CN116002752A - Chiral bismuth oxyhalide two-dimensional material containing ytterbium ions and silver and preparation method thereof - Google Patents
Chiral bismuth oxyhalide two-dimensional material containing ytterbium ions and silver and preparation method thereof Download PDFInfo
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- 229910052709 silver Inorganic materials 0.000 title claims abstract description 16
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- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(iii) oxide Chemical compound O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims abstract description 14
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- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 8
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 claims abstract description 7
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- 239000000126 substance Substances 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 4
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 claims description 2
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- 125000003827 glycol group Chemical group 0.000 claims description 2
- 229910052736 halogen Inorganic materials 0.000 claims description 2
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910000510 noble metal Inorganic materials 0.000 claims description 2
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims 7
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Abstract
The invention discloses a chiral bismuth oxyhalide two-dimensional material containing ytterbium and erbium ions and silver, which has the expression of BiYbErOX-Ag-Y, wherein X is Cl or Br, Y is D-sorbitol, and the preparation method comprises the following steps: dissolving ytterbium oxide and erbium oxide in concentrated nitric acid, dissolving all raw materials in an organic solvent, uniformly stirring, and regulating the pH value; heating and then preserving heat in a hydrothermal kettle; washing, drying and heat treating to obtain the final product. The material provided by the invention is an inorganic nonmetallic semiconductor and information functional material, has good light response characteristic, has stronger chiral light modulation efficiency and higher CD value than natural materials, can be used as a novel nano material, is used for scientific research in the fields of catalysis, luminescence and the like, and increases the exploration range of the chiral material scientific research field; the preparation method has the advantages of easy operation, easy control of operation conditions and easy preparation of two-dimensional materials with various morphologies.
Description
Technical Field
The invention belongs to the technical field of inorganic nonmetallic semiconductors and information functional materials, and particularly relates to a chiral bismuth oxyhalide two-dimensional material containing ytterbium and erbium ions and silver and a preparation method thereof.
Background
The present researches on chiral science and technology cover the fields of preparation of chiral compounds such as medicines, fine chemistry and the like, chiral display, sensing, optical devices and the like. With the continuous development of technology, chiral science can better serve the health and high-quality life of human beings, and meanwhile, the demand of chiral materials is increasing. Along with the increasing abundance of synthesis and characterization means, related fields such as crystal engineering, molecular engineering and the like are mature, various chiral crystalline materials with novel structures are sequentially synthesized, and great application potential is shown in the chiral science field.
In the current research, the main problems are: the interaction between the chiral material of the natural substance and light is weak, so that the application of the chiral photoresponsive property of the natural substance in luminescence and chiral catalysis is limited. The rare earth doped up-conversion material can convert near infrared photons into visible light or ultraviolet photons, and has potential in the aspects of anti-counterfeiting ink, 3D display, wavelength conversion layers of solar cells, fluorescent probes for biological imaging and drug delivery and the like. However, since the excitation cross section of the rare earth ion is small and the radiative transition rate of the odd-even forbidden 4f shell transition is low, the up-conversion luminescence intensity is often insufficient for practical application. In order to improve the upconversion efficiency, researchers have utilized surface plasmon resonance of metal nanostructures. A variety of composite Nanoparticles (NPs) consisted of upconverting materials and metallic nanostructures and demonstrated enhancement of upconverting. Therefore, on the basis, the chiral material is combined with the surface plasmon resonance of the Ag nano structure to enhance up-conversion luminescence.
Therefore, in order to solve the problems, a chiral bismuth oxyhalide two-dimensional material containing ytterbium and erbium ions and silver and a preparation method thereof are provided.
Disclosure of Invention
In order to solve the technical problems, the invention designs the chiral bismuth oxyhalide two-dimensional material containing ytterbium and erbium ions and silver and the preparation method thereof.
In order to achieve the technical effects, the invention is realized by the following technical scheme: the chiral bismuth oxyhalide two-dimensional material containing ytterbium ions and silver is characterized in that the chemical formula is BiYbErOX-Ag-Y; wherein X is one or more of Cl and Br, Y is D-sorbitol, and the chemical formula is C 6 H 14 O 6 。
The invention further aims at providing a preparation method of the chiral bismuth oxyhalide two-dimensional material containing ytterbium and erbium ions and silver, which is characterized by comprising the following steps of:
step1, raw material preparation: the molar ratio of Bi ion to Yb ion to Er ion to Ag ion to D-SOr is = (1-w-x) to w/x/y/z, wherein w=0.05-0.3, x=0.001-0.1, y=0.01-7,z =0.1-6, bismuth nitrate, ytterbium oxide, erbium oxide, silver nitrate, halogen salt and fructose are used as raw materials;
step2, firstly dissolving ytterbium oxide and erbium oxide by using concentrated nitric acid, then dissolving all raw materials in an organic solvent to prepare a solution with the molar concentration of 0.5-2.5 mol/L, and regulating the pH value to 2-6 after uniformly stirring;
step3, transferring the mixture into a hydrothermal kettle, wherein the filling degree is 0.4-0.8, then heating to 110-250 ℃, and preserving heat for 2-25 hours;
washing and drying the materials obtained in Step4 and Step3, and performing heat treatment at 300-600 ℃ for 1-5 hours to obtain the chiral bismuth oxyhalide two-dimensional material of ytterbium-erbium-doped rare earth ion noble metal silver with the chemical formula of BiYbErOX-Ag-D-Sor.
