CN113135595A - Preparation method of one-dimensional heterogeneous nano material of manganese sulfide and zinc sulfide - Google Patents
Preparation method of one-dimensional heterogeneous nano material of manganese sulfide and zinc sulfide Download PDFInfo
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- 229910052984 zinc sulfide Inorganic materials 0.000 title claims abstract description 51
- CADICXFYUNYKGD-UHFFFAOYSA-N sulfanylidenemanganese Chemical compound [Mn]=S CADICXFYUNYKGD-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 239000005083 Zinc sulfide Substances 0.000 title claims abstract description 48
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title abstract description 8
- BOXSVZNGTQTENJ-UHFFFAOYSA-L zinc dibutyldithiocarbamate Chemical compound [Zn+2].CCCCN(C([S-])=S)CCCC.CCCCN(C([S-])=S)CCCC BOXSVZNGTQTENJ-UHFFFAOYSA-L 0.000 claims abstract description 15
- 229910052946 acanthite Inorganic materials 0.000 claims abstract description 12
- 239000011572 manganese Substances 0.000 claims abstract description 11
- QXDQSQFLCULCEC-UHFFFAOYSA-L n,n-dibutylcarbamodithioate;manganese(2+) Chemical compound [Mn+2].CCCCN(C([S-])=S)CCCC.CCCCN(C([S-])=S)CCCC QXDQSQFLCULCEC-UHFFFAOYSA-L 0.000 claims abstract description 11
- XUARKZBEFFVFRG-UHFFFAOYSA-N silver sulfide Chemical group [S-2].[Ag+].[Ag+] XUARKZBEFFVFRG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229940056910 silver sulfide Drugs 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 229920000742 Cotton Polymers 0.000 claims abstract description 9
- 239000011261 inert gas Substances 0.000 claims abstract description 8
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 6
- 239000002105 nanoparticle Substances 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 239000012046 mixed solvent Substances 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims abstract description 5
- SZRLKIKBPASKQH-UHFFFAOYSA-M dibutyldithiocarbamate Chemical compound CCCCN(C([S-])=S)CCCC SZRLKIKBPASKQH-UHFFFAOYSA-M 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 11
- 239000002070 nanowire Substances 0.000 claims description 11
- 239000002243 precursor Substances 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical compound CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 claims description 4
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 abstract description 9
- 239000007772 electrode material Substances 0.000 abstract description 3
- 239000000696 magnetic material Substances 0.000 abstract description 3
- 238000012983 electrochemical energy storage Methods 0.000 abstract 1
- 239000011701 zinc Substances 0.000 description 8
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000011593 sulfur Substances 0.000 description 6
- 229910052717 sulfur Inorganic materials 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- 238000013507 mapping Methods 0.000 description 3
- 229910052950 sphalerite Inorganic materials 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- FSJWWSXPIWGYKC-UHFFFAOYSA-M silver;silver;sulfanide Chemical compound [SH-].[Ag].[Ag+] FSJWWSXPIWGYKC-UHFFFAOYSA-M 0.000 description 1
- 235000002639 sodium chloride Nutrition 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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Abstract
The invention relates to a one-dimensional heterogeneous nano material of manganese sulfide and zinc sulfide, belonging to the technical field of nano material preparation. The one-dimensional heterogeneous nano material of manganese sulfide and zinc sulfide is gray powder after being dried, the shape of powder particles is in a cotton swab rod shape, namely the head of the cotton swab is silver sulfide nano particles, the rod part of the cotton swab is composed of segmented zinc sulfide and manganese sulfide, and the material is applied to photoelectric devices as a luminescent material, or applied to magnetic devices as a magnetic material, or applied to electrochemical energy storage devices as an electrode material. The preparation method comprises the following steps: adding a silver sulfide nanoparticle catalyst and zinc dibutyl dithiocarbamate or manganese dibutyl dithiocarbamate into the mixed solvent, and uniformly stirring; heating and preserving heat under the protection of inert gas or vacuum, adding manganese dibutyldithiocarbamate or zinc dibutyldithiocarbamate, stirring uniformly, heating, preserving heat and cooling under the protection of inert gas or vacuum to obtain the material.
Description
Technical Field
The invention belongs to the technical field of nano material preparation, and particularly relates to a preparation method of a one-dimensional heterogeneous nano material of novel manganese sulfide and zinc sulfide with controllable composition and shape.
