CN113912025A - Preparation method, product and application of Te nano material with controllable morphology - Google Patents

Preparation method, product and application of Te nano material with controllable morphology Download PDF

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CN113912025A
CN113912025A CN202111513451.1A CN202111513451A CN113912025A CN 113912025 A CN113912025 A CN 113912025A CN 202111513451 A CN202111513451 A CN 202111513451A CN 113912025 A CN113912025 A CN 113912025A
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nano material
controllable morphology
polyvinylpyrrolidone
prepared
molecular weight
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宋孝辉
胡艳杰
吕晓静
刘振
马梓楠
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Henan Normal University
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Henan Normal University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00—Selenium; Tellurium; Compounds thereof
    • C01B19/02—Elemental selenium or tellurium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like

Abstract

The invention discloses a preparation method, a product and application of a Te nano material with controllable morphology, and relates to the technical field of preparation of Te materials. The method comprises the following steps: adding polyvinylpyrrolidone, an alkaline solution and hydrazine monohydrate into a sodium tellurite aqueous solution to carry out hydrothermal reaction to obtain the Te nano material with controllable morphology; when the average molecular weight of the polyvinylpyrrolidone is 8000, the prepared Te nano material is two-dimensional flaky; when the average molecular weight of the polyvinylpyrrolidone is 360000 or 1300000, the prepared Te nano material is in a one-dimensional linear shape. According to the invention, the growth speed of each crystal face of the Te material can be different by changing the average molecular weight of PVP, so that the Te nano material with a two-dimensional sheet shape with a small vertical and horizontal ratio or a one-dimensional linear shape with a large vertical and horizontal ratio is respectively prepared.