Further, the organic solvent is glycol solution or glycol aqueous solution.
Further, hydrochloric acid, nitric acid, KOH solution and NaOH solution are used for adjusting the pH value in Step 2.
Further, the hydrothermal kettle in Step3 is provided with a polytetrafluoroethylene lining.
Further, the Step4 is washed three times with deionized water and ethanol.
The beneficial effects of the invention are as follows:
the preparation method greatly reduces the difficulty of material preparation and the requirement on the professional of operators, can prepare two-dimensional materials with various morphologies by considering control, has stable physical and chemical properties, is available in raw material preparation and has low cost, and the material can be used as a novel nano material and has stronger chiral light modulation efficiency and higher CD value (circular dichroism) than natural materials.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is an XRD pattern of BiYbErOCl-Ag-D-SOr material prepared in example 1;
FIG. 2 is an XRD pattern of the BiYbErOBr-Ag-D-SOr material prepared in example 2;
FIG. 3 is an SEM image of a BiYbErOCl-Ag-D-SOr material prepared in example 1;
FIG. 4 is an SEM image of a BiYbErOBr-Ag-D-SOr material prepared in example 2;
FIG. 5 is a graph of chiral CD values for BiYbErOCl-Ag material;
FIG. 6 is a graph of chiral CD values for BiYbErOCl-Ag-D-SOr material;
FIG. 7 is a chiral CD value map of BiYbErOBr-Ag-D-SOr material;
FIG. 8 is a graph of the comparative luminous intensity of BiYbErOCl-Ag-D-SOr material versus a base sample BiYbErOCl-Ag material;
fig. 9 is an additional pictorial view of a chiral material structure.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Referring to fig. 1 to 9, the chemical formula of the chiral bismuth oxyhalide two-dimensional powder material is BiYbErOCl-Ag-D-SOr; the preparation method of the material comprises the following steps:
(1) The molar ratio of Bi ion to Yb ion to Ag ion to D-SOr to Cl ion=0.94:0.05:0.01:5:0.1:1, and Bi (NO 3 ) 3 ·5H 2 O、Yb 2 O 3 、Er 2 O 3 、AgNO 3 Dissolving ytterbium oxide and erbium oxide in concentrated nitric acid, and dissolving all the raw materials in an organic solvent glycol solution or a mixed solution formed by water and the organic solvent glycol to prepare a solution with the concentration of 1 mol/L; then adding the solution into a container, stirring and mixing uniformly, regulating the pH value to 4 by hydrochloric acid with the concentration of 1mol/L, and transferring into a hydrothermal kettle with a polytetrafluoroethylene lining, wherein the filling degree is0.4, then heating to 160 ℃, and preserving heat for 12 hours;
(2) And (3) respectively washing the material obtained in the step (1) with deionized water and ethanol for three times, drying, and performing heat treatment at 300 ℃ for 3 hours to obtain the chiral bismuth oxyhalide two-dimensional material with the chemical composition formula of BiYbErOCl-Ag-D-SOr, wherein an XRD pattern is shown as a figure 1, and the XRD result shows that the BiYbErOCl-Ag doped with 0.1mmol of D-sorbitol has obvious and sharp diffraction peaks, the peak positions are highly matched with the BiOCl with the layered structure of JCPDS card number 06-0249, and the peak positions are the same as the peak positions of Ag of JCPDS card number PDF#04-0783. It was demonstrated that Ag was also successfully complexed to BiYbErOCl. The material presents a sparse and loose-state dextrorotatory flower ball morphology structure under an SEM scanning electron microscope, the SEM morphology is shown as a figure 3, when a circular dichroism instrument is adopted for testing, the chiral CD value is found to be positive, the peak value is obvious, and the property and the function of the chiral material are proved to be endowed with the chirality, as shown in a figure 6.
