CN113443609A - Novel-phase two-dimensional galena silver telluride synthesized based on two-dimensional tellurium template method and preparation method and application thereof - Google Patents
Novel-phase two-dimensional galena silver telluride synthesized based on two-dimensional tellurium template method and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a method for synthesizing new-phase two-dimensional galena silver telluride based on a two-dimensional tellurium template method, a preparation method and application thereof, wherein the stoichiometric ratio of silver to tellurium is 4.53:3, and the method comprises the following steps: dissolving sodium tellurite and polyvinylpyrrolidone in deionized water, stirring by a magnetic stirrer to fully disperse and dissolve the solution, adding hydrazine hydrate and an alkaline solution, placing the solution into a hydrothermal reaction kettle, sealing the hydrothermal reaction kettle, placing the hydrothermal reaction kettle into an oven for reaction, centrifugally washing the obtained solution to obtain a solution containing silver gray two-dimensional tellurium nanocrystals, dissolving silver nitrate in deionized water to obtain a silver nitrate solution, dropwise adding the silver nitrate solution into the solution containing silver gray two-dimensional tellurium nanocrystals, stirring the solution at room temperature for reaction, and continuously dropwise adding the silver nitrate solution until the silver gray solution turns into yellow green. The invention has high stability and simple method, has an asymmetric central structure and is applied as a nano piezoelectric generator.
Description
Technical Field
The invention relates to the technical field of preparation of two-dimensional nano materials, in particular to a method for synthesizing a new phase of two-dimensional galena silver telluride based on a two-dimensional tellurium template method and a preparation method and application thereof.
Background
Chalcogenide tellurides exhibit exceptional performance and potentially enormous applications in many areas of information technology, semiconductor science, photovoltaics and thermoelectricity. Silver tellurideThe semiconductor with a narrow band gap has great magnetoresistance effect, good conductivity and potential thermoelectric performance. In this system of silver telluride, the ratio of silver to tellurium can be between 1:1 and 1:2, and the three ratios determine the crystal structure and the behaviour thereof to be quite different. The three compounds are respectively tellurium-silver ore (expressate) AgTe and Herssite (hessit) Ag2Te and galena (stuetizite) Ag4.53Te3. AgTe and Ag2The synthesis and properties of nanocrystals of Te are of great interest and research. However, research on galena is limited by the high difficulty of synthesis, the difficulty of controlling the reaction product, and the relatively complex structure. Of the three compounds, galena Ag4.53Te3Has a crystal structure of P-62m space group, so that it has the characteristic of non-centrosymmetric structure. Therefore, in addition to its own thermoelectric properties, it can also be used as a piezoelectric material in a self-powered system. Finally, the two-dimensional galena Ag of atomic thickness4.53Te3The preparation and characterization of (A) has not been reported.
The liquid phase method is often employed as a low cost, efficient and flexible method. If the two elements are directly reacted, many byproducts are easy to appear, and the morphology, crystallinity and stoichiometric ratio of the product are difficult to control. Therefore, the introduction of the template method to study the formation of two-dimensional galena Ag4.53Te3It becomes important to maintain the morphology and higher crystallinity of the two-dimensional tellurium sheet template.
Disclosure of Invention
The invention aims to provide a novel phase two-dimensional galena silver telluride synthesized based on a two-dimensional tellurium template method, a preparation method and application thereof4.53Te3Can be used for researching experiment of generating piezoelectric charge by nano piezoelectric generator, thereby being a new phase two-dimensional galena Ag4.53Te3Research provides experimental data support, and is wideThe flexible wearable device can be widely applied to flexible wearable devices such as flat panel displays and solar cells to provide theoretical basis.
The invention relates to a method for synthesizing new phase two-dimensional galena silver telluride based on a two-dimensional tellurium template method, wherein the stoichiometric ratio of silver to tellurium is 4.53: 3.
The invention relates to a preparation method for synthesizing new phase two-dimensional galena silver telluride based on a two-dimensional tellurium template method, which comprises the following steps:
s1: stirring and dissolving sodium tellurite and polyvinylpyrrolidone in a molar ratio of 52.4:1 in 25-33ml of deionized water to obtain a solution A, mixing hydrazine hydrate and an alkaline solution in a volume ratio of 1:2 to form a solution B, adding the solution B and the solution A in a volume ratio of 0.15-0.2 into the solution A, placing the solution B and the solution A into a hydrothermal reaction kettle, sealing, and placing the solution into an oven for reaction to obtain a product C.
S2: and centrifuging and washing the product C to obtain a solution D containing silver gray two-dimensional tellurium nanocrystals.