Background
In the field of nano materials, a one-dimensional semiconductor heterogeneous nano structure can integrate the advantages of different components and utilize the special physical and chemical properties of a heterogeneous interface to generate a synergistic effect or an enhancement effect superior to a single component. Zinc sulfide and manganese sulfide are important semiconductor materials, wherein the zinc sulfide is an important IIB-VIA group direct band gap semiconductor material, the band gap is about 3.7eV, and the zinc sulfide is widely applied to optoelectronic devices such as light emitting diodes, lasers, ultraviolet light detection devices and the like; manganese sulfide is an important VIIB-VIA family anti-iron weak magnetic semiconductor material, the band gap can reach 3.7eV (T = 0), and the manganese sulfide has a great potential application value in the aspects of preparing weak magnetic semiconductors, short-wave photoelectric devices, solar cells and the like. At present, the one-dimensional heterogeneous nano structure of high-quality manganese sulfide and zinc sulfide is constructed, the advantages of two components of manganese sulfide and zinc sulfide can be fully integrated, and the special physical and chemical properties of a heterogeneous interface of manganese sulfide and zinc sulfide are utilized, so that the method has important significance for constructing novel optical, electrical and magnetic devices.
Manganese sulfide crystals generally exhibit three crystal forms, including α -MnS in the green stable rock-salt structure, β -MnS in the pink metastable sphalerite structure, and γ -MnS in the pink metastable wurtzite structure. Two kinds of metastable manganese sulfide with sphalerite and wurtzite structures exist only at low pressure and low temperature. When the ambient temperature is raised to 200 ℃ or a certain pressure is applied, both will irreversibly convert to rock salt stable α -MnS. Most of reported manganese sulfide and zinc sulfide composite materials are in nanoparticle, core-shell structures or film structures, and the current literature reports about one-dimensional heterogeneous nanostructures of manganese sulfide and zinc sulfide, so that a process route for controllably preparing the one-dimensional heterogeneous nanostructures of manganese sulfide and zinc sulfide is urgently needed to be developed.
Based on the method, silver sulfide is used as a catalyst, manganese dibutyldithiocarbamate and zinc dibutyldithiocarbamate are used as precursors of manganese and zinc, a novel one-dimensional heterogeneous nano structure of manganese sulfide and zinc sulfide with controllable composition and appearance is prepared by a two-step method, and a novel material is provided for constructing novel optical, electrical and magnetic devices.
Disclosure of Invention
The invention solves the problem that the one-dimensional heterogeneous nano structure of manganese sulfide and zinc sulfide is difficult to be controllably prepared in the background technology, and provides a preparation method of the one-dimensional heterogeneous nano material of manganese sulfide and zinc sulfide.
One-dimensional heterogeneous nano material of manganese sulfide and zinc sulfide is dried to be gray powder, and the band gap size is 3.7-3.9 eV; the shape of the powder particles is a cotton swab rod, the head of the cotton swab is silver sulfide nanoparticles, the diameter of the cotton swab is 8-16 nm, the rod is composed of segmented zinc sulfide and manganese sulfide, the diameter of the rod is 7-11 nm, and the length of the rod is 40-200 nm.
The one-dimensional heterogeneous nano material of zinc sulfide and manganese sulfide is applied to photoelectric devices as a luminescent material, or applied to magnetic devices as a magnetic material, or applied to energy storage devices as an electrode material.
The preparation operation steps of the one-dimensional heterogeneous nano material of zinc sulfide and manganese sulfide are as follows:
(1) 15 mL of the mixed solvent and 2 mL of silver sulfide (Ag)2S) catalyst, 0.02-0.10 g zinc dibutyldithiocarbamate (Zn (ddtc)2) Or manganese dibutyldithiocarbamate (Mn (ddtc)2) Mixing and stirring uniformly;
the volume ratio of the mixed solvent is 3: 2, uniformly mixing dodecyl mercaptan and dodecylamine;
the zinc dibutyldithiocarbamate (Zn (ddtc))2) Or manganese dibutyldithiocarbamate (Mn (ddtc)2) Is a precursor;
(2) under the protection of inert gas or vacuum, heating to 120-140 ℃, and preserving heat for 20-30 min to obtain zinc sulfide nanowires or manganese sulfide nanowires;
(3) further, 0.02 to 0.10g of manganese dibutyldithiocarbamate (Mn (ddtc))2) Or zinc dibutyldithiocarbamate (Zn (ddtc)2) Stirring uniformly, heating to 120-140 ℃ under the protection of inert gas or vacuum, preserving heat for 20-30 min, cooling to room temperature, and centrifugally washing for 6 times by using cyclohexane to obtain the one-dimensional heterogeneous nano material of manganese sulfide and zinc sulfide.
