublimes upwards and deposits on the surface facing Sb2O3On a substrate of raw material to obtain a two-dimensional inorganic molecular crystal Sb formed on the substrate2O3And (3) nano materials.
Preferably, said pair Sb2O3Heating the raw materials, specifically: sb2O3Placing the powder on a heating plate for heating to Sb2O3The temperature of the powder is heated to 420-650 ℃.
Preferably, the heating time is 30s-20 min.
Preferably, the preset distance is less than or equal to 1 cm.
Preferably, the substrate is a mica substrate.
According to another aspect of the present invention, there is provided a two-dimensional inorganic molecular crystal Sb2O3And (3) nano materials.
Preferably, the two-dimensional inorganic molecular crystal Sb2O3The nano material is alpha phase.
According to still another aspect of the present invention, there is provided a two-dimensional inorganic molecular crystal Sb2O3Use of nanomaterials as semiconductorsDielectric material in the device.
In general, at least the following advantages can be obtained by the above technical solution contemplated by the present invention compared to the prior art.
(1) The preparation method provided by the invention has the advantages of simple equipment, low cost and short synthesis time, and avoids expensive equipment requirements and severe growth conditions of the traditional gas phase method. And no carrier gas is input in the reaction process, so that a turbulent airflow environment is avoided, and a stable material growth environment is provided. Meanwhile, the two-dimensional Sb prepared by the invention2O3The molecular crystal has smooth surface, regular appearance and high crystallinity, and has wide application prospect in the field of photoelectronic devices.
(2) In the invention, raw material Sb2O3The powder is vertically sublimated upwards for a small distance to participate in the reaction, so that Sb is shortened2O3The transportation distance improves the utilization rate of the raw materials.
(3) According to the invention, through the change of heating conditions and preset distances, high-quality two-dimensional Sb with different thicknesses and sizes can be prepared2O3And (4) molecular crystals.
Drawings
FIG. 1 is a two-dimensional inorganic molecular crystal Sb prepared in example 12O3A schematic diagram of a device structure of the nano material;
in FIG. 2, (a) to (f) are two-dimensional inorganic molecular crystals Sb prepared in examples 1 to 6, respectively2O3Optical microscope photograph of the nano material;
in FIG. 3, (a) and (b) are two-dimensional inorganic molecular crystals Sb prepared in example 52O3Atomic force microscope pictures and height measurement pictures of the nano materials;
FIG. 4 shows two-dimensional inorganic molecular crystal Sb prepared in example 12O3A Raman spectrum of the nanomaterial;
FIG. 5 shows two-dimensional inorganic molecular crystal Sb prepared in example 12O3An X-ray diffraction pattern of the nanomaterial;
in FIG. 6, (a) and (b) are each the two-dimensional inorganic particles prepared in example 1Molecular crystal Sb2O3The Sb element composition analysis chart and the O element composition analysis chart of the nano material;
FIG. 7 shows a two-dimensional inorganic molecular crystal Sb prepared in example 12O3Selected area electron diffraction patterns of nanomaterials.
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.
The invention provides a two-dimensional inorganic molecular crystal Sb2O3A method of preparing a nanomaterial comprising: in Sb2O3Setting a substrate at a predetermined distance above the raw material, and aligning Sb2O3Heating the raw material to make Sb2O3The raw material sublimes upwards and deposits on the surface facing Sb2O3On a substrate of raw material to obtain a two-dimensional inorganic molecular crystal Sb formed on the substrate2O3And (3) nano materials.
In some embodiments, the pair of Sb2O3Heating the raw materials, specifically: sb2O3Heating the raw materials on a heating plate to make Sb2O3The temperature of the raw material is heated to 420-650 ℃. The heating time is 30s-20 min. The preset distance is less than or equal to 1 centimeter. The substrate is a mica substrate.
In some embodiments, Sb placement on the carrier sheet may be employed, as shown in fig. 12O3Raw materials, the mica substrate is erected on two sides through glass sheets with preset thickness, so that Sb can be adjusted by changing the thickness of the glass sheets2O3The distance between the raw material and the mica substrate is increased by arranging a heating plate at the bottom of the carrier plate to align Sb2O3The raw materials are heated.
The invention also provides a two-dimensional inorganic molecular crystal Sb2O3Nanomaterial, the two-dimensional inorganic molecular crystal Sb2O3The nano material is alpha phase.
The invention also provides a two-dimensional inorganic molecular crystal Sb2O3Application of nano material as dielectric material in semiconductor device.
The technical solution of the present invention is further illustrated by the following specific examples.