Description

Preparation method, product and application of Te nano material with controllable morphology
Technical Field
The invention relates to the technical field of nano material preparation, in particular to a preparation method, a product and application of a Te material with controllable morphology.
Background
Tellurium (Te) is an important elemental semiconductor material, which is composed of Te atomsIndividual helical strands are formed by van der waals forces stacking together. Te is generally a P-type semiconductor material with direct band gap, the forbidden band width of bulk material at room temperature is 0.32eV, and the hole mobility is about 590 cm2/V•S-1. In the last decade, the exploration of various Te nano-structures is greatly advanced, and a series of Te nano-materials with different morphologies, such as nano-rods, nano-wires, nano-tubes, nano-sheets, feather-shaped Te and the like, are successfully prepared and studied in detail. The shape and size of Te can be regulated and controlled, and the Te has an inseparable relation with the application field thereof. One-dimensional Te has excellent characteristics of low thermal conductivity, strong piezoelectric effect, nonlinear optical response and the like, and has wide application in the fields of thermoelectricity, piezoelectricity, nonlinear optics and the like. In recent years, as a new member of two-dimensional materials, research finds that two-dimensional Te has a plurality of attractive excellent properties, theoretical calculation and experiments show that the Te has good physical and chemical properties, such as high carrier mobility at room temperature, excellent on-state current density, adjustable band gap and good air stability at room temperature, and has potential application value in the fields of field effect transistors, photodetectors, lithium ion batteries and the like. Particularly, the Te has great application potential in the aspect of lithium ion batteries, and the electric conductivity of the Te serving as a narrow band gap p-type semiconductor material can reach 2 multiplied by 102 S·m-1Much higher than S and Se of the same main group. (Liu Y., Wang J.W., Wang C.S., et al, Lithium-tellurium batteries based on tellurium/porous carbon composite [ J]J. Mater. chem. A, 2014(2) 12201-12207) although the theoretical mass capacity of Te is only 429 mAh.g-1However, the theoretical volume capacity is 2621 mAh.cm-3(based on a density of 6.24g.cm-3）,（Seo J., Seong G.K., Park C.M. Te/C nanocomposites for Li-Te secondary batteries[J]Science Reports, 2015(5): 7969.) furthermore, the energy density of Te is 823.2 wh.kg-1Much higher than the lithium ion battery commercialized at present, and thus is considered to be one of the best candidate cathode materials for the next generation lithium battery.
The lattice structure of tellurium (Te) is highly anisotropic and can be modeled as a multi-dimensional nanoscale under a nanostructure. The research finds that the shape and structure of Te determine the performance of Te, thereby influencing the application of Te. Therefore, the research on Te with different shapes and structures becomes a hot point of research. The current common synthesis methods of Te comprise molecular beam epitaxy, physical vapor deposition, liquid phase stripping, hydrothermal reaction and the like. Among the preparation methods, the hydrothermal method is synthesized in a closed space, so that the external interference is reduced to the maximum extent, and the purity of the generated product is greatly improved. In addition, the hydrothermal method has the advantages of simple process, low cost and wide application. However, some Te synthesized by the hydrothermal reaction reported at present is one-dimensional rod-shaped, some Te synthesized by the hydrothermal reaction is two-dimensional sheet-shaped, and the controllability is poor.
Disclosure of Invention
The invention aims to provide a preparation method, a product and application of a Te nano material with controllable morphology, which aim to solve the problems in the prior art. The preparation process is simple, is beneficial to industrial production, and can be applied to the research fields of lithium ion batteries, field effect transistors, photoelectric detectors and the like.
In order to achieve the purpose, the invention provides the following scheme:
one of the technical schemes of the invention is a preparation method of a Te nano material with controllable morphology, which comprises the following steps:
adding polyvinylpyrrolidone, an alkaline solution and hydrazine monohydrate into a sodium tellurite aqueous solution to carry out hydrothermal reaction to obtain the Te nano material with controllable morphology;
the morphology of the Te nano material is regulated and controlled by regulating and controlling the average molecular weight of the polyvinylpyrrolidone.
Further, the polyvinylpyrrolidone has an average molecular weight of one of 8000, 360000, or 1300000.
When the average molecular weight of the polyvinylpyrrolidone is 8000, the Te nano material is mostly in a two-dimensional sheet shape with small aspect ratio; when the molecular weight of polyvinylpyrrolidone is 360000 and 1300000, the appearance of Te nano-material is mostly one-dimensional linear with large aspect ratio.
Further, the method also comprises the steps of cooling, centrifuging, separating and washing in sequence after the hydrothermal reaction is finished.
Further, the centrifugation is specifically centrifugation for 10min at the rotating speed of 5000r/min, and the centrifugation is carried out twice.
Further, the alkaline solution is one of ammonia water, a potassium hydroxide aqueous solution and a sodium hydroxide aqueous solution.
The alkaline solution is added to adjust the pH of the mixed solution to 10-12, preferably pH = 11.
Further, the mass ratio of the sodium tellurite to the polyvinylpyrrolidone is 1-300: 1, preferably 8.06: 1.
further, the hydrothermal reaction is specifically 100-200 ℃ for 4-36h, preferably 160-180 ℃ for 14-20 h.
According to the second technical scheme, the Te nano material with controllable morphology is prepared by the preparation method.
In the third technical scheme of the invention, the Te nano material with controllable morphology is applied to lithium ion batteries, field effect transistors and photoelectric detectors.
The invention discloses the following technical effects:
the invention provides a preparation method of a Te nano material with controllable morphology, which utilizes sodium tellurite as a precursor, polyvinylpyrrolidone as a stabilizer, hydrazine monohydrate as a reducing agent and deionized water as a solvent to synthesize the low-dimensional Te nano material by a hydrothermal method. By changing the average molecular weight of PVP, the growth speed of each crystal face of the Te material can be different, so that the Te nano material with a two-dimensional sheet shape with a small vertical-to-horizontal ratio or a one-dimensional linear shape with a large vertical-to-horizontal ratio can be respectively prepared. The provided controllability can be used for preparing Te nanometer materials with different dimensions, and the Te nanometer materials can be widely applied to experiments and industries. First, because Te has excellent electrical properties, it is a hot material selected for field effect transistors in two-dimensional material experiments, and many recent documents report that field effect transistors and photodetectors based on van der waals heterojunctions, in which one-dimensional Te and two-dimensional Te are made into different dimensions from other materials, have excellent properties. The preparation method provided by the invention provides great convenience for the mixed-dimensional heterojunction based on the Te nano material in the later period; secondly, according to literature reports, the surface morphology and size difference of materials in the lithium ion battery can influence the battery performance, and the method provided by the inventor provides a material basis for the subsequent research of improving the performance of the lithium ion battery based on the Te material.
The preparation method has the advantages of simple process, easily obtained raw materials and low production cost, and is very favorable for realizing industrial production.
