CN110817810B - Flexible nano material growing with bismuth, trinickel and diselenide and preparation method thereof - Google Patents

Flexible nano material growing with bismuth, trinickel and diselenide and preparation method thereof Download PDF

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CN110817810B
CN110817810B CN201911250171.9A CN201911250171A CN110817810B CN 110817810 B CN110817810 B CN 110817810B CN 201911250171 A CN201911250171 A CN 201911250171A CN 110817810 B CN110817810 B CN 110817810B
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diselenide
bismuth
trinickel
preparation
flexible
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CN110817810A (en
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简基康
杜炳生
王盛儒
雷仁博
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Guangdong University of Technology
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    • C01B19/00Selenium; Tellurium; Compounds thereof
    • C01B19/007Tellurides or selenides of metals
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    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract

The invention belongs to the technical field of semiconductor materials, and particularly relates to a flexible nano material growing with bismuth, trinickel and diselenide and a preparation method thereof. The flexible nano material with the grown bismuth trinickel diselenide is prepared by placing bismuth nitrate and selenium dioxide in a mixed solution according to a molar weight ratio of 1 (1.3-1.7) and carrying out solvothermal reaction with a metal nickel flexible material, and has the advantages of conductivity, nano-property and flexibility, wide application prospect, simple preparation method operation and suitability for large-scale industrial production.

Description

Flexible nano material growing with bismuth, trinickel and diselenide and preparation method thereof
Technical Field
The invention belongs to the technical field of semiconductor materials. More particularly, relates to a flexible nano material with bismuth, trinickel and diselenide growing and a preparation method thereof.
Background
Bismuth is a metal element, has relatively rich reserves, is widely applied to the field of inorganic semiconductors, has excellent performance in the fields of energy, catalysis and luminescence, is also a key element in novel thermoelectric materials and topological insulator materials, and is widely applied. Bismuth trinickel diselenide (Bi) 2 Ni 3 Se 2 ) The bismuth-based semiconductor material also has a monoclinic crystal structure, has a space group of C2/m (No.12), and has a narrow band gap, so that the bismuth-based semiconductor material has a good application prospect in the field of photoelectricity.
At present, most of the bismuth, the nickel and the diselenide are prepared by a solid-phase sintering method, but the sintering temperature needs to be about 1000-1500 ℃, the volatilization speed of bismuth in the sintering process is fast, a large amount of energy and raw materials need to be consumed, and the bismuth, the nickel and the diselenide are not suitable for large-scale industrial production. In addition to solid-phase sintering, Richard Weihrich et al disclose a method of sintering Bi 2 X 3 (X ═ Se, S) is converted in a glycol liquid phase system to Bi, NiBi, NiBiSe and Ni 3 Bi 2 X 2 Method of preparing a compound, but obtaining Ni 3 Bi 2 X 2 The material of (A) is a solid powder, a large amount of second phase exists, and Ni is obtained 3 Bi 2 X 2 The grain size is relatively large (Rommel S M, Krach A, Peter P, et al. conversion Reactions of solutions: From a Surprising Three-Step Mechanism facing direct ProductFormation[J].Chemistry-A European Journal,2016,22(18):6333-6339.)。
With the research and development of portable electronic devices and devices, the requirements on the conductivity, the portability and the flexibility of the required semiconductor materials are higher and higher, and the dibismuth trinickel diselenide prepared at present cannot meet the requirements of the portable electronic devices or devices. Therefore, it is urgently needed to provide a flexible nano material with bismuth, trinickel and diselenide grown and a preparation method thereof.
Disclosure of Invention
The invention aims to solve the technical problems of the prior art that the solid-phase sintering method has more energy and raw material loss, the crystal grain size obtained by liquid-phase conversion is large, and the requirements of portable electronic equipment or devices cannot be met, and provides a preparation method of a flexible nano material growing with bismuth, tri-nickel and diselenide.
The invention also aims to provide the flexible nano material which is prepared by the preparation method and grows with the dibismuth, trinickel and diselenide.
The invention also aims to provide application of the flexible nano material with the growth of the dibismuth trinickel diselenide in the field of semiconductor materials.