Example 2
The chemical formula of the chiral bismuth oxyhalide two-dimensional powder material is BiYbErOBr-Ag-D-SOr; the preparation method of the material comprises the following steps:
(1) The molar ratio of Bi ion, yb ion, er ion, ag ion, D-SOr, br ion=0.6:0.3:0.1:7:5:1, and Bi (NO 3 ) 3 ·5H 2 O、Yb 2 O 3 、Er 2 O 3 、AgNO 3 Dissolving ytterbium oxide and erbium oxide in concentrated nitric acid, dissolving all the raw materials in an organic solvent glycol solution or a mixed solution formed by water and the organic solvent glycol to prepare solutions with the concentration of 2mol/L respectively, adding the solutions into a container, stirring and mixing uniformly, regulating the pH value to 3 by using nitric acid with the concentration of 0.5mol/L, transferring the solution into a hydrothermal kettle with a polytetrafluoroethylene lining, wherein the filling degree is 0.6, then heating to 140 ℃, and preserving heat for 24 hours;
(2) And (3) respectively washing the material obtained in the step (1) with deionized water and ethanol for three times, drying, and performing heat treatment at 400 ℃ for 2 hours to obtain the chiral bismuth oxyhalide two-dimensional material with the chemical composition formula of BiYbErOBr-Ag-D-SOr, wherein an XRD pattern is shown as a graph 2, and the XRD result shows that the BiYbErOBr-Ag doped with 5mmol of dextrorotatory sorbitol has obvious and sharp diffraction peaks, the peak position is highly matched with the BiOBr with the layered structure of JCPDS card number 09-0393, and the peak position is the same as the peak position of the Ag of JCPDS card number PDF#04-0783. It was demonstrated that Ag was also successfully complexed to BiYbErOBr. The material presents a sparse and loose-state dextrorotation flower ball morphology structure under an SEM scanning electron microscope, and the SEM morphology is shown as figure 4. When tested by a circular dichroism instrument, the chiral CD value is found to be positive, the maximum value is about 65mdeg, and the peak value is obvious. It was confirmed that it imparts chiral properties and functions as shown in fig. 7.
FIG. 5 is a graph of chiral CD values for BiYbErOCl-Ag material, showing that pure BiYbErOCl-Ag has no helical chiral structure when tested with a circular dichroism instrument, as found to be 0.
FIG. 8 is a graph of the luminescence intensity of BiYbErOCl-Ag-D-SOr material under 980nm laser excitation compared with that of the as-received BiYbErOCl-Ag material, demonstrating that the chiral right-handed sorbitol doped BiYbErOCl-Ag (BiYbErOCl-Ag-D-SOr) has a greater luminescence intensity and can be used for up-conversion luminescence exploration.
Fig. 9 is an additional pictorial view of the chiral material structure, visually illustrating the existence of a twisted helical structure in the chiral material itself.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.
Claims (6)
1. The chiral bismuth oxyhalide two-dimensional material containing ytterbium ions and silver is characterized in that the chemical formula is BiYbErOX-Ag-Y; wherein X is one or more of Cl and Br, Y is D-sorbitol, and the chemical formula is C 6 H 14 O 6 。
2. The preparation method of the chiral bismuth oxyhalide two-dimensional material containing ytterbium and erbium ions and silver is characterized by comprising the following steps of:
step1, raw material preparation: the molar ratio of Bi ion to Yb ion to Er ion to Ag ion to D-SOr is = (1-w-x) to w/x/y/z, wherein w=0.05-0.3, x=0.001-0.1, y=0.01-7,z =0.1-6, bismuth nitrate, ytterbium oxide, erbium oxide, silver nitrate, halogen salt and fructose are used as raw materials;
step2, firstly dissolving ytterbium oxide and erbium oxide by using concentrated nitric acid, then dissolving all raw materials in an organic solvent to prepare a solution with the molar concentration of 0.5-2.5 mol/L, and regulating the pH value to 2-6 after uniformly stirring;
step3, transferring the mixture into a hydrothermal kettle, wherein the filling degree is 0.4-0.8, then heating to 110-250 ℃, and preserving heat for 2-25 hours;
washing and drying the materials obtained in Step4 and Step3, and performing heat treatment at 300-600 ℃ for 1-5 hours to obtain the chiral bismuth oxyhalide two-dimensional material of ytterbium-erbium-doped rare earth ion noble metal silver with the chemical formula of BiYbErOX-Ag-D-Sor.
3. The method for preparing the chiral bismuth oxyhalide two-dimensional material containing ytterbium and erbium ions and silver according to claim 2, which is characterized in that: the organic solvent is glycol solution or glycol water solution.
4. The method for preparing the chiral bismuth oxyhalide two-dimensional material containing ytterbium and erbium ions and silver according to claim 2, which is characterized in that: and the pH value of Step2 is regulated by using hydrochloric acid, nitric acid, KOH solution and NaOH solution.
5. The method for preparing the chiral bismuth oxyhalide two-dimensional material containing ytterbium and erbium ions and silver according to claim 2, which is characterized in that: the hydrothermal kettle in Step3 is provided with a polytetrafluoroethylene lining.
6. The method for preparing the chiral bismuth oxyhalide two-dimensional material containing ytterbium and erbium ions and silver according to claim 2, which is characterized in that: the Step4 is washed three times with deionized water and ethanol.
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