In steps (2) - (3), the inert gas may be argon (Ar) or nitrogen.
The beneficial technical effects of the invention are embodied in the following aspects:
1. the one-dimensional heterogeneous nano material of manganese sulfide and zinc sulfide can be used as a luminescent material to be applied to photoelectric devices, or used as a magnetic material to be applied to magnetic devices, or used as an electrode material to be applied to energy storage devices.
2. In the process of preparing the manganese sulfide and zinc sulfide one-dimensional heterogeneous nano structure, silver sulfide is used as a catalyst. Firstly, catalytically growing a section of zinc sulfide nanowire, and catalytically growing a section of manganese sulfide nanowire at the same temperature after the zinc dibutyl dithiocarbamate precursor is completely consumed; or firstly catalyzing and growing a section of manganese sulfide nanowire, and catalyzing and growing a section of zinc sulfide nanowire at the same temperature after the dibutyl dithiocarbamate manganese precursor is completely consumed. The length of the growing zinc sulfide or manganese sulfide nanowire can be adjusted by adjusting the dosage of the precursor zinc dibutyl dithiocarbamate or manganese dibutyl dithiocarbamate.
3. The process has the advantages of low cost of raw materials, good process controllability, uniform size distribution of products and excellent quality, and is favorable for batch production and industrialization of the one-dimensional heterogeneous nano structure of manganese sulfide and zinc sulfide.
Drawings
FIG. 1 is an X-ray diffraction (XRD) pattern of one-dimensional heterogeneous nanomaterial of manganese sulfide and zinc sulfide obtained in example 1.
FIG. 2 is a Transmission Electron Microscope (TEM) image of one-dimensional heterogeneous nanomaterial of manganese sulfide and zinc sulfide prepared in example 1.
FIG. 3 is an element Mapping diagram of a one-dimensional heterogeneous nanomaterial of single manganese sulfide and zinc sulfide prepared in example 1.
FIG. 4 is the UV-VIS absorption spectrum of the one-dimensional heterogeneous nanomaterial of single manganese sulfide and zinc sulfide prepared in example 1.
FIG. 5 is an element Mapping diagram of a one-dimensional heterogeneous nanomaterial of single manganese sulfide and zinc sulfide prepared in example 2.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
(1) In a flask with vacuum stopper, 9 g of dodecanethiol, 6 mL of dodecylamine, and 0.02 g of zinc dibutyldithiocarbamate (Zn (ddtc))2) Precursor, and 2 mL of silver sulfide (Ag)2S) uniformly stirring the catalyst dispersion liquid;
(2) introducing nitrogen for protection, rapidly heating to 120 ℃, and reacting for 20 min to obtain zinc sulfide nanowires;
(3) an additional 0.02 g of manganese dibutyldithiocarbamate (Mn (ddtc))2) Stirring uniformly, introducing nitrogen for protection, rapidly heating to 120 ℃, and reacting for 15 min; cooling to room temperature, and centrifugally washing with cyclohexane for 6 times to obtain the one-dimensional heterogeneous nano material of manganese sulfide and zinc sulfide.
As can be seen from FIG. 1, the characteristic diffraction peaks in the XRD spectrum of the product of this example 1 indicate that the product is made of Ag2S, ZnS and MnS.
As can be seen from fig. 2, the one-dimensional heterogeneous nano material of manganese sulfide and zinc sulfide in this embodiment 1 is a gray powder after being dried, the shape of the powder particles is a swab-shaped shape, that is, the head of the swab is silver sulfide nano particles, the diameter of the swab is 8 to 16nm, the rod part is composed of segmented manganese sulfide and zinc sulfide, the diameter of the rod part is 7 to 11nm, and the length of the rod part is 50 to 90 nm.
As can be seen from fig. 3, the composition of the one-dimensional heterogeneous nanostructure measured by element Mapping can be described as: the head part consists of silver element and sulfur element, the rod part can be expressed in a sectional way, the part close to the head part consists of manganese element and sulfur element, and the tail part consists of zinc element and sulfur element. The composition is consistent with the feeding sequence of the precursors of the manganese dibutyldithiocarbamate and the zinc dibutyldithiocarbamate, and the process of the invention has good controllability.