The above purpose of the invention is realized by the following technical scheme:
a preparation method of a flexible nano material growing with bismuth, trinickel and diselenide comprises the following steps:
preparing a mixed solution of oleic acid containing polyvinylpyrrolidone and N, N-dimethylacetamide, adding bismuth nitrate and selenium dioxide, uniformly stirring, adding a metal nickel flexible material, carrying out a solvothermal reaction at a temperature of 150-200 ℃, cooling, taking out the metal nickel flexible material, washing and drying to obtain the composite material;
the oleic acid and N, N-dimethylacetamide mixed solution is prepared by mixing oleic acid and N, N-dimethylacetamide according to a volume ratio of 1 (1-3); the molar weight ratio of the bismuth nitrate to the selenium dioxide is 1 (1.3-1.7).
According to the invention, bismuth nitrate and selenium dioxide are placed into a mixed solution of oleic acid and N, N-dimethylacetamide according to a molar weight ratio of 1 (1.3-1.7), a conductive metal nickel flexible material is added for solvothermal reaction, nickel elements in the metal nickel flexible material are utilized to react to generate nano-flaky bismuth trinickel diselenide which is uniformly distributed on the surface of the metal nickel flexible material, and the obtained material has conductivity, nano-property and flexibility and can completely meet the requirements of portable electronic equipment or devices on semiconductor materials.
Preferably, the molar weight ratio of the bismuth nitrate to the selenium dioxide is 1 (1.3-1.5).
More preferably, the molar weight ratio of bismuth nitrate to selenium dioxide is 1: 1.5.
Preferably, the reaction temperature is 180-200 ℃.
More preferably, the reaction temperature is 200 ℃.
The reaction temperature of the invention is 150-200 ℃, compared with a solid-phase sintering method, the temperature required by the reaction is obviously reduced, and the energy consumption is greatly reduced.
Preferably, the volume ratio of the oleic acid to the N, N-dimethylacetamide is 1 (1-2).
More preferably, the volume ratio of oleic acid to N, N-dimethylacetamide is 1: 2.
Further, the reaction time is 5-15 h.
Preferably, the reaction time is 10-15 h.
More preferably, the reaction time is 15 h.
Furthermore, the weight-to-volume ratio of the polyvinylpyrrolidone to the mixed solution of oleic acid and N, N-dimethylacetamide is 1 (10-13) g/mL.
Preferably, the weight-to-volume ratio of the polyvinylpyrrolidone to the mixed solution of oleic acid and N, N-dimethylacetamide is 1 (12-13) g/mL.
More preferably, the weight-to-volume ratio of the polyvinylpyrrolidone to the mixed solution of oleic acid and N, N-dimethylacetamide is 1:12 g/mL.
Further, the metal nickel flexible material is nickel foil or foam nickel. When the metal nickel flexible material is foam nickel, nano spheres formed by self-assembling bisbismuth trinickel diselenide nano sheets can be grown on the foam nickel; when the metal nickel flexible material is nickel foil, a compact and upright bismuthyl trinickel diselenide nanosheet can be grown on the nickel foil.
Preferably, the metallic nickel flexible material is a nickel foil.
Furthermore, the container for the solvothermal reaction is a reaction kettle.
Preferably, the reaction vessel has a polytetrafluoroethylene liner.
In addition, the invention also provides the flexible nano material which is prepared by the preparation method and grows with the dibismuth, the trinickel and the diselenide.
In addition, the invention also provides application of the flexible nano material with the growth of the dibismuth trinickel diselenide in the field of semiconductor materials.
The invention has the following beneficial effects:
(1) the invention provides a novel preparation method of a flexible nano material with growing bismuth trinickel diselenide, bismuth nitrate and selenium dioxide are placed in a mixed solution according to the molar weight ratio of 1 (1.3-1.7) to carry out solvothermal reaction with an added metal nickel flexible material, so that uniformly distributed nano flaky bismuth trinickel diselenide can be generated.
(2) The flexible nano material growing with the dibismuth trinickel diselenide prepared by the method has conductivity, nano property and flexibility, can completely meet the requirements of portable electronic equipment or devices on semiconductor materials, and has wide application prospect.
Drawings
FIG. 1 is a diffraction phase characterization diagram of a flexible nanomaterial grown with bismuth trinickel diselenide in example 1 of the present invention.
FIG. 2 is a graph showing the morphology of the flexible nanomaterial of example 1 of the present invention grown with bismuth, trinickel, diselenide.
FIG. 3 is a diffraction phase characterization diagram of the flexible nanomaterial of example 3 grown with dibismuth, trinickel, diselenide according to the present invention.
FIG. 4 is a graph showing the morphology of the flexible nanomaterial of example 3 of the present invention in which bismuth, trinickel, diselenide has grown.
FIG. 5 is a graph showing the morphology of the flexible nanomaterial of comparative example 1 of the present invention grown with bismuth, trinickel, diselenide.