Example 1
This example provides a two-dimensional inorganic molecular crystal Sb2O3Preparation method of nano material and two-dimensional inorganic molecular crystal Sb prepared by method2O3And (3) nano materials.
FIG. 1 shows a method for preparing a two-dimensional inorganic molecular crystal Sb according to the present invention2O3Schematic diagram of device structure of nano material.
As shown in FIG. 1, the heating plate is first heated to a desired temperature of 500 ℃ for use; then 2mg of commercially available Sb was weighed out2O3Powder was spread in the center of a glass slide and placed on a hot plate, and Sb2O3Two glass sheets with the thickness of 1mm are also placed on the two sides of the powder; placing the cut mica substrate on the above-mentioned two-sided glass sheet so that the substrate and Sb are in contact2O3The powders were separated by a 1mm pitch; waiting for 4 minutes to obtain high-quality two-dimensional inorganic molecular crystal Sb on the mica substrate2O3And (3) nano materials.
Example 2
This example provides a two-dimensional inorganic molecular crystal Sb2O3Preparation method of nano material and two-dimensional inorganic molecular crystal Sb prepared by method2O3And (3) nano materials.
This example was prepared following the same procedure as in example 1, except that Sb2O3The powder heating temperature was 540 ℃.
Example 3
This example provides a two-dimensional inorganic molecular crystal Sb2O3Preparation method of nano material and two-dimensional inorganic molecular crystal Sb prepared by method2O3And (3) nano materials.
This example was prepared following the same procedure as in example 1, except that Sb2O3The powder heating temperature was 460 ℃.
Example 4
This example provides a two-dimensional inorganic molecular crystal Sb2O3Preparation method of nano material and two-dimensional inorganic molecular crystal Sb prepared by method2O3And (3) nano materials.
This example was prepared following the same procedure as in example 1, except that a mica substrate was placed in the Sb2O3The heating time above the powder was 10 minutes.
Example 5
This example provides a two-dimensional inorganic molecular crystal Sb2O3Preparation method of nano material and two-dimensional inorganic molecular crystal Sb prepared by method2O3And (3) nano materials.
This example was prepared following the same procedure as in example 1, except that a mica substrate was placed in the Sb2O3The heating time above the powder was 1 minute.
Example 6
This example provides a two-dimensional inorganic molecular crystal Sb2O3Preparation method of nano material and two-dimensional inorganic molecular crystal Sb prepared by method2O3And (3) nano materials.
This example was prepared following the same procedure as in example 1, except that the mica substrate and Sb were used2O3The vertical spacing of the powders was fixed at 2 mm.
Results and analysis
Two-dimensional inorganic molecular crystals Sb prepared in examples 1 to 6 were each subjected to an optical microscope2O3Characterization of surface morphology of nano-materialsThe results are shown in fig. 2 (a), fig. 2 (b), fig. 2 (c), fig. 2 (d), fig. 2 (e) and fig. 2 (f), respectively. As can be seen from fig. 2 (a), fig. 2 (d), fig. 2 (e) and fig. 2 (f), the materials prepared by the examples have regular shapes, smooth surfaces and good crystallization quality. Comparing fig. 2 (a) with fig. 2 (b) and fig. 2 (c), it can be seen that temperature has a significant effect on the synthesis of the material; high heating temperatures cause the material to join into a thin film, while low heating temperatures result in material morphology irregularities and poor crystallinity. Comparing fig. 2 (a) with fig. 2 (d) and fig. 2 (e), it can be seen that the heating time of the substrate can affect the obtaining of the two-dimensional inorganic molecular crystal Sb2O3The size and thickness of the material; the sample prepared by short heating time is small in size and thin in thickness, and the sample prepared by long heating time is large in size and thick. Comparing FIG. 2 (a) with FIG. 2 (f), it can be seen that by changing the substrate and Sb2O3The distance between the raw materials indirectly adjusts the temperature of the mica substrate and also has a significant effect on the size and thickness of the sample.
Method for scanning sample surface with atomic force microscope probe for the two-dimensional inorganic molecular crystal Sb prepared in example 52O3Measuring the thickness of the nano material; as shown in (a) and (b) of FIG. 3, the two-dimensional Sb prepared in example 5 was measured2O3The thickness of the nano material can be as thin as 2.7 nm.
Two-dimensional Sb prepared in example 1 was subjected to confocal Raman spectroscopy2O3The nano material is subjected to a characterization test of Raman spectrum, and the test result is shown in figure 4. Raman peaks appearing in the figure and the literature reported alpha-Sb2O3The positions of the Raman peaks remained the same, confirming that the prepared Sb2O3The nano material is alpha phase.