The Te nano material with controllable morphology prepared by the invention has high purity, good dispersibility and excellent electrical property, and can be used as a functional material to be applied to the fields of lithium ion batteries, field effect transistors, photoelectric detectors, thermoelectric devices and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in 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 it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is an optical microscope photograph of the Te material with controllable morphology prepared in examples 1-3; wherein (a) is example 1, (b) is example 2, and (c) is example 3;
FIG. 2 is an SEM spectrum of the Te material with controllable morphology prepared in example 2;
FIG. 3 is an atomic force microscope spectrum of the Te material with controllable morphology prepared in example 2;
FIG. 4 is a Raman spectrum of the Te material with controllable morphology prepared in examples 1-3; wherein the numerical values in the table represent the average molecular weight of polyvinylpyrrolidone;
FIG. 5 is an XRD spectrum of the Te material with controllable morphology prepared in example 2;
FIG. 6 is a graph showing the electrical property results of the Te material with controllable morphology prepared in example 2; wherein (a) is an I-V characteristic curve and (b) is a transfer characteristic curve.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The description and examples are intended to be illustrative only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The "room temperature" in the examples of the present invention means 20 to 25 ℃ unless otherwise specified.
Example 1
Step 1, weighing 0.0462g Na2TeO3And 1.5g PVP with an average molecular weight of 8000, adding Na2TeO3Adding the mixed solution into 16mL of deionized water, uniformly stirring, then adding PVP, and stirring again to obtain a transparent colloidal mixed solution A;
step 2, adding 1.66mL of ammonia water and 0.840mL of hydrazine monohydrate into the mixed solution A, fully stirring, transferring to the inner liner of a 25mL reaction kettle, sealing, and placing in an air-blast drying oven to heat for 14h at 180 ℃;
and 3, immediately cooling by using flowing water at 15 ℃ after the hydrothermal reaction in the step 2 is finished, adding 10mL of deionized water into the obtained solution, setting the centrifugal rotation speed to be 5000r/min and the centrifugal time to be 10min, centrifuging twice, and separating and washing the precipitate to obtain the Te nano material with controllable morphology. And finally, adding 15ml of deionized water into the precipitate for dispersion (the dispersion purpose is that the precipitate is spun on a substrate for observation to obtain a Te solution, and the precipitate after centrifugation has too high concentration and is difficult to observe) to obtain the Te material solution with controllable morphology.
The Te material solution with controllable morphology prepared in the embodiment is spin-coated on a substrate, and is observed and photographed, an optical microscope image and a raman spectrum of the Te material solution are respectively shown in fig. 1 (a) and fig. 4, and as can be seen from fig. 1 (a), the Te material prepared in the embodiment is a 2D sheet with small vertical and horizontal size, the length is 10-100 μm, the width is 5-20 μm, and the thickness is about 18 nm; as can be seen from the raman spectrum of fig. 4, the raman vibrational peak of Te prepared in this example is consistent with the report of the related literature, indicating that the material quality is better.
Example 2
Step 1, weighing 0.0462g Na2TeO3And 1.5g PVP with an average molecular weight of 360000, mixing Na2TeO3Adding the mixed solution into 16mL of deionized water, uniformly stirring, then adding PVP, and stirring again to obtain a transparent colloidal mixed solution A;
step 2, adding 1.66mL of ammonia water and 0.840mL of hydrazine monohydrate into the mixed solution A, fully stirring, transferring to the inner liner of a 25mL reaction kettle, sealing, and placing in an air-blast drying oven to heat for 14h at 180 ℃;
and 3, immediately cooling by using flowing water at 15 ℃ after the hydrothermal reaction in the step 2 is finished, adding 10mL of deionized water into the obtained solution, setting the centrifugal rotation speed to be 5000r/min and the centrifugal time to be 10min, centrifuging twice, and separating and washing the precipitate to obtain the Te nano material with controllable morphology. Finally, 15ml of deionized water is added into the precipitate for dispersion, wherein the dispersion purpose is that the precipitate is spun on a substrate for observation in order to obtain a Te solution, and the precipitate after centrifugation has too high concentration and is difficult to observe), so that the Te material solution with controllable morphology can be obtained;
the Te material solution with controllable morphology prepared in the embodiment is spin-coated on a substrate, and is observed and photographed, wherein an optical microscope picture, a SEM picture, an atomic force microscope picture, a Raman picture, an XRD picture and an electrical property picture are respectively shown in figures 1 (b), 2, 3, 4, 5 and 6, and as can be seen from figures 1 (b), 2 and 3, the Te material prepared in the embodiment is 1D linear with large vertical and horizontal sizes, the length is 5-50 mu m, the width is 200nm-1 mu m, and the thickness is about 51 nm; as can be seen from fig. 4 and 5, the Te crystal prepared by the present embodiment is better and has higher quality; it can be seen from fig. 6 (a) and (b) that Te is excellent in conductivity and has a field modulation behavior.
Example 3
Step 1, weighing 0.0462g Na2TeO3And 1.5g of PVP with an average molecular weight of 1300000, adding Na2TeO3Adding the mixed solution into 16mL of deionized water, uniformly stirring, then adding PVP, and stirring again to obtain a transparent colloidal mixed solution A;
step 2, adding 1.66mL of ammonia water and 0.840mL of hydrazine monohydrate into the mixed solution A, fully stirring, transferring to the inner liner of a 25mL reaction kettle, sealing, and placing in an air-blast drying oven to heat for 14h at 180 ℃;
and 3, immediately cooling by using flowing water at 15 ℃ after the hydrothermal reaction in the step 2 is finished, adding 10mL of deionized water into the obtained solution, setting the centrifugal rotation speed to be 5000r/min and the centrifugal time to be 10min, centrifuging twice, and separating and washing the precipitate to obtain the Te nano material with controllable morphology. Finally, 15ml of deionized water is added into the precipitate for dispersion, wherein the dispersion purpose is that the precipitate is spun on a substrate for observation in order to obtain a Te solution, and the precipitate after centrifugation has too high concentration and is difficult to observe), so that the Te material solution with controllable morphology can be obtained;
the Te material solution with controllable morphology prepared in the embodiment is spin-coated on a substrate, and is observed and photographed, an optical microscope image and a raman spectrum of the Te material solution are respectively shown in fig. 1 (c) and fig. 4, and as can be seen from fig. 1 (c), the Te material prepared in the embodiment is similar to that of embodiment 2, is 1D linear with large vertical and horizontal aspect ratio, has a length of 5-100 μm and a width of 100nm-1 μm, and has a thickness similar to that of embodiment 2; as can be seen from the raman spectrum of fig. 4, the Te prepared in this example has a good quality.
The effect of the Te material with controllable morphology prepared in the embodiments 1-3 is verified, and the ohmic contact between Te and the electrode can be seen, so that the Te material has good conductivity and field modulation behavior.
From the experimental results of examples 1-3, we can conclude that: the average molecular weight of the polyvinylpyrrolidone can effectively regulate and control the morphology of the tellurium material, and the specific expression is that when the average molecular weight of the polyvinylpyrrolidone is smaller, most of the prepared Te is 2D sheets with smaller vertical and horizontal ratio; when the average molecular weight of polyvinylpyrrolidone is large, most of the prepared Te is 1D linear with a large aspect ratio.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.