Detailed Description
The invention is further described with reference to the drawings and the following detailed description, which are not intended to limit the invention in any way. The reagents, methods and apparatus employed in the present invention are conventional in the art, except as otherwise indicated.
Unless otherwise indicated, reagents and materials used in the following examples are commercially available.
Example 1A Flexible nanomaterial grown with bismuth, trinickel, diselenide
The flexible nano material growing with the bismuth, the nickel and the diselenide is prepared by the following steps:
dissolving 3g of polyvinylpyrrolidone in a mixed solution of 12mL of oleic acid and 24mL of N, N-dimethylacetamide, adding 0.4849g of bismuth nitrate pentahydrate and 0.1663g of selenium dioxide, uniformly stirring, placing the mixture in a 50mL of polytetrafluoroethylene reaction kettle, adding 1cm × 2cm of foamed nickel, screwing the reaction kettle, placing the reaction kettle into an oven, reacting for 15 hours at the temperature of 200 ℃, cooling to room temperature, taking out the foamed nickel, washing with water and absolute ethyl alcohol in sequence, and drying in vacuum to obtain the polyvinylpyrrolidone.
Example 2A Flexible nanomaterial grown with bismuth, trinickel and diselenide
The flexible nano material growing with the bismuth, the nickel and the diselenide is prepared by the following steps:
dissolving 3g of polyvinylpyrrolidone in a mixed solution of 18mL of oleic acid and 18mL of N, N-dimethylacetamide, adding 0.4847g of bismuth nitrate pentahydrate and 0.1442g of selenium dioxide, uniformly stirring, placing the mixture in a 50mL of polytetrafluoroethylene reaction kettle, adding 1cm multiplied by 2cm of foamed nickel, screwing the reaction kettle, placing the reaction kettle into an oven, reacting at the temperature of 150 ℃ for 10 hours, cooling to room temperature, taking out the foamed nickel, washing with water and absolute ethyl alcohol in sequence, and drying in vacuum to obtain the polyvinylpyrrolidone.
Diffraction phase characterization and morphology characterization of the materials prepared in examples 1-2 were determined, wherein the diffraction phase characterization and morphology characterization results of example 1 are shown in fig. 1-2, and the results of example 2 are similar to those of example 1.
As can be seen from FIG. 1, the material prepared in example 1 of the present invention and Bibismuth trinickel diselenide (Bi) 2 Ni 3 Se 2 ) The peak positions of the standard diffraction cards can be in one-to-one correspondence, which shows that the bismuth trinickel diselenide prepared successfully in the embodiment 1 of the invention has Ni diffraction peaks from the substrate nickel foam, and in addition, a small part of impurity NiSe exists in the sample.
As can be seen from fig. 2, the dibismuth trinickel diselenide is nanospheres with a size of about 1 μm formed by self-assembling nanosheets with a thickness of about 5-10 nm, and the nanospheres uniformly and tightly grow on the foam nickel skeleton in a large area, which indicates that the flexible nanomaterial growing with dibismuth trinickel diselenide is successfully prepared in embodiment 1 of the present invention.
Example 3A Flexible nanomaterial grown with bismuth, Trinickel, and diselenide
The flexible nano material growing with the bismuth, the nickel and the diselenide is prepared by the following steps:
dissolving 3g of polyvinylpyrrolidone in a mixed solution of 12mL of oleic acid and 24mL of N, N-dimethylacetamide, adding 0.4848g of bismuth nitrate pentahydrate and 0.1662g of selenium dioxide, uniformly stirring, placing the mixture in a 50mL of polytetrafluoroethylene reaction kettle, adding a nickel foil with the thickness of 1cm multiplied by 2cm, screwing the reaction kettle, placing the reaction kettle in an oven, reacting at the temperature of 200 ℃ for 15 hours, cooling to room temperature, taking out the nickel foil, washing with water and absolute ethyl alcohol in sequence, and drying in vacuum to obtain the polyvinylpyrrolidone.
Example 4A Flexible nanomaterial grown with bismuth, trinickel, diselenide
The flexible nano material growing with the dibismuth, the trinickel and the diselenide is prepared by the following steps:
dissolving 3g of polyvinylpyrrolidone in a mixed solution of 9mL of oleic acid and 27mL of N, N-dimethylacetamide, adding 0.4850g of pentahydrate bismuth nitrate and 0.1887g of selenium dioxide, uniformly stirring, placing the mixture in a 50mL of polytetrafluoroethylene reaction kettle, adding a nickel foil with the thickness of 1cm multiplied by 2cm, screwing the reaction kettle, placing the reaction kettle in an oven, reacting at the temperature of 150 ℃ for 10 hours, cooling to the room temperature, taking out the nickel foil, washing with water and absolute ethyl alcohol in sequence, and drying in vacuum to obtain the copper-based catalyst.