S3: dissolving silver nitrate in deionized water to obtain a silver nitrate solution with the concentration of 1-10mg/mL, dropwise adding the silver nitrate solution into the solution D, wherein the volume ratio of the solution D to the silver nitrate solution is 10:1-10:5, stirring at room temperature for reaction, continuously dropwise adding the silver nitrate solution when the silver gray solution becomes yellow green, and generating the two-dimensional galena Ag after the reaction is finished when the yellow green solution becomes grey green4.53Te3。
Further, the deionized water in the steps S1, S2, and S3 has a conductivity of 18.2M Ω.
Further, the concentration of the solution A in the step S1 is 0.014mol/L-0.018 mol/L.
Further, the alkaline solution in step S1 is ammonia water.
Further, the molecular weight of the polyvinylpyrrolidone in the step S1 is 58000.
Further, the temperature of the oven in the step S1 is 160-200 ℃, and the reaction time is 30-36 h.
Further, in step S2, the centrifugal washing process is: centrifuging the product C by a centrifuge at the rotating speed of 3000-.
Further, the concentration of the silver nitrate solution in the step S3 is 2.5 mg/mL.
The invention also provides application of the novel phase two-dimensional galena silver telluride synthesized based on the two-dimensional tellurium template method in a nano generator.
The invention has the beneficial effects that:
1. the invention takes the two-dimensional tellurium sheets as templates, realizes chemical conversion, prepares the high-quality and high-crystallinity two-dimensional silver telluride sheets, and synthesizes the two-dimensional galena Ag on a two-dimensional scale4.53Te3And two-dimensional galena Ag4.53Te3Has a non-centrosymmetric structure.
2. The invention carries out film coating forming on the two-dimensional silver telluride, so that the two-dimensional silver telluride can be applied to the nano generator on the flexible substrate.
Drawings
FIG. 1 shows two-dimensional galena Ag obtained in example 2 of the present invention4.53Te3Light microscope photograph.
FIG. 2 shows two-dimensional galena Ag obtained in example 2 of the present invention4.53Te3X-ray diffraction pattern of and according to Ag4.53Te3Structural features simulated X-ray diffraction patterns.
FIG. 3 shows two-dimensional galena Ag obtained in example 2 of the present invention4.53Te3EDS-mapping chart of tellurium element and silver element under transmission electron microscope.
FIG. 4 shows two-dimensional galena Ag obtained in example 2 of the present invention4.53Te3And (3) an atomic structure simulation diagram.
FIG. 5 shows two-dimensional galena Ag obtained in example 2 of the present invention4.53Te3Open circuit voltage of nanogenerator fabricated from core material.
FIG. 6 shows two-dimensional galena Ag obtained in example 3 of the present invention4.53Te3Light microscope photograph.
FIG. 7 shows Ag obtained in comparative example 2 of the present invention2X-ray diffraction pattern of Te and from Ag2Te structural characteristic modelpseudo-X-ray diffraction patterns.
Detailed Description
The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
s1: 0.1g of sodium tellurite and 0.5g of polyvinylpyrrolidone with the molecular weight of 58000 are dissolved in 30mL of deionized water with the conductivity of 18.2M omega cm, the mixture is stirred for 30 minutes under a magnetic stirrer to form a solution A with the concentration of 0.015mol/L, then 1.65mL of hydrazine hydrate and 3.3mL of ammonia water are mixed to form a solution B, the solution B is added into the solution A, the solution B is placed into a hydrothermal reaction kettle, the hydrothermal reaction kettle is sealed, and the solution B is reacted in a 180-degree oven for 36 hours to obtain a product C.
S2: and centrifuging the product C by using a centrifuge at the rotating speed of 5000rpm for 10 minutes to remove the upper-layer solution, and then adding acetone and deionized water with the conductivity of 18.2M omega cm into the centrifuge tube to repeatedly wash for three times to obtain a solution D containing silver gray two-dimensional tellurium nanosheet crystals.
S3: dissolving silver nitrate in deionized water with the conductivity of 18.2M omega-cm to obtain a silver nitrate solution with the concentration of 1mg/mL, dropwise adding 3mL of the silver nitrate solution into 37mL of the solution D, stirring and reacting at room temperature, continuously dropwise adding the silver nitrate solution when the silver gray solution becomes yellow-green, and generating the two-dimensional galena Ag after the reaction is finished when the yellow-green solution becomes grey-green4.53Te3。
Example 2:
s1: 0.1g of sodium tellurite and 0.5g of polyvinylpyrrolidone with the molecular weight of 58000 are dissolved in 33mL of deionized water with the conductivity of 18.2M omega cm, the mixture is stirred for 30 minutes under a magnetic stirrer to form a solution A with the concentration of 0.014mol/L, then 1.65mL of hydrazine hydrate and 3.3mL of ammonia water are mixed to form a solution B, the solution B is added into the solution A, the solution B is placed into a hydrothermal reaction kettle, the hydrothermal reaction kettle is sealed, and the solution B is reacted in a 160-DEG oven for 34 hours and taken out to obtain a product C.