As can be seen from fig. 4, the band gap of the one-dimensional hetero nanostructure of the synthesized manganese sulfide and zinc sulfide is 3.8 eV.
Example 2
(1) In a flask with vacuum stopper, 9 g of dodecanethiol, 6 mL of dodecylamine and 0.02 g of manganese dibutyldithiocarbamate (Mn (ddtc))2) And 2 mL of silver sulfide (Ag)2S) uniformly stirring the catalyst dispersion liquid;
(2) introducing argon (Ar) for protection, rapidly heating to 120 ℃, and reacting for 15 min to obtain manganese sulfide nanowires;
(3) further, 0.02 g of zinc dibutyldithiocarbamate (Zn (ddtc))2) Stirring uniformly, introducing argon (Ar) for protection, and quickly heating to 120 ℃ for reaction for 20 min; cooling to room temperature, and centrifugally washing for 6 times by using cyclohexane to obtain the one-dimensional heterogeneous nano material of manganese sulfide and zinc sulfide.
As can be seen from fig. 5, the one-dimensional heterogeneous nanomaterial of manganese sulfide and zinc sulfide of this example 2 is a gray powder after drying, the shape of the powder particles is a swab-like shape, the head portion is composed of silver and sulfur, the composition of the rod portion can be expressed in segments, the portion near the head portion is composed of zinc and sulfur, and the tail portion is composed of manganese and sulfur. The composition is consistent with the feeding sequence of the precursors of zinc dibutyldithiocarbamate and manganese dibutyldithiocarbamate, and the process of the invention has good controllability.
Claims (3)
1. A one-dimensional heterogeneous nano material of manganese sulfide and zinc sulfide is characterized in that: the one-dimensional heterogeneous nano material of zinc sulfide and manganese sulfide is dried to form gray powder, and the band gap size is 3.7-3.9 eV; the shape of the powder particles is a cotton swab rod, the head of the cotton swab is silver sulfide nanoparticles, the diameter of the cotton swab is 8-16 nm, the rod is composed of segmented zinc sulfide and manganese sulfide, the diameter of the rod is 7-11 nm, and the length of the rod is 40-200 nm.
2. The method for preparing one-dimensional heterogeneous nano materials of zinc sulfide and manganese sulfide according to claim 1, which is characterized by comprising the following steps:
(1) mixing 15 mL of mixed solvent, 2 mL of silver sulfide catalyst, and 0.02-0.10 g of zinc dibutyldithiocarbamate or manganese dibutyldithiocarbamate, and uniformly stirring;
the volume ratio of the mixed solvent is 3: 2, uniformly mixing dodecyl mercaptan and dodecylamine;
the zinc dibutyl dithiocarbamate or the manganese dibutyl dithiocarbamate is used as a precursor;
(2) under the protection of inert gas or vacuum, heating to 120-140 ℃, and preserving heat for 15-30 min to obtain zinc sulfide nanowires or manganese sulfide nanowires;
(3) and then adding 0.02-0.10 g of manganese dibutyldithiocarbamate or zinc dibutyldithiocarbamate, uniformly stirring, heating to 120-140 ℃ under the protection of inert gas or under vacuum conditions, preserving heat for 15-30 min, cooling to room temperature, and centrifugally washing for 6 times by using cyclohexane to obtain the one-dimensional heterogeneous nano material of manganese sulfide and zinc sulfide.
3. The method of claim 2, wherein: in steps (2) - (3), the inert gas may be argon (Ar) or nitrogen.
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| CN114538388A (en) * | 2022-04-15 | 2022-05-27 | 合肥工业大学 | Preparation method of zinc selenide nanowire with controllable composition |
| CN114560504A (en) * | 2022-04-15 | 2022-05-31 | 合肥工业大学 | Preparation method of manganese sulfide nanocone material |
| CN114602508A (en) * | 2022-04-02 | 2022-06-10 | 吉林化工学院 | Preparation and application of MnS @ ZnS core-shell hollow sphere with photocatalytic performance |
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| CN114602508A (en) * | 2022-04-02 | 2022-06-10 | 吉林化工学院 | Preparation and application of MnS @ ZnS core-shell hollow sphere with photocatalytic performance |
| CN114602508B (en) * | 2022-04-02 | 2023-08-04 | 吉林化工学院 | Preparation and application of MnS@ZnS core-shell hollow sphere catalyst with photocatalytic performance |
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