X-ray diffraction of the two-dimensional Sb prepared in example 12O3The nano material is subjected to characterization tests of phase and structure, and the test result is shown in figure 5. Sb in the figure2O3The sharp diffraction peak of the nanosheet can be well corresponding to the crystal face of the standard PDF card, no redundant diffraction peak appears, and the high-crystallinity prepared sample is disclosedQuality and high purity.
Two-dimensional Sb prepared in example 1 was subjected to energy dispersive X-ray spectroscopy2O3The nanomaterial was subjected to elemental composition analysis, and the test results are shown in (a) and (b) of fig. 6. The Sb element and the O element on the sample are uniformly distributed, which shows that the surface of the sample is smooth and flat, the thickness of the sample is uniform, and the crystallization quality of the sample is good.
Two-dimensional Sb prepared in example 1 was subjected to a transmission electron microscope2O3The nano material is subjected to structural characterization, and the electron diffraction pattern of the nano material is shown in figure 7; the band axis of the electron diffraction pattern is [111 ]]The crystal orientation, and the X-ray diffraction pattern results in fig. 5 can be matched.
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 (7)
1. Two-dimensional inorganic molecular crystal Sb2O3The preparation method of the nano material is characterized by comprising the following steps: in Sb2O3Setting a substrate at a predetermined distance above the raw material Sb2O3Heating is carried out so that Sb2O3Sublimed upwards and deposited on the surface facing the raw material Sb2O3To obtain a two-dimensional inorganic molecular crystal Sb formed on the substrate2O3And (3) nano materials.
2. The method according to claim 1, wherein the para-Sb is2O3Heating the raw material to Sb2O3The temperature of the raw material is heated to 420-650 ℃.
3. The method of claim 1, wherein the heating time is from 30s to 20 min.
4. The method of claim 1, wherein the predetermined distance is less than or equal to 1 cm.
5. Two-dimensional inorganic molecular crystal Sb prepared by the method according to any one of claims 1 to 42O3And (3) nano materials.
6. The two-dimensional inorganic molecular crystal Sb of claim 52O3Nanomaterial characterized in that the two-dimensional inorganic molecular crystal Sb2O3The nano material is alpha phase.
7. The two-dimensional inorganic molecular crystal Sb of claim 5 or 62O3Use of nanomaterials as dielectric materials in semiconductor devices.
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Citations (5)
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| US20030230238A1 (en) * | 2002-06-03 | 2003-12-18 | Fotios Papadimitrakopoulos | Single-pass growth of multilayer patterned electronic and photonic devices using a scanning localized evaporation methodology (SLEM) |
| CN106917064A (en) * | 2017-02-16 | 2017-07-04 | 上海大学 | Single step original position flash method growth ABX3The preparation method of type perovskite thin film |
| CN111621746A (en) * | 2020-05-29 | 2020-09-04 | 华中科技大学 | Van der Waals dielectric material and preparation method and application thereof |
| CN112185804A (en) * | 2020-09-22 | 2021-01-05 | 华中科技大学 | Structure of inorganic molecular crystal packaging two-dimensional material and packaging and de-packaging method thereof |
| CN112456553A (en) * | 2020-12-10 | 2021-03-09 | 温州大学新材料与产业技术研究院 | Preparation method for controllably synthesizing two-dimensional antimony trioxide molecular crystal by using hot plate |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030230238A1 (en) * | 2002-06-03 | 2003-12-18 | Fotios Papadimitrakopoulos | Single-pass growth of multilayer patterned electronic and photonic devices using a scanning localized evaporation methodology (SLEM) |
| CN106917064A (en) * | 2017-02-16 | 2017-07-04 | 上海大学 | Single step original position flash method growth ABX3The preparation method of type perovskite thin film |
| CN111621746A (en) * | 2020-05-29 | 2020-09-04 | 华中科技大学 | Van der Waals dielectric material and preparation method and application thereof |
| CN112185804A (en) * | 2020-09-22 | 2021-01-05 | 华中科技大学 | Structure of inorganic molecular crystal packaging two-dimensional material and packaging and de-packaging method thereof |
| CN112456553A (en) * | 2020-12-10 | 2021-03-09 | 温州大学新材料与产业技术研究院 | Preparation method for controllably synthesizing two-dimensional antimony trioxide molecular crystal by using hot plate |
Non-Patent Citations (2)
| Title |
|---|
| A.L.J.PEREIRA ET AL.: "Structural and vibrational study of cubic Sb2O3 under high pressure", 《PHYSICAL REVIEW B》 * |
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