S2: and centrifuging the product C by using a centrifuge at the rotating speed of 4500rpm for 10 minutes to remove the upper-layer solution, and then adding acetone and deionized water with the conductivity of 18.2M omega cm into the centrifuge tube to repeatedly wash for three times to obtain a solution D containing silver gray two-dimensional tellurium nanosheet crystals.
S3: dissolving silver nitrate in deionized water with the conductivity of 18.2M omega-cm to obtain a silver nitrate solution with the concentration of 2.5mg/mL, dropwise adding 5mL of the silver nitrate solution into 50mL of the solution D, stirring and reacting at room temperature, continuously dropwise adding the silver nitrate solution when the silver gray solution becomes yellow-green, and generating the two-dimensional galena Ag after the reaction is finished when the yellow-green solution becomes grey-green4.53Te3。
Using the two-dimensional galena Ag obtained in example 24.53Te3And (3) carrying out structural characterization:
the results of the measurement are shown in FIG. 1, which shows Ag4.53Te3Is a two-dimensional sheet crystal structure with the width of 15-25 microns, the length of 92-105 microns and the thickness of 40-50 nanometers;
the results of the X-ray diffraction measurements are shown in FIG. 2, where the red diffraction peak is the experimental result and the black diffraction peak is based on two-dimensional galena Ag4.53Te3The crystal structure simulates a structure, and the experimental result is completely consistent with the simulated peak position;
the EDS-mapping of the tellurium element and the silver element under a transmission electron microscope shows that the test results are shown in FIG. 3, and the red silver element and the green tellurium element in the graph are uniformly distributed on the nanosheets.
The test results obtained by atomic structure simulation are shown in fig. 4.
The two-dimensional galena Ag of example 2 was used4.53Te3And the application of the nano generator to generate piezoelectric charge is carried out:
the reaction product obtained in example 2, two-dimensional galena Ag4.53Te3Washing with deionized water for three times, dispersing in ethanol solution, uniformly coating the slurry on indium oxide conductive flexible substrate with a brush, leading out copper wire as electrode, and testing with two-dimensional galena Ag4.53Te3Nanogenerators as core materials, e.g.As shown in FIG. 5, the piezoelectric direction is perpendicular to the c-axis direction as seen from the c-axis direction, and the peak value in the figure is the open circuit voltage, about 3.5V, which shows the synthesized two-dimensional galena Ag4.53Te3The nano generator as a core material can generate piezoelectric charges in a flexible device, so that the output open circuit voltage of the flexible nano generator can reach 3.5V.
Example 3:
s1: 0.1g of sodium tellurite and 0.5g of polyvinylpyrrolidone with the molecular weight of 58000 are dissolved in 28mL of deionized water with the conductivity of 18.2M omega cm, the mixture is stirred for 30 minutes under a magnetic stirrer to form a solution A with the concentration of 0.016mol/L, then 1.65mL of hydrazine hydrate and 3.3mL of ammonia water are mixed to form a solution B, the solution B is added into the solution A, the solution B is placed into a hydrothermal reaction kettle, the hydrothermal reaction kettle is sealed, the mixture is reacted in a 165-degree oven for 32 hours, and the reaction product C is taken out to obtain the product C.
S2: and centrifuging the product C by using a centrifuge at the rotating speed of 4000rpm for 10 minutes to remove the upper-layer solution, and then adding acetone and deionized water with the conductivity of 18.2M omega cm into the centrifuge tube to repeatedly wash for three times to obtain a solution D containing silver gray two-dimensional tellurium nanosheet crystals.
S3: dissolving silver nitrate in deionized water with the conductivity of 18.2M omega-cm to obtain a silver nitrate solution with the concentration of 7.5mg/mL, dropwise adding 3mL of the silver nitrate solution into 29mL of the solution D, stirring and reacting at room temperature, continuously dropwise adding the silver nitrate solution when the silver gray solution becomes yellow-green, and generating the two-dimensional galena Ag after the reaction is finished when the yellow-green solution becomes grey-green4.53Te3。
Using the two-dimensional galena Ag obtained in example 34.53Te3And (3) carrying out structural characterization:
the results of the measurement by optical microscope are shown in FIG. 6, Ag4.53Te3Is a two-dimensional plate-shaped crystal structure with the width of 15-25 microns, the length of 92-105 microns and the thickness of 40-50 nanometers and a byproduct nanowire.