Diffraction phase characterization and morphology characterization of the materials prepared in examples 3-4 were determined, wherein the diffraction phase characterization and morphology characterization results of example 3 are shown in fig. 3-4, and the results of example 4 are similar to those of example 1.
As can be seen from FIG. 3, the material prepared in example 3 of the present invention and Bibismuth trinickel diselenide (Bi) 2 Ni 3 Se 2 ) The peak positions of the standard diffraction cards can be in one-to-one correspondence, which shows that the bismuth trinickel diselenide is successfully prepared in the embodiment 3 of the invention, wherein the existing Ni diffraction peak comes from the substrate nickel foil, does not contain NiSe impurity, and is pure phase bismuth trinickel diselenide.
As can be seen from fig. 4, the dibismuth trinickel diselenide is in the shape of a nanosheet with a thickness of 10-20 nm, and the nanosheets uniformly and tightly vertically grow on the nickel foil, which indicates that the flexible nanomaterial on which the dibismuth trinickel diselenide grows is successfully prepared and obtained in embodiment 3 of the present invention.
Comparative example 1A Bibismuth trinickel diselenide Material
The bismuth trinickel diselenide material is prepared by the following steps:
dissolving 3g of polyvinylpyrrolidone in a mixed solution of 12mL of oleic acid and 24mL of N, N-dimethylacetamide, adding 0.7272g of bismuth nitrate pentahydrate and 0.1664g of selenium dioxide, uniformly stirring, placing the mixture in a 50mL of polytetrafluoroethylene reaction kettle, adding 1cm multiplied by 2cm of foamed nickel, screwing the reaction kettle, placing the reaction kettle in an oven, reacting at the temperature of 200 ℃ for 15 hours, cooling to room temperature, taking out the foamed nickel, washing with water and absolute ethyl alcohol in sequence, and drying in vacuum to obtain the polyvinylpyrrolidone.
The morphology characterization of the bismuthyl trinickel diselenide material prepared in comparative example 1 was determined, and the results are shown in fig. 5.
As can be seen from FIG. 5, when the molar weight ratio of bismuth nitrate to selenium dioxide does not satisfy 1 (1.3-1.7), the grown bismuthyltrinickel diselenide is not well combined with the foamed nickel, but is dispersed in the pores of the foamed nickel, and the particles of the synthesized sample are large, and most of the particles are in the micrometer scale.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (9)

1. A preparation method of a flexible nano material growing with bismuth, trinickel and diselenide is characterized by comprising the following steps:
preparing a mixed solution of oleic acid containing polyvinylpyrrolidone and N, N-dimethylacetamide, adding bismuth nitrate and selenium dioxide, uniformly stirring, adding a metal nickel flexible material, carrying out a solvothermal reaction at a temperature of 150-200 ℃, cooling, taking out the metal nickel flexible material, washing and drying to obtain the composite material;
the oleic acid and N, N-dimethylacetamide mixed solution is prepared by mixing oleic acid and N, N-dimethylacetamide according to a volume ratio of 1 (1-3); the molar weight ratio of the bismuth nitrate to the selenium dioxide is 1 (1.3-1.7).
2. The preparation method of claim 1, wherein the molar weight ratio of the bismuth nitrate to the selenium dioxide is 1 (1.3-1.5).
3. The preparation method of claim 2, wherein the molar weight ratio of the bismuth nitrate to the selenium dioxide is 1: 1.5.
4. The method according to any one of claims 1 to 3, wherein the reaction temperature is 180 to 200 ℃.
5. The method according to any one of claims 1 to 3, wherein the reaction time is 5 to 15 hours.
6. The preparation method according to any one of claims 1 to 3, wherein the weight/volume ratio of the polyvinylpyrrolidone to the mixed solution of oleic acid and N, N-dimethylacetamide is 1 (10 to 13) g/mL.
7. The preparation method according to any one of claims 1 to 3, wherein the metallic nickel flexible material is nickel foil or nickel foam.
8. The flexible nano material growing with the dibismuth trinickel diselenide prepared by the preparation method of any one of claims 1 to 7.
9. The use of the flexible nanomaterial grown with bismuthyltrinickel diselenide according to claim 8 in the field of semiconductor materials.
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