Claims (7)

1. A preparation method of a Te nano material with controllable morphology is characterized by comprising the following steps:
adding polyvinylpyrrolidone, an alkaline solution and hydrazine monohydrate into a sodium tellurite aqueous solution to carry out hydrothermal reaction to obtain the Te nano material with controllable morphology;
the polyvinylpyrrolidone has an average molecular weight of one of 8000, 360000 or 1300000;
when the average molecular weight of the polyvinylpyrrolidone is 8000, the prepared Te nano material is two-dimensional flaky; when the average molecular weight of the polyvinylpyrrolidone is 360000 or 1300000, the prepared Te nano material is in a one-dimensional linear shape.
2. The method for preparing a Te nano material with a controllable morphology according to claim 1, wherein the method further comprises the steps of cooling, centrifuging, separating and washing in sequence after the hydrothermal reaction is finished.
3. The method for preparing a Te nanomaterial with controllable morphology according to claim 1, wherein the alkaline solution is one of ammonia water, aqueous potassium hydroxide solution and aqueous sodium hydroxide solution.
4. The method for preparing a Te nano material with controllable morphology according to claim 1, wherein the ratio of the sodium tellurite to the polyvinylpyrrolidone is 1-300: 1.
5. the method as claimed in claim 1, wherein the hydrothermal reaction is carried out at 200 ℃ for 4-36h and at 100 ℃.
6. The Te nano-material with controllable morphology, which is prepared by the preparation method according to any one of claims 1 to 5.
7. The use of the Te nanomaterial with controllable morphology of claim 6 in lithium ion batteries, field effect transistors, photodetectors.
CN202111513451.1A 2021-12-13 2021-12-13 Preparation method, product and application of Te nano material with controllable morphology Pending CN113912025A (en)

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