Example 4:
s1: 0.1g of sodium tellurite and 0.5g of polyvinylpyrrolidone with the molecular weight of 58000 are dissolved in 25mL of deionized water with the conductivity of 18.2M omega cm, the mixture is stirred for 30 minutes under a magnetic stirrer to form a solution A with the concentration of 0.018mol/L, then 1.65mL of hydrazine hydrate and 3.3mL of ammonia water are mixed to form a solution B, the solution B is added into the solution A, the solution B is placed into a hydrothermal reaction kettle, the hydrothermal reaction kettle is sealed, the reaction kettle is placed into a 200-DEG oven to react for 30 hours, and the solution B is taken out to obtain a product C.
S2: and centrifuging the product C by using a centrifuge at the rotating speed of 3000rpm for 10 minutes to remove the upper-layer solution, and then adding acetone and deionized water with the conductivity of 18.2M omega cm into the centrifuge tube to repeatedly wash for three times to obtain a solution D containing silver gray two-dimensional tellurium nanosheet crystals.
S3: dissolving silver nitrate in deionized water with the conductivity of 18.2M omega-cm to obtain a silver nitrate solution with the concentration of 10mg/mL, dropwise adding 5mL of the silver nitrate solution into 10mL of the solution D, stirring and reacting at room temperature, continuously dropwise adding the silver nitrate solution when the silver gray solution becomes yellow-green, and generating the two-dimensional galena Ag after the reaction is finished when the yellow-green solution becomes grey-green4.53Te3。
Example 5:
s1: 0.1g of sodium tellurite and 0.5g of polyvinylpyrrolidone with the molecular weight of 58000 are dissolved in 25mL of deionized water with the conductivity of 18.2M omega cm, stirred for 30 minutes under a magnetic stirrer to form a solution A with the concentration of 0.018mol/L, then 1.65mL of hydrazine hydrate and 3.3mL of ammonia water are mixed to form a solution B, the solution B is added into the solution A, the solution B is placed into a hydrothermal reaction kettle, the hydrothermal reaction kettle is sealed, the solution B is reacted in a 180-degree oven for 30 hours, and the reaction product C is taken out to obtain the product C.
S2: and centrifuging the product C by using a centrifuge at the rotating speed of 5000rpm for 10 minutes to remove the upper-layer solution, and then adding acetone and deionized water with the conductivity of 18.2M omega cm into the centrifuge tube to repeatedly wash for three times to obtain a solution D containing silver gray two-dimensional tellurium nanosheet crystals.
S3: dissolving silver nitrate in deionized water with the conductivity of 18.2M omega-cm to obtain a silver nitrate solution with the concentration of 8mg/mL, dropwise adding 5mL of the silver nitrate solution into 48mL of the solution D, stirring and reacting at room temperature, continuously dropwise adding the silver nitrate solution when the silver gray solution becomes yellow-green, and generating the two-dimensional galena Ag after the reaction is finished when the yellow-green solution becomes grey-green4.53Te3。
Comparative example 1:
s1: 0.1g of sodium tellurite and 0.5g of polyvinylpyrrolidone with the molecular weight of 58000 are dissolved in 33mL of deionized water with the conductivity of 18.2M omega cm, the mixture is stirred for 30 minutes under a magnetic stirrer to form a solution A with the concentration of 0.014mol/L, then 1.65mL of hydrazine hydrate and 3.3mL of ammonia water are mixed to form a solution B, the solution B is added into the solution A, the solution B is placed into a hydrothermal reaction kettle, the hydrothermal reaction kettle is sealed, the reaction kettle is placed into a 180-degree oven for reaction for 3 hours, and the solution B is taken out to obtain a product C.
S2: and centrifuging the product C by using a centrifuge at the rotating speed of 5000rpm for 10 minutes to remove the upper solution, and then adding acetone and deionized water with the conductivity of 18.2M omega cm into the centrifuge tube to repeatedly wash for three times to obtain a solution D containing the blue-black one-dimensional tellurium nanowire crystals.
S3: dissolving silver nitrate in deionized water with the conductivity of 18.2M omega-cm to obtain a silver nitrate solution with the concentration of 2.5mg/mL, dropwise adding 3mL of the silver nitrate solution into 37mL of the solution D, stirring and reacting at room temperature, continuously dropwise adding the silver nitrate solution when the silver gray solution becomes yellow-green, and generating one-dimensional hessian Ag after the reaction is finished when the yellow-green solution becomes dark green and is black2Te。
Use of Ag from comparative example 12And Te is subjected to structural characterization:
the results of the test obtained by X-ray diffraction are shown in FIG. 7, where the red diffraction peak is the experimental result and the black diffraction peak is based on Ag2The Te crystal structure simulates the structure, and the experimental result is completely consistent with the simulated peak position.
Therefore, the two-dimensional galena Ag prepared by the invention4.53Te3The shape and high crystallinity of the two-dimensional tellurium sheet template are maintained, the structure is more complex and has an asymmetric central structure, the crystal structure belongs to a P-62m space group and is used as a potential application of a nano piezoelectric generator, and the material can be widely applied to flexible wearable equipment such as a flat panel display, a solar cell and the like due to high stability and simplicity and low price of the method.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for synthesizing new phase two-dimensional galena silver telluride based on a two-dimensional tellurium template method is characterized in that the stoichiometric ratio of silver to tellurium is 4.53: 3.
2. A preparation method for synthesizing new phase two-dimensional galena silver telluride based on a two-dimensional tellurium template method is characterized by comprising the following steps:
s1: stirring and dissolving sodium tellurite and polyvinylpyrrolidone in a molar ratio of 52.4:1 in deionized water to obtain a solution A, mixing hydrazine hydrate and an alkaline solution in a volume ratio of 1:2 to form a solution B, adding the solution B and the solution A in a volume ratio of 0.15-0.2 into the solution A, placing the solution B and the solution A into a hydrothermal reaction kettle, sealing the hydrothermal reaction kettle, and placing the solution B into an oven for reaction to obtain a product C;
s2: centrifuging and washing the product C to obtain a solution D containing silver gray two-dimensional tellurium nanocrystals;
s3: dissolving silver nitrate in deionized water to obtain a silver nitrate solution with the concentration of 1-10mg/mL, dropwise adding the silver nitrate solution into the solution D, wherein the volume ratio of the solution D to the silver nitrate solution is 10:1-10:5, stirring at room temperature for reaction, continuously dropwise adding the silver nitrate solution when the silver gray solution becomes yellow green, and generating the two-dimensional galena Ag after the reaction is finished when the yellow green solution becomes grey green4.53Te3。
3. The method for preparing a new phase of two-dimensional galena silver telluride based on the two-dimensional tellurium template method according to claim 1, wherein the deionized water in the steps S1, S2 and S3 has a conductivity of 18.2M Ω.
4. The method for preparing a new phase of two-dimensional galena silver telluride based on the two-dimensional tellurium template method according to claim 1, wherein the concentration of the solution A in the step S1 is 0.014mol/L-0.018 mol/L.
5. The preparation method for synthesizing new phase two-dimensional galena silver telluride based on the two-dimensional tellurium template method according to claim 1, wherein the alkaline solution in the step S1 is ammonia water.
6. The method for preparing a new phase of two-dimensional galena silver telluride based on the two-dimensional tellurium template method according to claim 1, wherein the molecular weight of the polyvinylpyrrolidone in the step S1 is 58000.
7. The preparation method for synthesizing new phase two-dimensional galena silver telluride based on the two-dimensional tellurium template method as claimed in claim 1, wherein the temperature of the oven in the step S1 is 160-200 ℃, and the reaction time is 30-36 h.
8. The method for preparing a new phase of two-dimensional galena silver telluride based on the two-dimensional tellurium template method according to claim 1, wherein in the step S2, the centrifugal washing process is as follows: centrifuging the product C by a centrifuge at the rotating speed of 3000-.
9. The preparation method for synthesizing new phase two-dimensional galena silver telluride based on the two-dimensional tellurium template method as claimed in claim 1, wherein the concentration of the silver nitrate solution in the step S3 is 2.5 mg/mL.
10. The application of the new phase two-dimensional galena silver telluride synthesized based on the two-dimensional tellurium template method as claimed in claim 1 in a nanometer generator.
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| WALTER KA¨LIN ET AL.: "Preparation of Ag5-xTe3 Thin Films and Confirmation of Their Crystal Structure by High Resolution Electron Microscopy", 《JOURNAL OF SOLID STATE CHEMISTRY》 * |
| 夏传俊等: "碲化银纳米晶的室温合成及表征", 《化学通报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114164484A (en) * | 2021-12-08 | 2022-03-11 | 之江实验室 | Preparation method of double-chiral two-dimensional tellurium twin crystals |
| CN114164484B (en) * | 2021-12-08 | 2022-04-29 | 之江实验室 | Preparation method of double-chiral two-dimensional tellurium twin crystals |
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